(Rapra Technology Limited) ISBN 1-85957-333-9 · Rapra Technology Limited, Shawbury, ... Abstract...

Analysis of Plastics

ISBN 1-85957-333-9

Martin J. Forrest

(Rapra Technology Limited)

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1. A commissioned expert review, discussing a key topic of current interest, and referring to the References andAbstracts section. Reference numbers in brackets refer to item numbers from the References and Abstractssection. Where it has been necessary for completeness to cite sources outside the scope of the Rapra Abstractsdatabase, these are listed at the end of the review, and cited in the text as a.1, a.2, etc.

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Item 1Macromolecules33, No.6, 21st March 2000, p.2171-83EFFECT OF THERMAL HISTORY ON THE RHEOLOGICALBEHAVIOR OF THERMOPLASTIC POLYURETHANESPil Joong Yoon; Chang Dae HanAkron,University

The effect of thermal history on the rheological behaviour of ester- andether-based commercial thermoplastic PUs (Estane 5701, 5707 and 5714from B.F.Goodrich) was investigated. It was found that the injectionmoulding temp. used for specimen preparation had a marked effect on thevariations of dynamic storage and loss moduli of specimens with timeobserved during isothermal annealing. Analysis of FTIR spectra indicatedthat variations in hydrogen bonding with time during isothermal annealingvery much resembled variations of dynamic storage modulus with timeduring isothermal annealing. Isochronal dynamic temp. sweep experimentsindicated that the thermoplastic PUs exhibited a hysteresis effect in theheating and cooling processes. It was concluded that the microphaseseparation transition or order-disorder transition in thermoplastic PUs couldnot be determined from the isochronal dynamic temp. sweep experiment.The plots of log dynamic storage modulus versus log loss modulus variedwith temp. over the entire range of temps. (110-190C) investigated. 57 refs.

GOODRICH B.F.USA

Accession no.771897

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Previous Titles Still AvailableVolume 1Report 3 Advanced Composites, D.K. Thomas, RAE, Farnborough.

Report 4 Liquid Crystal Polymers, M.K. Cox, ICI, Wilton.

Report 5 CAD/CAM in the Polymer Industry, N.W. Sandlandand M.J. Sebborn, Cambridge Applied Technology.

Report 8 Engineering Thermoplastics, I.T. Barrie, Consultant.

Report 11 Communications Applications of Polymers,R. Spratling, British Telecom.

Report 12 Process Control in the Plastics Industry,R.F. Evans, Engelmann & Buckham Ancillaries.

Volume 2Report 13 Injection Moulding of Engineering Thermoplastics,

A.F. Whelan, London School of Polymer Technology.

Report 14 Polymers and Their Uses in the Sports and LeisureIndustries, A.L. Cox and R.P. Brown, RapraTechnology Ltd.

Report 15 Polyurethane, Materials, Processing andApplications, G. Woods, Consultant.

Report 16 Polyetheretherketone, D.J. Kemmish, ICI, Wilton.

Report 17 Extrusion, G.M. Gale, Rapra Technology Ltd.

Report 18 Agricultural and Horticultural Applications ofPolymers, J.C. Garnaud, International Committee forPlastics in Agriculture.

Report 19 Recycling and Disposal of Plastics Packaging,R.C. Fox, Plas/Tech Ltd.

Report 20 Pultrusion, L. Hollaway, University of Surrey.

Report 21 Materials Handling in the Polymer Industry,H. Hardy, Chronos Richardson Ltd.

Report 22 Electronics Applications of Polymers, M.T.Goosey,Plessey Research (Caswell) Ltd.

Report 23 Offshore Applications of Polymers, J.W.Brockbank,Avon Industrial Polymers Ltd.

Report 24 Recent Developments in Materials for FoodPackaging, R.A. Roberts, Pira Packaging Division.

Volume 3Report 25 Foams and Blowing Agents, J.M. Methven, Cellcom

Technology Associates.

Report 26 Polymers and Structural Composites in CivilEngineering, L. Hollaway, University of Surrey.

Report 27 Injection Moulding of Rubber, M.A. Wheelans,Consultant.

Report 28 Adhesives for Structural and EngineeringApplications, C. O’Reilly, Loctite (Ireland) Ltd.

Report 29 Polymers in Marine Applications, C.F.Britton,Corrosion Monitoring Consultancy.

Report 30 Non-destructive Testing of Polymers, W.N. Reynolds,National NDT Centre, Harwell.

Report 31 Silicone Rubbers, B.R. Trego and H.W.Winnan,Dow Corning Ltd.

Report 32 Fluoroelastomers - Properties and Applications,D. Cook and M. Lynn, 3M United Kingdom Plc and3M Belgium SA.

Report 33 Polyamides, R.S. Williams and T. Daniels,T & N Technology Ltd. and BIP Chemicals Ltd.

Report 34 Extrusion of Rubber, J.G.A. Lovegrove, NovaPetrochemicals Inc.

Report 35 Polymers in Household Electrical Goods, D.Alvey,Hotpoint Ltd.

Report 36 Developments in Additives to Meet Health andEnvironmental Concerns, M.J. Forrest, RapraTechnology Ltd.

Volume 4Report 37 Polymers in Aerospace Applications, W.W. Wright,

University of Surrey.

Report 39 Polymers in Chemically Resistant Applications,D. Cattell, Cattell Consultancy Services.

Report 41 Failure of Plastics, S. Turner, Queen Mary College.

Report 42 Polycarbonates, R. Pakull, U. Grigo, D. Freitag, BayerAG.

Report 43 Polymeric Materials from Renewable Resources,J.M. Methven, UMIST.

Report 44 Flammability and Flame Retardants in Plastics,J. Green, FMC Corp.

Report 45 Composites - Tooling and Component Processing,N.G. Brain, Tooltex.

Report 46 Quality Today in Polymer Processing, S.H. Coulson,J.A. Cousans, Exxon Chemical International Marketing.

Report 47 Chemical Analysis of Polymers, G. Lawson, LeicesterPolytechnic.

Volume 5Report 49 Blends and Alloys of Engineering Thermoplastics,

H.T. van de Grampel, General Electric Plastics BV.

Report 50 Automotive Applications of Polymers II,A.N.A. Elliott, Consultant.

Report 51 Biomedical Applications of Polymers, C.G. Gebelein,Youngstown State University / Florida Atlantic University.

Report 52 Polymer Supported Chemical Reactions, P. Hodge,University of Manchester.

Report 53 Weathering of Polymers, S.M. Halliwell, BuildingResearch Establishment.

Report 54 Health and Safety in the Rubber Industry, A.R. Nutt,Arnold Nutt & Co. and J. Wade.

Report 55 Computer Modelling of Polymer Processing,E. Andreassen, Å. Larsen and E.L. Hinrichsen, Senter forIndustriforskning, Norway.

Report 56 Plastics in High Temperature Applications,J. Maxwell, Consultant.

Report 57 Joining of Plastics, K.W. Allen, City University.

Report 58 Physical Testing of Rubber, R.P. Brown, RapraTechnology Ltd.

Report 59 Polyimides - Materials, Processing and Applications,A.J. Kirby, Du Pont (U.K.) Ltd.

Report 60 Physical Testing of Thermoplastics, S.W. Hawley,Rapra Technology Ltd.

Volume 6Report 61 Food Contact Polymeric Materials, J.A. Sidwell,

Rapra Technology Ltd.

Report 62 Coextrusion, D. Djordjevic, Klöckner ER-WE-PA GmbH.

Report 63 Conductive Polymers II, R.H. Friend, University ofCambridge, Cavendish Laboratory.

Report 64 Designing with Plastics, P.R. Lewis, The Open University.

Report 65 Decorating and Coating of Plastics, P.J. Robinson,International Automotive Design.

Report 66 Reinforced Thermoplastics - Composition, Processingand Applications, P.G. Kelleher, New Jersey PolymerExtension Center at Stevens Institute of Technology.

Report 67 Plastics in Thermal and Acoustic Building Insulation,V.L. Kefford, MRM Engineering Consultancy.

Report 68 Cure Assessment by Physical and ChemicalTechniques, B.G. Willoughby, Rapra Technology Ltd.

Report 69 Toxicity of Plastics and Rubber in Fire, P.J. Fardell,Building Research Establishment, Fire Research Station.

Report 70 Acrylonitrile-Butadiene-Styrene Polymers,M.E. Adams, D.J. Buckley, R.E. Colborn, W.P. Englandand D.N. Schissel, General Electric Corporate Researchand Development Center.

Report 71 Rotational Moulding, R.J. Crawford, The Queen’sUniversity of Belfast.

Report 72 Advances in Injection Moulding, C.A. Maier,Econology Ltd.

Volume 7

Report 73 Reactive Processing of Polymers, M.W.R. Brown,P.D. Coates and A.F. Johnson, IRC in Polymer Scienceand Technology, University of Bradford.

Report 74 Speciality Rubbers, J.A. Brydson.

Report 75 Plastics and the Environment, I. Boustead, BousteadConsulting Ltd.

Report 76 Polymeric Precursors for Ceramic Materials,R.C.P. Cubbon.

Report 77 Advances in Tyre Mechanics, R.A. Ridha, M. Theves,Goodyear Technical Center.

Report 78 PVC - Compounds, Processing and Applications,J.Leadbitter, J.A. Day, J.L. Ryan, Hydro Polymers Ltd.

Report 79 Rubber Compounding Ingredients - Need, Theoryand Innovation, Part I: Vulcanising Systems,Antidegradants and Particulate Fillers for GeneralPurpose Rubbers, C. Hepburn, University of Ulster.

Report 80 Anti-Corrosion Polymers: PEEK, PEKK and OtherPolyaryls, G. Pritchard, Kingston University.

Report 81 Thermoplastic Elastomers - Properties and Applications,J.A. Brydson.

Report 82 Advances in Blow Moulding Process Optimization,Andres Garcia-Rejon,Industrial Materials Institute,National Research Council Canada.

Report 83 Molecular Weight Characterisation of SyntheticPolymers, S.R. Holding and E. Meehan, RapraTechnology Ltd. and Polymer Laboratories Ltd.

Report 84 Rheology and its Role in Plastics Processing,P. Prentice, The Nottingham Trent University.

Volume 8

Report 85 Ring Opening Polymerisation, N. Spassky, UniversitéPierre et Marie Curie.

Report 86 High Performance Engineering Plastics,D.J. Kemmish, Victrex Ltd.

Report 87 Rubber to Metal Bonding, B.G. Crowther, RapraTechnology Ltd.

Report 88 Plasticisers - Selection, Applications and Implications,A.S. Wilson.

Report 89 Polymer Membranes - Materials, Structures andSeparation Performance, T. deV. Naylor, The SmartChemical Company.

Report 90 Rubber Mixing, P.R. Wood.

Report 91 Recent Developments in Epoxy Resins, I. Hamerton,University of Surrey.

Report 92 Continuous Vulcanisation of Elastomer Profiles,A. Hill, Meteor Gummiwerke.

Report 93 Advances in Thermoforming, J.L. Throne, SherwoodTechnologies Inc.

Report 94 Compressive Behaviour of Composites,C. Soutis, Imperial College of Science, Technologyand Medicine.

Report 95 Thermal Analysis of Polymers, M. P. Sepe, Dickten &Masch Manufacturing Co.

Report 96 Polymeric Seals and Sealing Technology, J.A. Hickman,St Clair (Polymers) Ltd.

Volume 9

Report 97 Rubber Compounding Ingredients - Need, Theoryand Innovation, Part II: Processing, Bonding, FireRetardants, C. Hepburn, University of Ulster.

Report 98 Advances in Biodegradable Polymers, G.F. Moore &S.M. Saunders, Rapra Technology Ltd.

Report 99 Recycling of Rubber, H.J. Manuel and W. Dierkes,Vredestein Rubber Recycling B.V.

Report 100 Photoinitiated Polymerisation - Theory andApplications, J.P. Fouassier, Ecole Nationale Supérieurede Chimie, Mulhouse.

Report 101 Solvent-Free Adhesives, T.E. Rolando, H.B. FullerCompany.

Report 102 Plastics in Pressure Pipes, T. Stafford, RapraTechnology Ltd.

Report 103 Gas Assisted Moulding, T.C. Pearson, Gas Injection Ltd.

Report 104 Plastics Profile Extrusion, R.J. Kent, TangramTechnology Ltd.

Report 105 Rubber Extrusion Theory and Development,B.G. Crowther.

Report 106 Properties and Applications of ElastomericPolysulfides, T.C.P. Lee, Oxford Brookes University.

Report 107 High Performance Polymer Fibres, P.R. Lewis,The Open University.

Report 108 Chemical Characterisation of Polyurethanes,M.J. Forrest, Rapra Technology Ltd.

Volume 10

Report 109 Rubber Injection Moulding - A Practical Guide,J.A. Lindsay.

Report 110 Long-Term and Accelerated Ageing Tests on Rubbers,R.P. Brown, M.J. Forrest and G. Soulagnet,Rapra Technology Ltd.

Report 111 Polymer Product Failure, P.R. Lewis,The Open University.

Report 112 Polystyrene - Synthesis, Production and Applications,J.R. Wünsch, BASF AG.

Report 113 Rubber-Modified Thermoplastics, H. Keskkula,University of Texas at Austin.

Report 114 Developments in Polyacetylene - Nanopolyacetylene,V.M. Kobryanskii, Russian Academy of Sciences.

Report 115 Metallocene-Catalysed Polymerisation, W. Kaminsky,University of Hamburg.

Report 116 Compounding in Co-rotating Twin-Screw Extruders,Y. Wang, Tunghai University.

Report 117 Rapid Prototyping, Tooling and Manufacturing,R.J.M. Hague and P.E. Reeves, Edward MackenzieConsulting.

Report 118 Liquid Crystal Polymers - Synthesis, Properties andApplications, D. Coates, CRL Ltd.

Report 119 Rubbers in Contact with Food, M.J. Forrest andJ.A. Sidwell, Rapra Technology Ltd.

Report 120 Electronics Applications of Polymers II, M.T. Goosey,Shipley Ronal.

Volume 11

Report 121 Polyamides as Engineering Thermoplastic Materials,I.B. Page, BIP Ltd.

Report 122 Flexible Packaging - Adhesives, Coatings andProcesses, T.E. Rolando, H.B. Fuller Company.

Report 123 Polymer Blends, L.A. Utracki, National ResearchCouncil Canada.

Report 124 Sorting of Waste Plastics for Recycling, R.D. Pascoe,University of Exeter.

Report 125 Structural Studies of Polymers by Solution NMR,H.N. Cheng, Hercules Incorporated.

Report 126 Composites for Automotive Applications, C.D. Rudd,University of Nottingham.

Report 127 Polymers in Medical Applications, B.J. Lambert andF.-W. Tang, Guidant Corp., and W.J. Rogers, Consultant.

Report 128 Solid State NMR of Polymers, P.A. Mirau,Lucent Technologies.

Report 129 Failure of Polymer Products Due to Photo-oxidation,D.C. Wright.

Report 130 Failure of Polymer Products Due to Chemical Attack,D.C. Wright.

Report 131 Failure of Polymer Products Due to Thermo-oxidation,D.C. Wright.

Report 132 Stabilisers for Polyolefins, C. Kröhnke and F. Werner,Clariant Huningue SA.

Volume 12

Report 133 Advances in Automation for Plastics InjectionMoulding, J. Mallon, Yushin Inc.

Report 134 Infrared and Raman Spectroscopy of Polymers,J.L. Koenig, Case Western Reserve University.

Report 135 Polymers in Sport and Leisure, R.P. Brown.

Report 136 Radiation Curing, R.S. Davidson, DavRad Services.

Report 137 Silicone Elastomers, P. Jerschow, Wacker-Chemie GmbH.

Report 138 Health and Safety in the Rubber Industry, N. Chaiear,Khon Kaen University.

Report 139 Rubber Analysis - Polymers, Compounds andProducts, M.J. Forrest, Rapra Technology Ltd.

Report 140 Tyre Compounding for Improved Performance,M.S. Evans, Kumho European Technical Centre.

Report 141 Particulate Fillers for Polymers, Professor R.N.Rothon, Rothon Consultants and ManchesterMetropolitan University.

Report 142 Blowing Agents for Polyurethane Foams, S.N. Singh,Huntsman Polyurethanes.

Report 143 Adhesion and Bonding to Polyolefins, D.M. Brewisand I. Mathieson, Institute of Surface Science &Technology, Loughborough University.

Report 144 Rubber Curing Systems, R.N. Datta, Flexsys BV.

Volume 13

Report 145 Multi-Material Injection Moulding, V. Goodship andJ.C. Love, The University of Warwick.

Report 146 In-Mould Decoration of Plastics, J.C. Love andV. Goodship, The University of Warwick

Report 147 Rubber Product Failure, Roger P. Brown

Report 148 Plastics Waste – Feedstock Recycling, ChemicalRecycling and Incineration, A. Tukker, TNO


ISBN 1-85957-333-9

Martin J. Forrest

(Rapra Technology Limited)


1

Contents

1. Introduction .............................................................................................................................................. 3

2. Analytical Techniques ............................................................................................................................. 3

2.1 Wet Chemistry Techniques ............................................................................................................. 3

2.2 Spectroscopic Techniques ............................................................................................................... 4

2.2.1 Infrared Spectroscopy (IR) ................................................................................................. 42.2.2 Ultraviolet Light Spectroscopy (UV) ................................................................................. 42.2.3 Nuclear Magnetic Resonance Spectroscopy (NMR) ......................................................... 42.2.4 Atomic Absorption Spectroscopy (AAS) ........................................................................... 42.2.5 X-Ray Fluorescence Spectroscopy (XRF) ......................................................................... 52.2.6 Raman Spectroscopy .......................................................................................................... 5

2.3 Chromatographic Techniques ......................................................................................................... 5

2.3.1 Gas Chromatography-Mass Spectrometry (GC-MS) ......................................................... 52.3.2 Gas Chromatography (GC) ................................................................................................ 62.3.3 High Performance Liquid Chromatography (HPLC) ......................................................... 62.3.4 Liquid Chromatography-Mass Spectroscopy (LC-MS) ..................................................... 62.3.5 Gel Permeation Chromatography (GPC) ........................................................................... 62.3.6 Thin Layer Chromatography (TLC) ................................................................................... 7

2.4 Thermal Techniques ........................................................................................................................ 7

2.4.1 Differential Scanning Calorimetry (DSC) ......................................................................... 72.4.2 Dynamic Mechnanical Thermal Analysis (DMTA) ........................................................... 82.4.3 Thermogravimetric Analysis (TGA) .................................................................................. 9

2.5 Elemental Techniques ................................................................................................................... 12

2.6 Microscopy Techniques ................................................................................................................ 12

2.7 Miscellaneous Techniques ............................................................................................................ 12

3. Determination of Molecular Weight and Microstructure of Plastic Polymers ................................ 12

3.1 Determination of Molecular Weight ............................................................................................. 12

3.1.1 Gel Permeation Chromatography (GPC) ......................................................................... 133.1.2 Viscosity ........................................................................................................................... 143.1.3 Osmometry ....................................................................................................................... 143.1.4 Light Scattering ................................................................................................................ 143.1.5 Other Methods .................................................................................................................. 15

3.2 Monomer Types and Microstructure ............................................................................................ 15

4. Determination of Polymer Type ........................................................................................................... 15

5. Determination of the Plasticiser and Filler in a Plastic Compound ................................................. 19

5.1 Determination of Plasticiser ......................................................................................................... 19

5.2 Determination of Fillers ................................................................................................................ 19

5.2.1 Particulate Fillers .............................................................................................................. 195.2.2 Fibrous Fillers ................................................................................................................... 20

6. Determination of Stabilisers in a Plastics Compound ....................................................................... 21

6.1 UV Stabilisers ............................................................................................................................... 21

6.2 Antioxidants .................................................................................................................................. 22


2

The views and opinions expressed by authors in Rapra Review Reports do not necessarily reflect those ofRapra Technology Limited or the editor. The series is published on the basis that no responsibility orliability of any nature shall attach to Rapra Technology Limited arising out of or in connection with anyutilisation in any form of any material contained therein.

7. Determination of Functional Additives ............................................................................................... 24

7.1 Process Aids and Lubricants ......................................................................................................... 24

7.2 Slip Additives ................................................................................................................................ 25

7.3 Pigments ........................................................................................................................................ 25

7.4 Antistatic Agents ........................................................................................................................... 25

7.5 Crosslinking Agents and Co-Agents............................................................................................. 26

7.6 Blowing Agents ............................................................................................................................. 27

7.7 Flame Retardants .......................................................................................................................... 28

7.8 Impact Modifiers ........................................................................................................................... 28

8. Analysis of Plastics for Food Contact Use ........................................................................................... 28

8.1 Global Migration Tests ................................................................................................................. 29

8.2 Specific migration and residual monomer tests ............................................................................ 30

9. Determination of Stabilisers in PVC ................................................................................................... 31

10. Analysis of Plastic Laminates and Fibres ............................................................................................ 32

11. Surface Analysis of Plastics ................................................................................................................... 34

11.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................................................... 34

11.2 Laser Induced Mass Analysis (LIMA) ......................................................................................... 34

11.3 Secondary Ion Mass Spectroscopy (SIMS) .................................................................................. 36

12. Failure Diagnosis ................................................................................................................................... 36

12.1 Common Compositional Problems ............................................................................................... 36

12.2 Environmental Stress Cracking .................................................................................................... 37

12.3 Contamination Problems .............................................................................................................. 37

12.4 Odour and Emissions Problems .................................................................................................... 37

13. Conclusions ............................................................................................................................................. 38

Additional References ................................................................................................................................... 39

Appendix 1. Solubility Parameters of Plastics, Plasticisers and Typical Solvents .................................. 41

Appendix 2. Specific Gravities of Plastics and Compound Ingredients .................................................. 43

Abbreviations and Acronyms ....................................................................................................................... 45

Abstracts from the Polymer Library Database .......................................................................................... 47

Subject Index ............................................................................................................................................... 133


3

1 Introduction

Plastics present chemical analysts with one of their mostdifficult, but satisfying, challenges. In order to obtainuseful products that perform under a variety ofdemanding conditions, the plastic matrix can be tailormade by the bringing together of a wide range ofpolymers and additives. There is a very wide range ofpolymer types available and in some cases they areblended together. The technology of plastics is thereforea mature one, allowing fine tuning of a compound to fita number of design criteria and product requirements.

The choice of materials available means that plasticscan be used in many applications, ranging fromreplacement windows to packaging materials, andfrom mundane products such as disposable cutlery tohighly specialised components in electrical andaerospace products.

The plastics analyst has therefore to bear in mind thepossible complexity of the system that confronts himand the potential interferences that may be broughtinto play. When reverse engineering a plasticcompound a considerable number of elemental,spectroscopic, chromatographic and thermaltechniques have to be used in an integrated andstructured approach in order to accumulate and crosscheck the data necessary for an accurate result. Withsufficient experience and access to the necessaryinstrumental techniques, it should be possible for theanalyst to successfully elucidate a formulation. Thedetermination of the particular ‘grade’ of plastic,although a consistent request, is however rarelypossible. This is mainly due to the fact that a numberof manufacturers produce very similar, if not identical,products or that the material has been speciallycompounded for a particular purpose. Commercialconfidentiality can also restrict the ability to use theanalytical data to identify a particular manufacturer’sproduct as a significant amount of compositionalinformation may not be disclosed.

The objective of this review is to present, as fully as ispossible within this format, an introduction to thetechniques and methods that are used to characteriseand carry out quality control work on plastics; toinvestigate the failure of plastic products; and todeformulate plastic compounds.

With respect to the last category, the analyst’s job whencharacterising ‘unknowns’ is always made much easierif at least some information is available on the sampleand the types of species that may be present in it. Armedwith this knowledge they can work much more

efficiently and obtain better results. To assist in theacquisition of this knowledge opportunities have beentaken within the text to not only detail the analyticalmethods, but provide examples of the species that theymay be used to detect and quantify. In other words, inorder to have a full understanding of the principlesbehind and surrounding the analytical methods andapproaches it is vital to have an understanding of plastictechnology itself.

Relevant books and academic papers are citedthroughout the review, but there are also a number ofgeneral texts which will provide useful further reading(79, 199, 315, 377, 387, 398, a.1-a7).

The appendices provide useful additional information.Appendix 1 gives solubility parameters of a range ofmaterials. Appendix 2 lists the specific gravities of arange of plastics and compounding ingredients.

2 Analytical Techniques

2.1 Wet Chemistry Techniques

Before the advent of modern instrumental techniques,plastic analysis relied on a sequence of wet chemistryreactions to determine information such as the genericpolymer type of a material.

The amount of wet chemistry carried out in the modernpolymer analysis laboratory in the 21st Century isminimal. There are some tests which can still begrouped under this heading, although even some ofthese can employ an instrumental technique to providethe final answer.

One such method is the oxygen flask combustionmethod, which can be used on PVC products todetermine the amount of PVC in the formulation byquantifying the chlorine present.

The oxygen flask method (ISO 6528.1-1992 and BS7164 Section 23.1- 1993) uses an initial burn in oxygen(although the sample is trapped between two platinumgauge ‘flags’) and trapping of the volatile products inan absorbing solution comprising 1-5 ml of 0.05Mpotassium hydroxide, 0.2 ml of 30% hydrogen peroxideand 10 ml of distilled water. Once the volatiles havebeen trapped there is a choice of analytical method. Atitration can be performed, or ion chromatography canbe used to quantify the chloride ion.


4

2.2 Spectroscopic Techniques

2.2.1 Infrared Spectroscopy (IR)

Infrared spectroscopy (IR) is used extensively in theanalysis of plastics. It is a very good, relatively quicktechnique for the determination of the polymer presentin a plastic product. Unlike rubbers, where the majorityof compounds contain additives such as carbon blackand plasticisers that can interfere with the infrared dataobtained, it is normally possible to record infrared spectradirectly from the plastic sample using either a surfacetechnique (e.g., attenuated total reflectance (ATR)spectroscopy) or in transmission through the samplefrom a film produced by pressing a specimen above itsglass transition or melting point.

Some plasticised plastics products (e.g., PVC or nylon11) will need to be extracted with a solvent (e.g.,methanol) first to remove the plasticiser. Products thatare filled (e.g., polypropylene/talc kettle bodies) willrequire a pyrolysis technique where a pyrolysiscondensates infrared library, such as the one publishedby Rapra Technology, needs to be available.

It is also possible with amorphous plastics that are solublein conventional solvents (e.g., chloroform) at roomtemperature to record infrared spectra from films castfrom solution. This approach has the drawback that allthe solvent needs to be removed from the film ifinterference bands are to be avoided.

Analysis of the solvent extract obtained to prepare theplastic sample for an IR technique can be used to identifythe plasticiser present in a compound. IR analysis of anash of the compound obtained by heating at 550 °C canhelp to identify inorganic fillers. IR can also be used toidentify specialist additives such as fire retardants.

2.2.2 Ultraviolet Light Spectroscopy (UV)

Although not as universally used as IR, UV is anotherspectroscopic technique which has a role to play in the

analysis of plastics. It is used in the qualitative andquantitative analysis of additives, particularlyantioxidants and UV stabilisers.

2.2.3 Nuclear Magnetic Resonance Spectroscopy(NMR)

NMR is a powerful tool for the determination ofpolymer structure. It is at its most sensitive when usedon analytes in solution. Table 1 gives examples ofsolvents used for NMR. Amorphous plastics, such aspolystyrene can be dissolved in deuterated chloroform,whereas for the less soluble semi-crystalline plastics(e.g., PET) solvents such as trichloroacetic acid haveto be used. Of the conventional instruments, both protonand carbon 13 instruments have been used in plasticsanalysis. Combinations of two solvents can be used toachieve a good degree of solubility and elevatedtemperatures (e.g., 70 °C) are also common. The protonNMR solvents can be used for carbon 13 experiments,but the reverse is rarely the case.

Techniques are available for work on a specific plastictype, e.g., in the analysis of polyvinylidene fluoride,fluorine 19 NMR can be used. In this case a solventsuch as dimethylformamide is employed.

The 13C NMR spectrum for a polypropylene-polyethylene copolymer is shown in Figure 1. Thespectrum was obtained at 90 °C in a solution of ortho-dichlorobenzene. The major peaks at 21, 27 and 46ppm are due to the polypropylene, with the other, minorpeaks being due to polyethylene.

2.2.4 Atomic Absorption Spectroscopy (AAS)

This technique, and the related inductively coupledplasma (ICP), are used where it is necessary to quantifymetals in a plastic compound. Although not oftenrequired it can be of use in the analysis of flameretardant systems, where additives such as antimonytrioxide and zinc borate have been used.

scitsalpnokrowRMNnidesustnevlosfoselpmaxE1elbaT

RMNnotorP RMN31nobraC

mroforolhcdetaretueD ohtrO enezneborolhcid

dicacitecaoroulfirT enezneborolhcirT

eneznebdetaretueD enatpeh,.g.e,snobracordyhcitahpilA

enahtedetaretued-orolhcarteT-2,2,1,1


5

2.2.5 X-Ray Fluorescence Spectroscopy (XRF)

This technique is very useful for obtaining semi-quantitative elemental data from plastic compounds andtheir ashes. Among other things, it helps to identifyinorganic fillers and pigments in samples. Thetechnique is usually used in conjunction with IR.

When it comes to analysing small samples, samplesurfaces or contaminants in samples, the scanningelectron microscope (SEM)/XRF combination(sometimes referred to as energy dispersive analysis(Edax)) can be a very valuable tool.

2.2.6 Raman Spectroscopy

Until 1986 Raman spectrometers were either dispersivelong focal length double monochromators or shorterfocal length triple monochromators and required highlytrained scientists to obtain good quality data. The adventof the Fourier Transform (FT)-Raman technique in 1986significantly reduced data acquisition times and alsobrought the technical advantage of suppressing any laserinduced fluorescence within the sample. Furtherdevelopments have enabled smaller, low cost, highperformance, quality instruments to be produced and

have led to the development of the Raman microscope -an instrument analogous to the IR microscope.

This has enabled Raman spectroscopy to be usedroutinely for the identification of polymer types andthe analysis of contaminants within polymer samples.

2.3 Chromatographic Techniques

2.3.1 Gas Chromatography-Mass Spectrometry(GC-MS)

This powerful, versatile technique can be used toobtain a significant amount of compositionalinformation on plastic samples. It is particularly usefulin identifying minor components of the sample suchas the stabiliser, antistatic agent and, whereappropriate, the crosslinking system.

It can also be used to investigate the polymer fractionwithin a sample when the instrument is fitted with apyrolysis unit set at around 600 °C.

The technique also plays a role in failure diagnosis bybeing able to provide information on odours, and

Figure 113C NMR spectrum of polypropylene-polyethylene copolymer


6

organic contaminants that may have degraded theplastic matrix.

There are a variety of ways that the sample or fractionsof the sample (e.g., an extract) can be analysed by GC-MS. These include static headspace, dynamicheadspace, solution injection and pyrolysis.

2.3.2 Gas Chromatography (GC)

This technique can also be used to obtain polymer typeinformation by use of a pyrolysis approach, althoughthe technique is less powerful because of the absenceof a mass spectrometer, and a pyrogram ‘fingerprint’has to be used and a comparison made against a libraryof known standards.

This technique is also used for the identification andquantification of additives such as antioxidants and,where sufficient volatility exists, plasticisers andorganic flame retardants.

2.3.3 High Performance Liquid Chromatography(HPLC)

HPLC can be used to identify and quantify additivesthat are either too involatile or insufficiently stable tobe determined by GC/GC-MS. This is particularly thecase with antioxidants such as Irganox 1010 and 1036.

HPLC also comes into its own in the quantification ofplasticisers such as dioctyl phthalate (DOP).

2.3.4 Liquid Chromatography-Mass Spectroscopy(LC-MS)

This instrument is essentially a coupling of an HPLCwith a mass selective detector and as such offers asignificant enhancement in performance to the polymerchemist. Although such combinations have been aroundfor many years, they were complex and expensive (i.e.,effectively research tools only), and it is only withinthe last five years or so that single quadrupole benchtopLC-MS systems have become reasonably commonplace due to their relative ease of use and cost.

A mass spectrometer can be the ideal detector forliquid chromatography because it offers bothuniversality and the required selectivity for complexanalytical problems. For many years developmentwork has concentrated particular on the design of

the interface between the chromatograph and thedetector. Today, the two most popular types ofinterface for the benchtop single quadrupole LC-MSare the particle beam interface and the atmosphericpressure ionisation (API) interface. The particlebeam interface is used to generate electron ionisation(EI) spectra and the API interface is used to generateeither electrospray (ESI) or atmospheric pressurechemical ionisation (APCI) spectra. A furthercomplexity is that the API interface can generateeither positive (i .e. , molecular ion plus onehydrogen) spectra or negative (i.e., molecular ionminus one hydrogen) spectra.

The particle beam interface is very good forqualitative work because the 70 eV spectra containa significant amount of structural information andcan be searched against conventional mass spectralibraries. However, in the full scan mode thesensitivity is restricted to the low nanogram levels.

In the case of the API interface, both the electrosprayand APCI modes are soft ionisation techniques whichleave the molecular ion (or pseudomolecular ion)intact without much fragmentation. The interfacetherefore offers more sensitivity and is ideal forquantitative work at low levels (e.g., contaminationof drug and food matrices by polymer additives/breakdown products).

2.3.5 Gel Permeation Chromatography (GPC)

For this technique to be successful the sample mustbe readily soluble in an organic solvent. It has a wideapplication in the analysis of plastic samples. It ispossible to obtain molecular weight data on bothamorphous plastics and semi-crystalline plastics. Inthe amorphous case (e.g., polystyrene), the systemused is set around ambient temperature (30 °C) andsolvents such as THF, chloroform and toluene areused. With semi-crystalline plastics (e.g.,polyolefins), more aggressive solvents such as ortho-dichlorobenzene and meta-cresol are used at elevated(140 °C) temperatures.

In the case of some complex plastic systems (e.g.,blends), the development of interfaces such as theLab Connections LC Transform, have proved veryuseful in increasing the amount of information thatcan be obtained in a GPC analysis by enabling IRdata to be recorded on the resultant chromatogram.Hence, with the correct choice of separating column,polymer blends can be separated and identified aswell as plasticisers.


7

2.3.6 Thin Layer Chromatography (TLC)

TLC is a relatively simple technique that can be usedfor both the separation and identification of additivessuch as antioxidants and UV stabilisers. A number ofapproaches are possible using different developingsolvents and spraying agents.

It is also the case that TLC can be used in a preparativeway for the isolation of sample fractions for subsequentchromatographic or spectroscopic analysis.

TLC does have the image of being somewhat oldfashioned and it is to be expected that the marketpenetration of LC-MS systems will further erode thestanding of this technique in the modern analyticallaboratory.

2.4 Thermal Techniques

2.4.1 Differential Scanning Calorimetry (DSC)

DSC is used extensively in the analysis of plastics,particularly those that are semi-crystalline - polyolefins,nylons, polyesters, etc. It is sensitive enough to

differentiate between different polyethylenes (i.e.,LDPE, LLDPE, HDPE, etc.) from their melting pointsand the appearance of their melting endotherms as wellas being able to detect and, with appropriate standardmaterials, quantify plastic blends, e.g., PP/PE and nylon6/nylon 6,6.

The DSC trace for a quenched sample of PET is shownin Figure 2. This trace shows the Tg (around 75 °C) ofthe material, the exothermic formation of the crystallinephase (at 156.9 °C) and the endotherm due to themelting of this phase (at 255 °C).

The DSC trace of a plastic blend is shown in Figure 3.The data obtained has been compared to standards andthe material has been shown to be a blend of ethylene-vinyl acetate copolymer (EVA) and LDPE. Theapproximate proportions of each is EVA 15-20%/LDPE20-25%. In addition the EVA copolymer is thought tocontain around 20-25% of vinyl acetate (VA).

Although not as sensitive as dynamic mechanicalthermal analysis (DMTA) to glass transitions, DSC canbe used to identify a plastic from the glass transition inits thermogram. The glass transition (Tg) and crystallinemelting temperatures (Tm) of a range of plastics aregiven in Table 2.

Figure 2

DSC trace for a quenched sample of PET


8

Figure 3

DSC trace of a blend of EVA and LDPE

It is also possible to use DSC to provide quality controlfingerprint thermograms from which deviations in thecomposition of a plastic compound can be detected.One reason for this is that although the technique isnot capable of determining the molecular weight of aplastic, differences in molecular weight will be apparentin the melting endotherm region.

Using appropriate standard materials it is alsopossible to use DSC to quantify the level of certainadditives, e.g., peroxides, in a sample.

DSC can also be used in thermal stability studies ofthe plastic compound, and to investigate theeffectiveness of antidegradants and fire retardants.

2.4.2 Dynamic Mechnanical Thermal Analysis(DMTA)

DMTA is very useful for generating modulus versustemperature data on plastic compounds. The effects

of temperature on this important material property canbe obtained over a wide temperature range (typically–150 °C to +200 °C), along with the glass transitiontemperature and information on thermal stability.

The use of DMTA to differentiate between plasticsamples that have a similar chemical composition, butvery different physical properties is shown inFigure 4. Both of these samples are polymethyl-methacrylate (PMMA), but the top one is crosslinkedhaving been prepared with a small amount ofdifunctional monomer and the bottom sample is thestandard thermoplastic material. It can be seen thatthe crosslinked sample does not melt and the modulusdoes not fall away significantly until thermaldegradation occurs.

The sensitivity of DMTA to glass transitiontemperatures (approximately 1,000 times greater thanDSC which measures heat capacity changes rather thanmodulus) is very useful in the analysis of plastics andtheir blends.


9

2.4.3 Thermogravimetric Analysis (TGA)

This technique is useful in the analysis of compoundedplastic samples. It is possible to obtain accuratequantifications of the principal compound constituentssuch as plasticiser, polymer and inorganic species.This data can be obtained on small (e.g., 10 mg)samples in a relatively short time (around 45 minutes).By the use of the temperature maxima at which weightevents occur it is also possible to use the technique toobtain some qualitative assignments for the plasticiserand polymer.

A typical TGA programme would be:

Heat from ambient to 550 °C in a nitrogen atmosphereat 20 °C/min until no further weight loss occurs. Then,reduce the heat to 300 °C, change the atmosphere toair and heat at 20 °C/min to 1,000 °C.

It is common to plot the weight loss derivative inconjunction with the weight loss, and this can be usedto detect the presence of a polymer blend of two or morecomponents. Thermal decomposition temperatures of arange of plastics are shown in Table 3.

T(noitisnartssalG2elbaT g T(serutarepmetgnitlemenillatsyrcdna) m scitsalpfoegnarafo)

epyTscitsalP Tg (° )C Tm (° )C

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)EPDL(501

)EPDM(511

)EPDH(531

enelyporpyloP 5 061

ene-1-tubyloP 02– 021

ene-1-tnepyloP 42 07

EFTP 511 723

)EFTCP(enelyhteoroulfirtorolhcyloP 25 122

lohoclalynivyloP 07 TwolebsesopmoceD g

edirolhclynivyloP 08 -

edirolhcenedilynivyloP 81– 091

elirtinolyrcayloP 041ot08 -

enerytsylopcitcatA 59 -

enerytsylopcitcatosI 001 032

TEP 76 652

etalyrcahtemlyhteM 001 -

AlonehpsibfoetanobracyloP 051 522

AlonehpsibfoenoflusyloP 591 -

6nolyN 05 512

6,6nolyN 06 662

edixoenelyhteyloP 55– 66

edixoenelyporpyloP 26– 56

rehtelyhtemlynivyloP 13– 441

rehtelyhtelynivyloP - 68

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10

Figure 4

DMTA results for (a) crosslinked and (b) standard grades of PMMA


11

Other uses for the technique include the production ofcompositional fingerprints for quality control purposesand the investigation of thermal stability and the effectsthat additives such as flame retardants and antioxidantshave on it.

It is possible to interface modern TGA instruments directlyto IR instruments or mass spectrometers, thus obtainingboth quantitative and qualitative data in one analytical step.

The introduction of high resolution TGA instrumentshas enabled more accurate quantifications of minorweight loss events to be made. For example, the use ofhigh resolution TGA to quantify the amount of residualmonomer in a sample of polymethylmethacrylate isshown in Figure 5. The residual monomer weight lossevent peaks at 297.5 °C.

scitsalpfoegnarafoserutarepmetnoitisopmocedlamrehT3elbaT

epyTcitsalP (*noitisopmoced%05eveihcaoterutarepmeT ° )C

edirolhclynivyloP 062

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Figure 5

High resolution TGA of polymethylmethacrylate


12

2.5 Elemental Techniques

The determination of the concentration of certainelements can be very useful in plastic analysis work.In particular, it is often necessary to determine theamount of nitrogen or a halogen such as chlorine orfluorine in the calculation of polymer content orpolymer blend proportions. Also, the targeting ofspecific elements can enable the quantity of aparticular additive (e.g., phosphate flame retardant ortitanium dioxide pigment) to be calculated.

The determination of nitrogen is usually done usingcarbon/hydrogen/nitrogen analysers and the techniqueis relatively simple and uses small amounts (e.g., 20-50 mg) of sample.

With the other elements, the technique will varyaccording to the element being quantified. Sulfur andchlorine, for example, can be determined usingoxygen combustion followed by ion chromatographyanalysis of the products.

2.6 Microscopy Techniques

High magnification (e.g., 150x) optical microscopycan be used to examine the dispersion of fillers withinthe plastic matrix. The success of this operation isusually dependent on the generation of high qualitymicrotome sections of the sample.

The technique of scanning electron microscopy hasalready been briefly mentioned in Section 2.2.5 inrelation to the elemental analysis of surfaces inconjunction with XRF. It can also be used in its ownright, where its high magnification powers can beemployed to determine the particle size of fillers andin the detailed examination of fracture surfaces.

Transmission electron microscopy (TEM) can be usedto investigate the phase morphology of polymerblends and the dispersion of fillers.

For other spectroscopic techniques see Section 2.2.

2.7 Miscellaneous Techniques

There are a number of other analytical techniques thatcan be used to characterise plastic samples and manyof these feature in the abstracts at the back of thisReview Report. These include X-ray diffraction(XRD) to identify between different crystalline forms

of inorganic additives (e.g., rutile and anatase formsof titanium dioxide) and direct probe massspectroscopy (for the determination of high molecularweight antioxidants).

Surface analysis techniques such as secondary ion massspectrometry (SIMS), laser induced mass analysis(LIMA) and X-ray photoelectron spectroscopy (XPS)are used for failure diagnosis work associated with suchthings as poor bonding to substrates and for surfacecharacterisation work.

A chromatography technique that achieved prominencein the research literature around ten to fifteen yearsago for the determination of relative high molecularweight additives (e.g., antioxidants) and the study ofplastic oligomers is supercritical fluid chromatography(SFC). This is essentially a liquid chromatographytechnique that uses similar analytical columns to HPLCbut where the mobile phase is a substance (e.g., carbondioxide) that is kept in a supercritical state by a suitablecombination of temperature and pressure. One of thebenefits of the technique is that the analytes can beeasily separated from the mobile phase once thechromatography has taken place so, for example, theycan be deposited on infrared transparent substrates foranalysis using an infrared microscope. The relativelyexpensive nature of the instrumentation and thedevelopment of other techniques (e.g., LC-MS) haverestricted its market penetration.

3 Determination of Molecular Weightand Microstructure of Plastic

Polymers

This section covers analytical techniques that can beapplied both to uncompounded plastic resins andcompounded materials.

3.1 Determination of Molecular Weight

In common with other polymers, plastics have adistribution of molecular weights. This distribution willbe widest for polymers produced by free radicalpolymerisation (e.g., polystyrene) and narrowest forplastics produced using specialised catalyst systemssuch as metallocenes.

There are a number of ways in which the molecularweight distribution of a plastic can be expressed:


13

Mn = Number average molecular weight = Sum nMSum n

Mw = Weight average molecular weight = Sum nM2Sum nM

Mz = Z average molecular weight = Sum nM3Sum nM2

where n = the number of molecules of molar mass M.

The Z average is very sensitive to high molecularweight molecules within the polymer. The weightaverage is always of greater value than the numberaverage. A measure of the breadth of the moleculardistribution of the polymer can be obtained by dividingthe weight average by the number average:

Polydispersity = MwMn

As the polymer tends to monodispersity thepolydispersity approaches unity.

There are a wide variety of methods that can be usedto obtain molecular weights. The principal ones areas follows.

3.1.1 Gel Permeation Chromatography (GPC)

This is the pre-eminent technique and has been refinedand developed extensively over the past 30 years.

It is possible to use it on both uncompounded resinsand plastic compounds and Mn, Mw and Mz valuescan be obtained. GPC is essentially a liquidchromatography technique where the sample isdissolved in a suitable solvent (e.g., THF forpolystyrene) and injected into a system where themolecules are separated according to their molecularsize by a column that contains a swollen, particulate,porous gel packing.

Figure 6 shows the GPC chromatograms for twopolymers that have different molecular weightdistributions but similar calculated molecular weightaverages.

The standard detector for GPC systems is the refractiveindex (RI) detector, but a feature of developments overthe past 10 years is the development of double (RI andviscosity) or triple detector systems (RI, viscosity andlight scattering). These multiple detection systemsprovide measures of ‘true’ molecular weight byobtaining the actual Mark-Houwink parameters (in thecase of the viscosity detector) for the polymer being

Figure 6

GPC chromatograms for two polymers with different molecular weight distributions but similarmolecular weight averages


14

analysed, as opposed to the polystyrene equivalentmolecular weight from the use of monodispersepolystyrene calibrants alone. An inherent property ofthe light scattering detector is that it provides ‘true’molecular weight data.

It is also possible to use spectroscopic detectors suchas infrared and ultraviolet. One practical use of thelatter is to determine if chemical modifiers (e.g., silanecoupling agents) are bound to polymer molecules.This is done by measuring the molecular weightdistribution of the modified plastic at a UVwavelength where the polymer itself does notcontribute to the absorbance and comparing this tothe distribution of the unmodified plastic.

The use of the LC transform module with GPC hasextended its capabilities by allowing IR data to begenerated on the species during the course of an analysis.This is done by impinging the species onto a germaniumdisc which is then placed into a module fitted into thesample compartment of an IR bench. IR data is collectedon the entire chromatogram using continuous collectionsoftware, which enables the IR spectrum of any particularsection to be viewed. This technique is very useful forplastic blends and highly compounded plastics such atPVC, as it allows the polymers in the blend to beidentified, as well as relatively high molecular weightadditives such as plasticisers.

3.1.2 Viscosity

This is a standard procedure for molecular weightdeterminations and involves the use of speciallydesigned viscometers to accurately measure theviscosity of a polymer solution. From this the intrinsicviscosity is determined and hence the molecular weight.The time taken for the polymer solution to pass betweentwo marks on the viscometer is compared to that ofpure solvent and the ratio is the viscosity of the solution.Successive dilutions give a range of concentrations andtimes from which the intrinsic viscosity can becalculated. The value for this is then entered into theMark-Houwink equation:

Intrinsic viscosity = KMX

where K and X are constants for the particular solventbeing used and are referred to as the Mark-Houwinkparameters.

Depending on the source of the Mark-Houwinkparameters the molecular weight can be expressed aseither the number or weight average.

3.1.3 Osmometry

There are two principal osmometry techniques: vapourpressure osmometry and membrane osmometry.

Vapour pressure osmometry involves the indirectmeasuring of the lowering of the vapour pressure of asolvent due to the presence of a solute. It is based on themeasurement of the temperature difference betweendroplets of pure solvent and of polymer solutionmaintained in an isothermal atmosphere saturated withthe solvent vapour. Calibration is by the analysis ofstandards of known molecular weight and should be overthe entire range of molecular weights of interest to ensurethe best results. The technique is useful for polymersthat have molecular weights in the 500-50,000 range.

Membrane osmometry involves the use of amembrane between the solvent and the polymersolution that is permeable to the solvent moleculesbut not to the solvated polymer molecules. This isthe major restriction on the technique and means thatit cannot be used for low molecular weight polymers(< approximately 50,000).

3.1.4 Light Scattering

Recent developments in instrumentation have led to aresurgence of this technique where the weight averagemolecular weight is obtained from the light scatteringbehaviour of polymer solutions. These developmentshave centred around low angle laser light scattering(LALLS), multi-angle laser light scattering (MALLS)and evaporative light scattering (ELS). As well as beingstand alone instruments, light scattering detectors havebeen developed for GPC systems. MALLS detectorscan provide direct information on the branching ratioof a polymer (a.8).

Care has to be taken to ensure that the polymer solutionis clear (to reduce variability) and low cell volumes(0.1 µl) and dilute solutions help this. Solvent choiceis also critical, with the best results being with solventsthat have a very different refractive index to thepolymer, and that are low-scattering themselves.

Evaporative light scattering involves the removal ofthe solvent from the solvated polymer as it elutes downa drift tube and the isolated polymer particles thenscatter light from the light source.

Light scattering can produce precise data and has beenused successfully on polymers with molecular weightsranging from 10,000 to 10,000,000.


15

3.1.5 Other Methods

Other methods include end group analysis (Mn),ultracentrifugation (Mw) and, indirectly by determiningglass transition temperatures, DSC/DTA.

A review of the determination of the molecular weightof polymers has been produced by Holding andMeehan (396).

3.2 Monomer Types and Microstructure

The use of transmission IR, pyrolysis IR and pyrolysisGC to determine the polymer type of a plastic is coveredin Section 2.1. Where appropriate standards areavailable, it is also possible to use IR to quantify theamounts of monomers in copolymers and terpolymers.

Another technique that is very effective at identifyingthe monomers present in a plastic materials is NMR.The NMR technique will also provide information onthe proportions of the various monomers in copolymersand tripolymers. In contrast to IR this information canbe obtained without having to analyse standards ofknown monomer composition; the areas under thediagnostic chemical shifts being used.

NMR instruments can also be used to obtainfundamental structural information on polymers suchas end group chemistry, branch points and structuralisomerism. It is also possible to use IR for the latter,although some of the isomeric structures have relativelyweak absorptions which makes detection difficult whenthey are at a low concentration.

4 Determination of Polymer Type

One of the most basic and useful tests to carry out on aplastic sample is to determine its polymer type.

Due to their relative simplicity, it is usually possible tocarry out an infrared analysis of the plastic material inthe as received state and identify the plastic by referenceto a standards database. The advent of the single bounceattenuated total reflectance (ATR) accessories forFourier transform infrared spectroscopy (FTIR)instruments enables this operation to be carried out ina matter of minutes on a sample a few millimetres insize. Some care should be taken as the relativeintensities of the bands present in ATR spectra can vary

compared to conventional transmission spectra(historically used to compile databases) and there is aslight shifting in the absorption wavenumber value ofthe bands.

If more traditional spectra are required, the usualapproach is to press a thin film of the samples using atemperature which is above the Tg or Tm and to recorda transmission spectrum. A transmission infraredspectrum of polypropylene produced from a filmpressed at 170 °C is shown in Figure 7. Anothertechnique that can be used to obtain transmissionspectra is to dissolve the sample up using a suitablesolvent and to cast a film. Care has to be taken toremove all of the solvent by drying in an oven otherwiseit can influence the data obtained. A transmissioninfrared spectrum of PVC produced from a film castfrom a solution in THF is shown in Figure 8.

For those plastic compounds that contain a plasticiserand/or organic flame retardant, a certain amount ofpreparation work is required to effectively remove theinterference of these constituents. After milling orcomminuting the sample to increase surface area, asolvent extraction is performed to remove these organicspecies. It is then usually possible to record the infraredspectrum using either an ATR technique or bytransmission through a hot pressed film.

One of the most comprehensive databases availableof plastic infrared spectra has been produced byHummel (a.9).

Where the plastic sample contains both a major organicadditive and a filler, it is necessary to pyrolyse theextracted portion of the sample and then record aninfrared spectrum of the collected pyrolysiscondensates. Providing that an extensive database ofpyrolysate spectra is available (234), this method isvery successful in identifying generic polymer typesand polymer blends. In the case of blends, it is alsopossible to express the results semi-quantitatively ifthe appropriate standards are available.

If the plastic only contains a filler, the pyrolysisapproach can be employed without using the initialsolvent extraction step.

The pyrolysate infrared spectra of nylon 6 and lowdensity polyethylene are shown in Figures 9 and 10,respectively.

Another method which enables the polymer type withina plastic sample to be identified is pyrolysis gaschromatography. This method can be applied to either


16

Figure 7

Transmission infrared spectrum of polypropylene produced from a film pressed at 170 °C

Figure 8

Transmission infrared spectrum of unplasticised PVC produced from a film cast from a THF solution


17

Figure 9

Pyrolysate infrared spectrum of nylon 6

Figure 10

Pyrolysate infrared spectrum of low density polyethylene


18

the extracted portion of the sample or the sample asreceived. In the former case any relatively low molecularweight plasticiser elutes early on and does not have asignificant influence on the pyrogram as a whole. Aswith pyrolysis IR, a database of standards needs to beput together and then the pyrogram fingerprints ofunknowns can be matched. The temperature that thepyrolysis unit is set at, and the design of the unit (e.g.,Curie point or microfurnace), will affect the pyrogramsproduced from a particular sample. Again, it is possibleto identify and quantify blends and blend ratios.

Typical experimental conditions for pyrolysis GCexperiments are as follows:

Sample weights 0.1-5.0 mg

Pyrolysis temperatures 400-800 °C (microfurnaceand Curie point)

800-1200 °C (platinumfilament)

Microfurnace type pyrolyser - specific example usingan SGE Pyrojector

Weight of sample 0.4 mg

Pyrolysis temperature 600 °C

Pyrolysis gas Helium at 0.10 MPa

GC column 5% Diphenyl siloxane 30m x 0.25 mm, 1.0 µm film

GC column temperature 2 min at 50 °C followedprogram by 10 °C/min to 280 °C

and then 10 min at 280 °C

GC carrier gas Helium at 0.06 MPa

GC injector temperature 320 °C

Detector Flame ionisation detector(FID) at 350 °C

Adding a mass spectrometer into the system, so thatthe technique becomes pyrolysis GC-MS, furtherincreases the usefulness of the method and theinformation that can be obtained.

The principal diagnostic pyrolysis species which canbe detected in pyrograms of plastics are shown inTable 4.

It can be seen from the above list that certain plastics‘unzip’ to regenerate their monomers whereas otherundergo decomposition reactions to generatecharacteristic breakdown products. In reality, acertain amount of both types of reaction take placefor the majority of polymers and it is the one thatpredominates that determines what the majorpyrolysis products will be.

With respect to the quantification of the polymercomponent within a plastic compound, the easiesttechnique to use is TGA. It is also possible to detect ablend of polymers with TGA and to often obtain asemi-quantification of the blend ratio by reference tothe splitting of the weight loss derivative.Unfortunately, some plastic types (e.g., PVC) undergotwo stage weight loss processes when heated and thefirst stage (loss of hydrogen chloride) will overlapwith the volatilisation of organics (e.g., plasticiser)stage. It is therefore not possible to use TGA alone todetermine the polymer content of these samples.

Another complicating factor is that a number of plastics(e.g., halogenated, polyamides, polyurethanes,polyesters, other heteroatom containing systems) donot completely pyrolyse during the nitrogenatmosphere region and leave a carbonaceous residuewhich essentially oxidises to carbon dioxide in the airregion. This carbonaceous residue, which may to anextent overlap with any weight loss due to a carbonblack pigment, has to be included in order to obtain anaccurate polymer content.

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19

5 Determination of the Plasticiser andFiller in a Plastic Compound

5.1 Determination of Plasticiser

Mention has already been made in Section 4 of theisolation of plasticisers from a plastic matrix bysolvent extraction. Careful choice of solvent isrequired to ensure that the polymer itself doesn’tundergo dissolution and that the plasticiser isselectively isolated. A solvent which has been foundto be useful for polymers such as PVC is methanol.The extraction is carried out under Soxhletconditions with the weight of extract being obtainedfrom the weight gain of the conditioned solventreservoir flask once the solvent has been dried offat 105 °C.

Having quantified the plasticiser present byextraction it is then possible to obtain anidentification by the use of transmission IR. Thereis an excellent database available (399) whichenables an identification to be made. Where theplasticisers have distinct IR spectra (e.g., phthalatesand sulfonamides) it is possible to detect thepresence of a blend of plasticisers. If a quantificationof the blend composition is required, though, this isusually easier to achieve by HPLC then IR.

The TGA technique can usually provide a goodquantification of plasticiser content. Plasticisers thathave higher molecular weights (e.g., so calledpolymerised plasticisers) can give problems as theweight loss event due to their volatilisation canmerge with the pyrolysis weight loss event of thepolymer. As mentioned in the above section,polymers that lose small molecules by heatdegradation (e.g., HCl lost by PVC) give morecomplicated TGA traces and will require a solventextraction step to determine their plasticiser level.

5.2 Determination of Fillers

5.2.1 Particulate Fillers

On some occasions, carbonaceous fillers such as aconducting black (acetylene black) or graphite areadded to a plastic to enable it to meet certainconductivity requirements. It is possible to use TGAto quantify these types of fillers. It is also a usefulway of differentiating between these materials and

conventional carbon black; the former having amaximum oxidation weight loss around 700 °C andthe latter around 550 °C.

The TGA trace for an EVA cable covering filled witha conducting black is shown in Figure 11.

The fact that a number of rubbers (e.g., halogenated,nitrile and polyurethane) produce carbonaceousresidues during the nitrogen atmosphere region hasalready been mentioned in Section 4.1, and care mustbe taken to ensure that these do not affect thequantification of the carbonaceous filler in the airatmosphere region. Use of a high resolution TGAinstrument will assist in this as it will improve theseparation of the two weight loss events.

TGA is also convenient for the quantification ofinorganic fillers such as barytes, silica and silicates.The limitation of the technique is that the totalinorganic content of the plastic is obtained, with noindication of the relative proportion if a blend ofinorganic fillers is present. It is therefore commonpractice to complement the TGA data with a least asemi-quantitative elemental technique such as XRFin order to obtain qualitative as well as quantitativedata. A useful exception to this rule is where thecompound contains calcium carbonate (a relativelycommon diluent filler), in which case the carbonatewill undergo quantitative degradation at around 680-700 °C into carbon dioxide and calcium oxide (whichremains as a residue). It is therefore possible toquantity the amount of calcium carbonate in thesample from the carbon dioxide weight loss (whichwill represent 44% of the carbonate by mass) andthe remaining quantity of residue will indicate if anyother inorganics are present.

The other technique commonly used for thequantification and isolation of inorganic materials(both fillers and additives such as glass fibres) isfurnace ashing. This method is described in ISO345-1 (1997) and a temperature of 500-600 °C isusually used.

Once the ash has been obtained, qualitativeinformation on the inorganic species present can beobtained by IR (liquid paraffin mull technique), XRFor, where the quantification of specific species isrequired, ICP.

Some of the principal diagnostic IR absorption bandsfor inorganic fillers are given in Table 5.


20

Figure 11

TGA trace for an EVA cable cover compound showing weight loss and derivative weight loss curves

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5.2.2 Fibrous Fillers

In certain applications it is necessary to impart thestrength required to a plastic part by the use of a fibrousfillers. The following types are among those used:

(1) Glass fibres

(2) Carbon fibres

(3) Synthetic polymer fibres (e.g., nylon)

(4) Wood flour

It is usually obvious whether a plastic contains a fibrousfiller from either a visual inspection or the use of arelatively low powered optical microscope.

Glass fibres can be isolated and gravimetricallydetermined by ashing at 600 °C in a muffle furnace.Higher temperatures (above 700 °C) can cause problemsas the glass will eventually reach its melting point.Confirmation that the fibres are glass can be carried outusing an infrared microscope. The IR microscope willalso give the cellulose spectrum which is expected for


21

the wood flour filler type, and be able to detect the typeof synthetic fibre (e.g., nylon or polypropylene) usedfrom its characteristic transmission spectrum.

TGA will enable the amount of carbon fibres in acomposite to be quantified. The oxidation temperatureof around 700 °C (instead of the 500-600 °Cexperienced with carbon blacks) will also provide aconfirmation of their presence.

As mentioned above, synthetic polymeric fibres can beidentified by the IR microscope once sufficiently isolatedor, by use of their melting point, by the hot stagemicroscope or DSC. In the case of DSC, somequantification data can be obtained from the size of themelting endotherm providing standards are available.

6 Determination of Stabilisers in aPlastics Compound

In common with other polymer systems, to maintainthe physical properties of a plastic compound stabilisersneed to be added to stop, or at least retard, degradationby a number of agencies (e.g., heat and UV light).

The use of an initial solvent extraction/dissolution stepis common in the analysis of a plastic matrix forantidegradants, as these species may not be volatileenough to be removed by heating the sample. In somecases (e.g., butylated hydroxytoluene) heating a sampleliberates enough of the species to enable an identificationto be made using GC-MS; however quantification willusually require removal by a solvent (to as near 100%efficiency as possible). Analysis of the extract can thenbe carried out by HPLC, UV spectroscopy, or GC if thespecies is heat stable and sufficiently volatile. Relativelynon-specific solvents (i.e., having mid-range solubilityparameters) such as chloroform are good extractingsolvents. Another common approach is to dissolve upthe sample in a suitable solvent and then add a non-solvent to precipitate the polymer. The stabiliser willremain in the solvent phase.

If the type of organic antidegradant in a compound iscompletely unknown, analysis of the solvent extractby GC-MS or LC-MS is an excellent method foridentification. Once the identification has beenachieved, a quantification can be carried out using apreferred method and a validated procedure if available.

Where the antidegradant is not volatile enough to beidentified using a GC based technique, direct probemass spectrometry or LC-MS can be used and the

antidegradant identified by reference to its molecularion and a database. The direct probe mass spectroscopytechnique can be carried out on samples in the asreceived state as well as sample extracts, whereas LC-MS is only used for extracts.

6.1 UV Stabilisers

There is a large range of commercial UV stabilisersfor plastic materials and a number of analyticalapproaches can be used for their detection andquantification.

The UV stabilisers can be divided into five differentgroups:

(a) Benzophenone derivatives

(b) Salicyclic acid esters

(c) Resorcinol esters

(d) Benzotriazole compounds

(e) Coumarin drivatives

In a number of cases specific methods have beendeveloped to determine a particular stabiliser within aparticular polymer. Some representative methods areoutlined next.

In some cases (e.g., the determination of 2-hydroxy-4-n-octoxybenzophenone in polyethylene) the stabiliserhas distinctive diagnostic bands and the relativesimplicity of the infrared characteristics of the polymermatrix enables it to be quantified using transmissioninfrared spectroscopy. A thin film of the sample isproduced by hot pressing at 120 °C, along with filmsof virgin polyethylene containing known amounts ofthe stabiliser. The absorbance maxima of the diagnosticband between 15.8 and 16.2 microns in the standardfilms is used to produce a calibration curve from whichthe amount of stabiliser in the unknown is calculated.The method is capable of detecting the stabiliser downto 0.02% w/w with an accuracy of +/- 5%.

A number of methods use the UV absorbing propertiesof the UV stabiliser. For example, Tinuvin 326 can bedetected in polypropylene down to 0.02% w/w by usingan extraction with chloroform under reflux followedby analysis of the extract using a UV/Vis spectrometer.The ultraviolet absorption peak at 355 nm is used anda calibration curve produced by dissolving knownamounts of Tinuvin 326 in chloroform.

Another technique uses the fluorescence of thesecompounds. Uvitex OB can be detected in a chloroform


22

solution (0.8% w/v of polymer) of polystyrene byexcitation at 370 nm and recording the fluorescence at435 nm. Standard solutions at the 0.8 w/v level of virginpolystyrene and known amounts of Uvitex OB are usedas calibrants.

It is also possible to use gas chromatography (e.g.,Tinuvin P, Tinuvin 326, Tinuvin 327 and CyasorbUV531 in toluene extracts of polyethylenes), thin layerchromatography (e.g., benzophenone and salicylic acidtypes in polyethylenes) and HPLC. This latter methodhas been used extensively for the determination ofantioxidants but has not received as much attention inthe literature for UV stabilisers.

It is also the case that the white pigment titaniumdioxide provides protection against UV light and sothis can be added at reasonable high loadings (e.g., 10%or greater) to products such as window frames. Theamount of titanium dioxide in a plastic can bedetermined after acid digestion of the matrix by theuse of an elemental technique such as AAS/ICP.

6.2 Antioxidants

HPLC based techniques have been widely used byanalysts for the determination of antioxidants in plasticsand a review has been provided by Sidwell (400).

The chromatogram obtained for the determination ofIrganox 1076 in an HDPE compound is shown inFigure 12. An extract of the polymer was analysedusing a C18 reverse phase column with UV detection at230 nm and a mobile phase of 70:30 methanol/waterchanging to 100% methanol.

There is a useful HPLC method which can be used onplastics for the detection and quantification of a widerange (20 species) of antidegradants. The sample isdissolved up using a suitable solvent at an elevatedtemperature if necessary. A non-solvent (e.g., methanol)is then added and the extract analysed by HPLC usingthe following conditions:

Injection volume 25 µl

HPLC column Aqua 5 C18 ODS reverse phasecolumn 150 mm x 3.0 mm(or similar)

Mobile phase A= 75:25 Methanol/Water

B= 50:50 Ethyl Acetate/Acetonitrile

Gradient Time %A %B

Initial 90 10

After 25 min 0 100

Flow rate 2.0 ml/min

Figure 12

HPLC chromatogram of HDPE for determining Irganox 1076


23

Detection UV detector set at 270 nm

Temperature 40 °C

The following antioxidants are examples of those thatcan be determined using this technique:

(1) Irganox 1010

(2) Irganox 1098

(3) Irganox 1076

(4) Irganox 1330

(5) Butylated hydroxytoluene

(6) Irgafos 168

(7) Triclosan

The chromatogram obtained using this method toseparate a complex cocktail of antidegradants is shownin Figure 13.

The wide applicability of this method is due to themobile phase mixture.

The capability of HPLC has been greatly extended bythe commercialisation of affordable liquidchromatography-mass spectroscopy (LC-MS)instruments. The mass selective detector enablesunknown samples to be analysed and the antioxidantspresent to be identified. The LC-MS techniquetherefore compliments GC-MS and, with it, enablesthe complete molecular weight/volatility/polarity rangeto be covered.

TLC is comparatively easy and cheap to use and it isboth quick and accurate for the identification of

Figure 13

HPLC chromatogram of a complex mixture of antidegradants


24

antioxidants in plastic extracts. Irrespective of thecomplexity of the extract composition and the amountused, this method can be used to give a sharp separationfor identification purposes. Distinctive Rf values andcolours can be seen for each antioxidant depending onthe stationary phase, the developing solvent used andthe detection agent.

TLC, in addition to being used for identificationpurposes, can be used in a semi quantitative way;the logarithm of the spot area being proportional tothe quantity of the analyte in the spot, and this valuebeing compared to spots containing standardamounts of the analyte.

Gas chromatography has been used for the analysis ofphenolic and amine type antioxidants. Antioxidantswhich have high boiling points cannot be directly byGC but they can be analysed as derivatives such asacetates, trifluoroacetates, trimethyl silyl-ethers, methylethers, etc. Trimethyl silane based antioxidants, forexample, give good separations on standard siliconebased columns (a.10).

Benchtop LC-MS instruments are proving to beexcellent tools in the analysis of plastics of unknowncomposition to identify and, once this is achieved,quantify the antioxidant present. Prior to the adventof LC-MS it was very difficult to use conventionalHPLC for this task because of the large range ofpossible compounds.

Using the general analysis conditions shown below anumber of antioxidants can be detected in toluene orchloroform extracts of plastics:

Sample preparation: Around 5 mg of extract is diluted1/20 with 80% acetonitrile/water

Instrument: Agilant 1100 series LC-MS

Column: Zorbac SB-C18, 5 um,2.1 mm x 150 mm

Mobile phase: A=water, B=acetonitrile

Gradient Time A B

Initially 15% 85%

after 10 min 1% 99%

or Initially 35% 65%

after 10 min 10% 90%

Flow rate: 0.7 ml/min

Injection volume: 5 µl

MS conditions: Atmospheric Pressure ChemicalIonisation (APCI)

Ion mode: Positive or negative

Vapouriser: 300 °C

Scan range: 200-1600 amu

Fragmentor: 70 or 120 volts (The fragmentorvoltage is chosen to modify thedegree of fragmentation andhence sensitivity)

Antioxidants which have been identified in polyolefinsusing the above conditions include:

• Irgafos 168

• Irganox 1076

• Irganox B225 (50:50 mixture of Irganox 1010and Irgafos 168)

7 Determination of FunctionalAdditives

7.1 Process Aids and Lubricants

In PVC technology certain polymeric additives can beconsidered as process aids. These polymers have asimilar composition to those used as impact modifiersin PVC formulations but are more compatible and soare primarily included to ensure more uniform flowand hence improve surface finish. Such process aidsinclude ABS, chlorinated polyethylene, MBS, EVA-PVC graft polymers and acrylate-methacrylatecopolymers. As these are usually found in unplasticisedPVC, direct analysis of the product by IR will usuallyindicate the presence of those that have a distinctivespectrum as no masking by plasticiser will take place.However, even rigid PVC can contain a small amountof phthalate and so it is advisable to carry out a solventextraction to clean up the matrix first. Where theprocess aid (e.g., chlorinated polyethylene) has arelatively bland spectrum, a technique such as NMRwill be required to both detect and quantify it. NMRwill usually be required to quantify the other types aswell, unless the spectrum is very distinctive andstandards of known composition are available.


25

In the case where a relatively large quantity of filler(talc) has to be incorporated into a polymer (e.g.,polypropylene) it is often necessary to use a processaid/lubricant such as a zinc or calcium stearate. Aquantification of the process aid can be achieved bythe analysis of the sample for the metal by aciddigestion-AAS. The stearate can be qualitativelydetected by solvent extraction GC-MS.

7.2 Slip Additives

It is common for aliphatic amides to be incorporatedinto plastics, particularly polyethylenes, to act as slipadditives.

It is possible to use LC-MS to detect these types ofslip additives in plastic samples. Using the LC-MSconditions described in Section 6.2, it is possible todetect Behenamide (mixture of two aliphatic amidesof molecular weight 331 and 339) and erucamide(molecular weight 337) in solvent extracts ofpolyethylene and polypropylene.

It is also possible to use GC and GC-MS to analysethese and another common slip additive oleamide inextracts from plastics as they have sufficient volatilityto elute from the GC column.

7.3 Pigments

Pigments are used extensively in plastic compoundsand can be of one of four main types:

(1) Inorganic compounds

(2) Organo-metallic compounds

(3) Organic compounds

(4) Carbon black

Pigments such as titanium dioxide and iron oxidebelong to the first group and the analysis of these isrelatively easy as they are thermally stable (so can bedetermined in both the sample ash or in the sample inthe as received state) and have a diagnostic metal atomtogether with a simple chemical structure. Analysistechniques used are therefore elemental methods suchas AAS and ICP.

Groups 2 and 3 present the analyst with a greaterchallenge as there is a very wide number commercially

available, they have relatively high molecular weightsand so cannot be easily removed from the matrix bysolvent extraction and can be thermally labile.

One technique which has been used to identify both thesetypes of pigment and inorganic ones is vapour phaseultraviolet absorption spectrometry at 200 nm (a.11). Inthis method the samples are powdered and then directlyvapourised in the heated graphite atomiser. Thermalultraviolet profiles of organic pigments show absorptionbands between 300 °C and 900 °C, while profiles ofinorganic pigments are characterised by absorption bandsat temperatures above 900 °C. Specific assignments aremade with respect to temperature, relative intensity andwidth of the absorption bands.

A relatively unknown technique (laser desorption fouriertransform ion cyclotron resonance mass spectroscopy)has been used (397) to identify dyes in plastics such aspolymethylmethacrylate. A detection limit of 0.1% wasobtained, which compared with a limit of 1-2% usingan ATR infrared spectroscopy technique.

Infrared spectroscopy techniques can be useful,particularly if the plastic matrix itself (e.g., polyethylene)has a relatively simple infrared spectrum and if standardinfrared spectra of a wide range of pigments is available.

Carbon black is used extensively as a black pigment inproducts such as cable sheaths. The amount present isusually less than 2% and so its quantification by TGAcan be difficult due to the small sample size (10 mg)used. The standard method to quantify the amount ofcarbon black in such a product is therefore the tubefurnace as much larger sample sizes can be used (e.g.,2 g) and hence more accurate quantifications obtained.

7.4 Antistatic Agents

Antistatic agents are usually hygroscopic compoundswhich readily attract moisture and so inhibit the buildup of a static charge on the surface of a plastic product.They are used in many applications from the body ofthe humble plastic pen to numerous packagingapplications.

The selection of an antistatic agent depends greatly onthe polymer matrix since a degree of incompatibilityis vital to ensure that migration to the surface of theproduct occurs at a fast rate after manufacture. Exactchemical composition information can be difficult toobtain from suppliers and so analysis for these additivescan be difficult.


26

In the case of polystyrene, quaternary ammoniumcompounds are widely used and for polyethylene,polyethylene glycol alkyl esters can be used.

In the case of the glycol esters, these can of sufficientlylow molecular weight to be extractable by solvents suchas diethyl ether and then identified by a chromatographictechnique such as GC-MS. As in a number of cases it isto be expected that LC-MS will play a role in the analysisof these additives in the future.

7.5 Crosslinking Agents and Co-Agents

For some plastic products (e.g., cable sheathing) itcan be necessary to impart a degree of crosslinkinginto the product to achieve the requisite physicalproperties. This can be achieved by irradiation usinggamma rays. However, some polymers degrade whensubjected to high energy radiation as illustrated inTable 6. Chemical agents such as peroxides are alsoused. These species produce diagnostic breakdownproducts the identification of which will reveal thetype of peroxide used.

The most useful technique for this type of work is GC-MS. There are two possible modes of sampleintroduction: solution injection and dynamicheadspace. In the case of the former a useful methodof sample preparation involves cryogenic grinding of0.3 g of the sample, followed by extraction using 2 mlof diethyl ether in an ultrasonic bath for 30 minutes.The resulting extract is then analysed under thefollowing conditions:

Instrument: Hewlett Packard 6890/5973 GC-MSD

Carrier: Helium @ 2.0 ml/min constant flow

Injection mode: 1 µl splitless (0.75 min; 50 ml/min)

Injection temperature: 320 °C

Column type: RTX5-MS 30 m x 0.25 mm,0.25 µm film thickness

Column temperature: 40 °C for 5 min, 20 °C/minup to 300 °C held for 12 min

MS settings: 20 to 620 Daltons scannedevery 0.33 s

In the case of the dynamic headspace approach arelatively small amount of sample (e.g., 3 mg) is heatedin the oven of a dynamic desorption unit and thevolatiles produced collected in a cryogenically cooledTenax filled trap. The experimental conditions are asfollows:

Dynamic Headspace

Instrument: Perkin Elmer ATD 400

Desorption temperature: 150 °C for 10 min

Desorption flow: Helium @ 20 ml/min

Trap collection temperature: –30 °C

Trap injection temperature: 250 °C

Trap outlet split flow: 9 ml/min

Trap inlet split flow: off

Split: 10:1

GC-MS

The conditions used are the same as for the diethylether method with the exception of the following:

GC Column temperature: –30 °C to 50 °C at 5 °C/min,following by 20 °C/min to300 °C and then held at300 °C for 12 min

Carrier Helium @ 0.07 MPa

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27

For either analytical approach, identification of thediagnostic cure system breakdown species is byreference to mass spectral libraries such as thoseproduced by the National Institute of Standards andTechnology (USA) (NIST), the Royal Society ofChemistry, Wiley/NBS (a.12) and the USEnvironmental Protection Agency (EPA)/NationalInstitute of Health (NIH). The mass spectra of themajority of species of interest are in these libraries andso, providing the knowledge to reconstruct cure systemsis available, successful attempts can be made.

One problem associated with this task is that a numberof peroxide curing agents breakdown to give more thatone product and a number of these are common to morethan one peroxide species. This is demonstrated inTable 7.

In addition to identifying the type of peroxide used,these GC-MS techniques will also identify the type ofco-agent (e.g., triallyl cyanurate (TAC) or triallylisocyanurate (TAIC)) used.

7.6 Blowing Agents

There are two main types of blowing agent used withpolymer systems in general:

(1) Chemical Chemical compounds (principallyorganic) that undergo chemicaldecomposition at the processingtemperature to form a gaseous species(e.g., nitrogen) which will create thecellular structure.

Examples include azo compounds,nitroso compounds, sulfonyl hydrazidecompounds and sodium bicarbonate.

(2) Physical Low boiling point organic compounds(e.g., dichloromethane or pentane)which volatilise at the processingtemperature to create a cellularstructure.

With plastics, the most widely used type are thephysical blowing agents.

Where it is suspected that a physical type blowingagent has been used to produce a foam, is it possibleto use headspace GC-MS to identify it. Even in theblown state, the high sensitivity of the techniqueenables an assignment to be made from the smallamount of residual blowing agent that will be present.It is usual to use this type of blowing agent inamorphous plastics that have glass transitiontemperatures around 100 °C, e.g., styrenics. Thisenable the expansion of the plastic to be wellcontrolled.

The reactivity of the chemical blowing agent type canmake analysis difficult (e.g., they will decompose inthe injection port of a GC-MS instrument), and theapproach that is used is to indirectly identify them bythe determination of breakdown fragments. The GC-MS instrument is the best choice for this and a libraryof typical breakdown fragments is required.

Quantification of the chemical blowing agent in anunblown product is very difficult as the polarity andreactivity (e.g., hydrogen bonding reactions andthermal instability) can cause problems during isolationfrom the compound and subsequent analysis. In termsof reverse engineering, this is unlikely to be requiredsince the product will invariably be already blown. Forlaboratories that are carrying out quality control work,other properties such density and expansion ration canbe used to determine compound loadings.

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28

7.7 Flame Retardants

As with blowing agents, there are two main categoriesof flame retardant: organic and inorganic.

The amount and type of organic flame retardant presentin a plastic compound can be determined in ananalogous way to the plasticiser, since this type of flameretardant is usually similar in molecular weight andpolarity and, hence, extractability. Once the type oforganic flame retardant has been determined by IR, anaccurate quantification can be obtained by carrying outan elemental analysis for the halogen (or other relevantelement, e.g., phosphorus) on the unextracted sample.The extract value itself will rarely provide a meaningfulquantification as other species, particularly any processaid/plasticiser, will contribute to it as well. In someinstances (e.g., organophosphates) it may be possibleto use an HPLC analysis of the extract to quantify theflame retardant. GC based techniques can also be usedin some cases, but bromide types present problems forthese techniques because of their relatively highmolecular weights (> 900).

Care must be taken over the quantification of inorganicflame retardants, since some of them (e.g., antimonytrioxide) can react with the organic flame retardantpresent, or break down to produce volatile products,under quantitative ashing conditions, and duringanalysis by thermal techniques such as TGA. A goodinitial approach is a semi-quantitative elementalanalysis by XRF, to see which types are present.Accurate quantifications can then be obtained byprecise elemental determinations.

If it is known that hydrated alumina is present in thesample, it is possible to quantify this reasonably wellusing TGA, by making use of the water loss data.Hydrated alumina loses close to 35% of its weight whenit is heated to 550 °C in a TGA experiment.

7.8 Impact Modifiers

The most commonly encountered impact modifiedplastic is high impact polystyrene (HIPS). The impactmodification is achieved by incorporating discreetdomains of a rubber (butadiene) within the polystyrenematrix. The level of butadiene can be varied accordingto the requirements of the end use. A high level canconvert a glassy brittle material into a ductile, toughproduct. The efficiency of the butadiene to improveimpact resistance alone is not solely related toconcentration, but is also dependent on the size and

distribution within the matrix of the domains thatcontain it. Actual impact performance is determinedby physical tests such as the Charpy and Izod impacttests, and the size and distribution of domains isinvestigated by transmission electron microscopy(TEM), but there are a number of chemical tests thatcan be carried out to determine the level of modifier.

(1) IR analysis - this is performed on a pressed filmand the relative size of the absorption bands due tostyrene (700 cm) and butadiene (966 cm) are takenand compared to standards of known styrene-butadiene levels.

(2) NMR - the plastic is dissolved and the level of thetwo polymers determined by specific shift areas.

(3) Classical wet chemistry - the butadiene level isdetermined in solution by reaction of a reagent withthe double bonds.

There are some instances (e.g., rubber impactmodification of nylon) where the chemical propertiesof the two polymers are so dissimilar that solubilitydifferences can be used to isolate and, in this case,quantify the rubber modifier. The test is carried out bytaking an accurately weighed sample and refluxing itin formic acid until the plastic is digested and only therubber phase remains. The rubber is then washed, driedand weighed.

Other plastics which can contain rubber modifiers (orat least modifiers that have lower glass transitiontemperatures than the plastic phase) include PET andPVC. In the case of PVC, acrylates and methacrylatesare common and the normal approach is to use IR todetect the modifier and then NMR to quantify it.

8 Analysis of Plastics for FoodContact Use

For more than 30 years work has been going oninvolving food contact plastics and the effect thatmigrants from plastics products have on food. The firstEuropean Directive (78/142/EEC), which was on thevinyl chloride monomer content of food contact PVC,was published in the late 1970s and this was followedultimately by the more comprehensive PlasticsDirective (90/128/EEC) in 1990. Since 1990, there hasbeen a gradual harmonisation of European testingrequirements through amendments to 90/128/EEC. Theseventh amendment (2002/17/EC) has recently been


29

published and the initial requirements for testing overalland specific monomer migration have now grown toinclude additive (e.g., antioxidant) migration.

In general, there are two types of analytical test thatare carried out on food contact plastics:

(1) Global migration tests - In these, the plastic is putinto contact with an appropriate food simulantunder representative end use conditions and thetotal amount of material that has migrated into thesimulant determined gravimetrically or, in the caseof involatile food simulants such as olive oil, bygas chromatography.

(2) Specific migration tests - Again, the plastic iscontacted with a food simulant but any analyticalwork in targeted on a specific additive and itsconcentration determined using an appropriatechromatographic technique.

In the case of certain plastics materials, e.g., ABS,grades that are intended for food use have to meetcertain residual monomer targets. Direct analysis ofthese polymers is undertaken to determine theconcentration of these monomers.

8.1 Global Migration Tests

The following food simulants are used for food contactplastics:

Distilled water - Aqueous food use

Distilled water 95%:Ethanol 5% - Alcoholicbeverages such as beers and lagers

Distilled water 85%:Ethanol 15% - Wines

Distilled water 60%:Ethanol 40% - Spirits

A solution of 3% w/v acetic acid in distilled water -Acidic aqueous foods

Olive oil* - Fatty foods (also isopropanol or hexane)

(*Isopropanol and Hexane have been introducedas fatty food simulants to circumvent the analyticalproblems that can occur with olive oil due to itspotential variability as a natural product andinvolatility.)

As mentioned, the global migration figure for a particularplastics material is determined gravimetrically. One

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30

approach is to use conditioned glass crucibles and todry off the simulant on a hot plate after the contactexperiment has been performed under the appropriateconditions (time and temperature).

Once the appropriate simulant has been chosen thecontact time and temperature to use are given in ECDirective 82/711/EEC (Table 8).

In addition, for plastics in contact with food for whicha preservation temperature of less than 20 °C is requiredthe test condition will be 10 days at 20 °C.

The overall global migration limit for plastics is statedin the EC Directive 90/128/EEC as being 10 mg/dm2

(surface area of plastic). This limit can be expressed as60 mg/kg of foodstuff in certain situations. To be usedfor food contact a plastics product must meet thisrequirement.

In a number of packaging types, only one side of aplastic film or laminate may contact the food. Specificsingle side migration cells have been developed (e.g.,by PIRA) to enable the migration from a material underthese conditions to be investigated.

8.2 Specific migration and residual monomer tests

In addition to the global migration limit 90/128/EECalso provides a number of specific migration limits(SMLs) for plastic monomers (Table 9).

There are also SMLs for plastic additives, someexamples are shown in Table 10.

In the case of some monomers, 90/128/EEC gives limits(called quantification limit-monomer (Qm)) relating tothe plastic material itself. For example, vinylidenechloride has a QM of 5 mg/kg of plastic.

Over the years, the detection of species migrating fromfood contact materials has advanced hand in hand withthe gradual lowering of analytical detection limitsbrought about by the refinement of the techniques. Forexample, the SML for acrylonitrile is set at notdetectable above 0.02 mg/kg (i.e., 20 parts per billion)and this would not be obtainable on a routine basiswithout the benefits of modern instrumentation.

The development of suitable methods for the detectionof the wide range of monomers and additives used in

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remonoM LMS

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elirtinolyrcA ffutsdoofgk/gm20.0evobaelbatcetedtoN

matcalorpaC ffutsdoofgk/gm51

edyhedlamroF ffutsdoofgk/gm51

dicacilahthpereT ffutsdoofgk/gm5.7

edirolhcenedilyniV ffutsdoofgk/gm50.0evobaelbatcetedtoN

)CEE/821/09(sevitiddacitsalpemosrofsLMS01elbaT

evitiddA LMS

sretseetalahthpdnaetapidA ffutsdoofgk/gm5.1

edixoirtynomitnA ffutsdoofgk/gm10.0

THB ffutsdoofgk/gm0.3

snobracordyhdetanegordyH ffutsdoofgk/gm0.3

snobracordyhlanoitnevnoC ffutsdoofgk/gm3.0

edimaraets/edimaelO esudoofyttafrofdesuebtonnaC


31

food contact materials requires the application of stateof the art analytical techniques. Normally, headspacemethods are preferred for volatile monomers as suchmethods overcome a lot of the problems of sample matrixclean-up. In principle the food contact simulant, foodstuffor plastic material is heated in a sealed vial fitted withan inert septum (usually PTFE coated rubber). The vialis heated to an accurate set temperature normally in therange 80-100 °C, for an equilibrium time of at least onehour. The headspace above the sample is then analysedfor the presence of the analyte. The quantity of analytein the headspace will always be in equilibrium with theamount present in the sample. Standard addition methodsare used to obtain calibration curves, with the calibrantvials being analysed under the same conditions (i.e., time,temperature and ratio of headspace to bulk material(polymer if necessary)) as the samples. To acquiresufficiently low detection limits it is sometimesnecessary to use specific detectors (e.g., a nitrogen/phosphorus detector (NPD)) or, in the case of massselective detectors, a single ion monitoring approach.For species that are too involatile for headspace basedmethods, other chromatographic and spectroscopicmethods are employed.

A summary of the analytical techniques used in foodmigration work is shown in Table 11.

In the cases where HPLC has been assigned, LC-MSwould also be applicable.

9 Determination of Stabilisers in PVC

Although it is one of the bulk thermoplastics, PVCsuffers from relatively poor stability to ageing agenciessuch as heat and UV light. In order to achieve its statusas an important plastic it was therefore necessary todevelop a specific additive group: PVC stabilisers.

These technological developments have resulted in arange of stabilisers being available that are appropriatefor different grades of PVC, products and end uses.Some of the main types are:

(a) Lead stabilisers (e.g., lead carbonate, lead stearate,lead phthalate)

(b) Metallic soaps (e.g., stearates, palmitates,ricinoleates and octoates of cadmium, barium,calcium and zinc)

(c) Organo-tin compounds (e.g., dibutyltin di-iso-octylthioglycollate)

(d) Epoxide stabilisers (e.g., epoxidised oils andbisphenol A epoxide resins).

The analyst has to bear in mind that it is common for anumber of different stabilisers to be used in a PVCcompound in order achieve the optimum ageing resistance.

gnitsetnoitargimnidesuseuqinhcetlacitylanA11elbaT

etylanA euqinhceT

edirolhclyniV CGecapsdaeH

enerytS CLPHdnaCGecapsdaeH

dicacilahthpereT CLPH

locylgenelyhtE CGecapsdaeH

elirtinolyrcA DPNhtiwCGecapsdaeH

eneidatuB )DSM(rotcetedevitcelesssamhtiwCGecapsdaeH

setanaycosI CLPHnoitasitavireD

edyhedlamroF yrtemirolocnoitasitavireD

sdicacinagrO CIroCLPHriapnoI

sresicitsalP CLPH

stnadixoitnA CFSroCG,CLPH

scinagronI PCIroSAA

scinagroraloP siserohportceleyrallipacdnaCLPH


32

It is obvious that a large number of these stabiliserscontain metal atoms and so a cost effective way ofachieving an initial evaluation of the type of stabiliserpresent is to use a semi-quantitative XRF techniqueon the sample in the as received state. Care should betaken with this as some inorganic pigments/fillers(e.g., titanium dioxide) can mask certain key elements(e.g., cadmium).

If it is a case of quantifying a known stabiliser, thenAAS or ICP can be used to quantify the metal and, withknowledge of the compound formula, the result obtained.

The organo-tin compounds are widely used and foranalytical considerations it is convenient to divide theminto those that contain sulfur and those that do not. Tothe first group belong compounds like dialkyltinmercaptides, mercaptoesters and mercaptocarboxylates, to the second, dialkyltin carboxylates andtheir esters. The identification of acids and alcoholspresent in tin stabilisers containing no sulfur and theidentification of alcohols from stabilisers containingmercaptoesters presents little or no difficulty. However,the identification of the thioacid and of the alkyl groupsattached directly to tin can prove more difficult,especially if long chain acids form part of the compoundor if the stabiliser is not pure, e.g., if it containsplasticiser. The thioacid may also tend to decomposeduring hydrolysis procedures. The application of anumber of analytical methods (e.g., NMR, IR and GC)to determine these types of stabiliser in PVC extractshave been described by Udris (a.13).

Some classic methods based on titration and TLC todetermine organo-tin compounds in solvent extractsof PVC include:

• Potentiometric titration of organo-tin in the extractwith standard sodium methoxide in pyridine usingantimony and calomel electrodes (a.14).

• Titration of dialkyltin thiol compounds in benzene/methanol extract with standard silver nitrate (in IPAmedium) using sulfide coated wire electrode (a.13).

• TLC of organo-tin thioacids and thiols usingKielselgel G plates with development withglacial acetic acid and detection with catecholviolet (a.15).

• TLC of organo-tins using Kieselgel GF 254 withdevelopment using butanol/glacial acetic acidand detection with catechol violet and UVirradiation (a.16).

Of the other types of organo-metallic stabilisers,Mal’kova and co-workers (a.17) have described analternating current polarographic method for thedetermination of cadmium, zinc and barium stearatesor laurates in PVC. Other techniques used on PVCextracts include, column chromatography for barium,cadmium and zinc salts of fatty acids, paperchromatography for cadmium, lead and zinc salts offatty acids (a.18) and polarography for cadmium, leadand zinc salts (a.19).

The advent of bench top LC-MS instruments hasenabled the analysis of stabilisers such as the organo-tin type to be re-examined and laboratories such asthe Analysis Division at Rapra Technology Limitedare investigating the capability of this technique inthis area. This could be another area of plasticsanalysis where LC-MS replaces the more traditionaltechniques.

10 Analysis of Plastic Laminates andFibres

Plastic laminates are used extensively from the ordinarycrisp packet to high specification products for medicaland pharmaceutical use. In all these cases, laminatesare used since the application demands a number ofproperties which no single polymer exhibits.

Taking the example of the crisp packet, the innermostlayer must be inert to the product and provide a barrierto air, the outside layer has to be capable of beingprinted onto and the middle layer (or tie layer) has tobe able to stick both of the other two together.

One of the principle analytical techniques for theanalysis of laminates is the infrared microscope. Thisinstrument is capable of recording transmission infraredspectra from sample down to 10 square microns in size.The approach is usually to prepare a section of thelaminate by microtoming a section and then recordinga spectrum of each layer aided by the masking off ofthe other layers. The sectioning is often undertakenobliquely in order to maximise the apparent layerthickness. The microscope also allows the thicknessof each layer to be determined.

It is also possible to use an ATR technique to recordinfrared spectra of the outside layers and reserve theIR microscope for the central layers. This is possiblebecause the ATR technique only penetrates a fewmicrons into the surface of the layers. It is also possibleby choosing the appropriate crystal (e.g., germanium,


33

zinc selenide, etc) to control the depth of penetration.This can be useful if the layers are particularly thin.

Using the knowledge gained by infrared spectroscopyof the generic polymer types present, the assignmentscan be refined by the use of DSC. Due to the fact thatlaminates by their nature are often constructed ofcompletely different plastic types, the completestructure can be analysed in one operation and themelting endotherm transitions obtained used todifferentiate between various grades. For example inthe case of a laminate which had been shown to becomprised of a polyethylene and a nylon, it would bepossible to differentiate between LLDPE, LDPE andHDPE, and nylon 6 from nylon 6,6.

It is also possible to use a Raman microscope to analysethe different layers that are present within a laminate.As with the IR microscope, it has the ability to isolateindividual layers and, given a satisfactory database, thespectra obtained can be used for identification purposes.

The Raman spectra for four common polymer typesare shown in Figure 14.

Examination of the cross section of laminate samplesunder an optical microscope enables the individuallayers to be viewed. Phase contrast microscopes canaid the differentiation of layers of similar refractiveindex. The use of a polarising microscope can also assistin characterising individual layers and is particularlyuseful when heating laminates under a microscope ona hot stage to recognize the characteristic meltingtemperature of the individual layers.

There are a number of synthetic fibres that can be usedto produce both woven and non-woven fabrics. Themost popular include polyamide, polyester and acrylicsand they can be used in products as varied as clothingand life rafts.

Once again, the infrared microscope is ideal atrecording generic polymer identification spectra fromindividual fibres. Once the generic type has beenestablished, further refinement of the assignment canbe obtained by DSC (e.g., specific polyamide type)and, where a number of fibres are available GPC(molecular weight).

Other microscopic techniques, such as optical (aspectratio), SEM (surface morphology) and EDAX(elemental analysis), Raman microscopy and atomicforce microscopy can be used to further characterisethe product.

Figure 14

Raman spectra of (a) polyethylene, (b) PVC, (c)polystyrene and (d) polyethylene terephthalate


34

11 Surface Analysis of Plastics

There are a number of analytical techniques that canbe used to obtain data on the surface of plasticsmaterials or products. Three of the techniques, IR andRaman microscopy and Edax are covered in Sections2.2.1, 2.2.6 and 2.6. It can be argued that thesetechniques have come into being as the logicaldevelopment of the original, general purposetechniques.

There are however a number of analytical instrumentsthat have been developed with the specific intention ofanalysing surfaces. Three of the principal ones will bementioned in this section.

11.1 X-Ray Photoelectron Spectroscopy (XPS)

In this case the surface of the sample is irradiated withsoft X-rays. These X-rays are sufficiently energetic tocause photoemission of electrons from the core levelsof atoms present on the sample surface. Thephotoelectrons generated are collected and passed toan electron energy analyser and detector. The measuredkinetic energy (KE) of an electron is given by :

KE = hv - BE - sigma

where: hv = energy of the X-ray photon

BE = Binding energy

sigma = work function of the spectrometer

The binding energy of a given core electron ischaracteristic of the element and it is this whichenables the elements on the surface of a sample to beidentified. It is also possible to carry out quantitativework by measuring the relative intensities of thephotoemission from each of the elements present. Thebinding energy of a core level depends principally onthe charge on the nucleus of the atom concerned andsmaller changes are induced as a result of chemicalbonding. Although small, such charges are measurableand provide a means of studying the chemistry of thesample surface (a.20, a.21).

Because only electrons from the top few atomic layerswill have sufficient energy to escape, the technique isvery surface specific and results are normally obtainedfrom between 5 and 10 nm depth at a detection limit ofaround 0.1 atom percent. The analysis area is typically3-10 mm2 and all the elements with the only exceptionof hydrogen can be detected.

Because of its ability to determine surface chemistry,XPS can be particularly useful in the analysis ofpolymer surfaces to see if oxidation has taken placeand, if so, what functional groups (e.g., ester, acid,aldehyde) the oxygen is present in.

This ability of XPS to detect oxygen containingfunctional groups is shown in the narrow and broadscan spectra of PET presented in Figure 15.

Another application is the analysis of polymers todetermine if certain surface treatments (e.g., coronadischarge) have been carried out satisfactorily.

In common with the other surface analysis techniques,it can also be used to investigate surfacecontamination problems and to determine thecomposition of the fracture surfaces in adhesionfailures.

11.2 Laser Induced Mass Analysis (LIMA)

In the LIMA technique, the surface of the sample issubjected to a pulsed UV laser which is sufficientlyenergetic to volatilise a small volume (about 1 µmcube) of material. The ionised fragments in thisvolume are then separated and identified by means ofa time of flight mass spectrometer. Both negative andpositive fragment data can be obtained.

The analysis area in a LIMA experiment is typically1-2 µm, the analysis depth 0.25-0.5 µm and thedetection limit 10-100 ppm. The technique has theability to detect all of the elements in a qualitative way.

The technique is very useful for determiningcompounds on the surface by means of these elementsand molecule fragments, but it is very sensitive, andcare must be taken to ensure that the surface is notcontaminated (e.g., by handling without gloves) andthat the representative control samples are availableto assist in the interpretation of the data.

Its sensitivity and surface specificity make it ideal inthe detection of very low levels of contamination/modification. For example, the detection of amonolayer of silicone contamination of a plastic partthat was hampering the wetting of a paint. It can alsobe used to analyse particulate impurities, fibres anddefects in surface coatings.

LIMA is also referred to as laser microprobe massspectroscopy (LAMMS).


35

Figure 15

XPS spectra of PET (a) narrow spectrum (b) broad spectrum

(a)

(b)


36

11.3 Secondary Ion Mass Spectroscopy (SIMS)

In this technique the sample surface is bombarded by aprimary ion beam (positive ions of argon, caesium,oxygen or gallium). These primary ions impart energyto the surface and, as a consequence of the collisionsproduced, ions, atoms and molecular fragments (calledsputtered particles) are ejected. The primary ions maypenetrate several atom layers into the surface, but thesputtered particles only come from the outer 2-3 atomlayers. In common with the other two techniques,therefore, SIMS is very surface specific and it is possibleto restrict it to a single monolayer. The analysis area istypically 150 µm, the detection limit is 1 ppm and allthe elements are detectable.

Two types of SIMS experiment can be carried out: staticSIMS and dynamic SIMS. In the former case, the surfaceis bombarded with low energy ions and molecular andatomic fragments are produced without the experimentchanging the nature of the surface appreciably; thesurface chemistry can therefore be investigated.Dynamic SIMS uses high energy ions to obtain highlysensitive elemental data down to ppb levels, but thestructural information is lost.

In the case of static SIMS, dedicated libraries are requiredto enable the mass spectra of the fragments to beidentified (a.22).

Another application of SIMS is in the study of themigration of additives (e.g., slip additives and antistats)onto the surface of plastics.

It is often the case that complementary surface analysistechniques such as SIMS and XPS can be used togetherin order to successfully solve a failure or characterisationproblem. In such cases, XPS would be used to generatequantitative information, whilst SIMS would providequalitative clues with respect to the chemistry. Anexample of this is where XPS has successfully detectedand quantified silicon on a surface which is notresponding well to bonding with an adhesive, but thechemical form that the silicon is in is not readily apparent,i.e., it could be silica, silicate or silicone. Analysis of thesame surface by static SIMS enables the mass spectrumof the sputtered top layer fragments to be determinedand the presence of m/e ions at 43, 73 and 147 confirmthat a polydimethyl siloxane is present.

12 Failure Diagnosis

It is an unfortunate fact that plastic products fail inservice. One of the major reasons for this is an incorrect

formulation of the product initially, which is atechnological failing, the other is where the formulationis correct for the application, but where there has beena problem in the mixing/processing side, leading to aproduct that does not meet the specification. Analysingthe plastic component can be useful in failure diagnosis.

12.1 Common Compositional Problems

If it is suspected that the composition of the product isnot correct, for example that the antioxidant or correctcure system has not been incorporated into thecompound, then the appropriate species specific teststhat have been discussed earlier can be carried out. Ifpossible, it is advisable to conduct the analysisalongside that of a sample known to be of the correctcomposition. This ensures that no product specificmatrix effects/interference reactions affect the dataobtained and hence the conclusions reached.

A surprisingly large number of failure problems can besolved by carrying out a simple series of tests including apolymer identification check by IR, a bulk compositionalanalysis by TGA and a molecular weight determination.

Molecular weight determination is very important in thecase of plastics because of the wide use (sometimesunauthorised) of regrind material. Unfortunately, thequality of regrind plastic can vary greatly due to thedegradation, and hence reduction in molecular weightand associated physical properties, that a plasticundergoes when it is reground. This depends greatly onthe conditions (e.g., heat and time of heating) that it issubjected to during the regrinding process. Also, if amaterial already contains a proportion of regroundmaterial the onset of degradation can be accelerated bystructural anomalies already present in the polymer. Thewidespread applicability of GPC to determine themolecular weight distribution of the majority of commonplastics makes it the perfect technique to investigate ifregrind is in a sample. Although small amounts (e.g.,5%) of reasonably high quality regrind can be hard tospot, any significant amount will reveal itself by a shiftin the distribution towards the low molecular weight end.As usual with GPC, the availability of reference samplesis important as the technique is mainly comparative.

Most of the failures that are associated with the use ofeither some or too much regrind are related to a reductionin the strength properties of the plastic, but anotherreasonably common type of failure is odour, especiallyin packaging applications. This odour is invariably dueto oxygenated degradation products of the plastic andcan be detected and analysed by headspace GC-MS.


37

12.2 Environmental Stress Cracking

Environmental stress cracking (ESC) is the prematureinitiation of cracking and embrittlement of a plasticdue to the simultaneous action of stress and strain andcontact with specific fluids. It is estimated that 15% ofall plastic component failures are due to ESC. Thesource of stress is often that which is unavoidablyprocessed in during moulding and so an applied stressis not a pre-requisite. The fluid is sometimes that forwhich the component was designed to contain orconduct, but it is often supplied by such agencies asadhesives, paints, cleaning agents and inks.

Because this type of failure is associated with relativelymobile (i.e., low molecular weight) liquids which arenormally present in small concentrations the techniqueof GC-MS is very well suitable to its investigation. Aparticularly effective approach is dynamic headspaceGC where any stress cracking fluid can be removedfrom the plastic matrix without the use of anothersolvent and long heating times enable it to beconcentrated up to aid detection. An area of plastic thathas not stress cracked can be used as a control.

There are cases where stress cracking can occur due tothe migration of a less volatile liquid (e.g., a plasticiser).An example of such a case is the stress cracking ofABS due to the migration of plasticiser from PVC, andthis can be approached by the detection of phthalate inthe ABS matrix by solvent extraction and then analysisof the extract using HPLC.

Where the liquid is relatively non-volatile and complexin composition (such as silicone oil which causescracking of polyethylene) again a solvent extractiontechnique has to be performed with either infraredmicroscopy analysis of a cast micro-film or a liquidchromatography method (i.e., LC-MS or HPLC) as theanalysis technique.

A review of the environmental stress cracking ofplastics has been produced by Wright (315).

12.3 Contamination Problems

Plastic products can fail, both aesthetically andphysically, because of contaminants. Chemicalresistance and electrical failure are less likely causesof failure as this type of contaminant is not usuallypresent at a high enough concentration.

Contamination can enter the product stream either inthe ingredients used in the production, or during the

manufacturing stage (e.g., mixing, extruding ormoulding).

More often than not this contamination is in the formof solid, discreet entities which makes their removalfrom the product relatively easy. Once removed themicroscopic techniques IR and Edax are excellent atobtaining assignment data in a cost effective way.Where enough of the contaminant is obtainable (e.g.,1 mg), and if a mixture of chemicals is suspected, abulk composition by TGA can be obtained. Ifidentification problems are still occurring, moresophisticated techniques such as GC-MS, SIMS andLIMA can be employed. Where the contamination isin a liquid form, a similar analytical regime can be used.A number of plastic products can suffer from solidinclusions, but it is probably most common in extrudedproducts such as car door seals.

It is also possible to use a Raman microscope systemfor the analysis of contaminants in plastic materials(293). One situation where the technique is particularlyuseful is in the identification of very small (e.g., a fewmicrometers in diameter) polymer gel inclusions withinthe same polymer matrix. Often these gels have a higherdegree of crystallinity and Raman spectroscopy withits high spatial resolution and ability to differentiatebetween difference degrees of crystallinity is the idealtechnique to differentiate between these andcontamination by a foreign material.

Contamination of plastics products by a species at alow level (i.e., less than 1% or at ppm levels) cansometimes be important, for example if a product is tobe used in the pharmaceutical industry. If it is suspectedthat the contaminant is, or contains, a metal, then AAScan be employed. If the presence of an organic moleculeis suspected, then headspace GC-MS can be used toidentify and quantify the species. The high sensitivityof this technique normally makes the use of a controlsample extremely important for a quick interpretationof the output, which is often complex.

12.4 Odour and Emissions Problems

The continuing drive to improve customer care and thehigh profile of health and safety issues, has led topressure on the suppliers of plastics components tocertain industries to minimise odours, and volatiles ingeneral, from their products. This is particular true ofthe automotive industry.

There are a number of specific tests that automotivecompanies insist that plastics components manufactured


38

by suppliers have to pass. An example of such a test isthe VW emissions test which involves placing thecomponent in a cell of given dimensions and heatingthe cell for a given time and a specified temperature.Rather than carry out a detailed analysis of thecomponents liberated from the component, the result isexpressed in terms of ppm of total organic compoundsas determined by an organic vapour analyser (OVA).Limits are given as to the permissible concentrations.

For quality control purposes it is the case at presentthat human smell panels will be used in preference toinstrumental analytical techniques which do not yetadequately mimic the human response. There arepractical drawbacks to this approach, leading to a lotof research going into ‘electronic noses’ utilising anumber (e.g., 32) of sensors based on organicconducting polymers. These devices enable fingerprintsof satisfactory products to be recorded which are usedas references for quality checks.

Work has been carried out to determine the additiveswhich contribute the most to the overall odour of plasticproducts. One of the most useful techniques isheadspace GC-MS. It is advisable to use the dynamicform of headspace sampling as this enables the volatilesfrom the sample to be concentrated. This benefit isimportant as some chemical species can cause an odourproblem at very low levels due to the specific sensitivityof the human nose.

For this type of work the dynamic headspace sampler(e.g., the Perkin Elmer ATD 400) is operated in adiffusion mode where the sample is heated at arelatively low temperature (e.g., 50 °C), which helpsto ensure that additional volatile species are notgenerated due to degradation of the sample, for arelatively long period of time (e.g., in excess of 30minutes). The odour species collected in the trap ofthe dynamic headspace sampler can then be analysedunder the following conditions:

Headspace trap injection temperature: 200 °C

GC column type: SGE RTX5 MS 30 m x0.25 mm, 0.25 µm film

GC column temperature –30 °C to 50 °C at 5 °C/min and then 20 °C/min

(cryogenic cooling) to 320 °C.

MS conditions 20 to 450 atomic mass unitsscanned every 0.33 s

13 Conclusion

This review describes the analysis of plastics, plasticcompounds and plastic products in as comprehensivea way as is possible within the format of a RapraReview Report. The abstracts from the RapraPolymer Library and the additional readingreferences provided should greatly assist the analystwho requires more information on recentdevelopments.

For the future, the reduction in cost of LC-MSsystems will increase their accessibility and, incombination with GC-MS, will greatly improve theefficiency and accuracy with which the analysis ofantidegradants, cure systems, plasticisers and otheradditives can be carried out. The combination ofthese two instruments will enable the full spectrumof polarity and molecular weight to be covered andenable a quantum leap in capability to be achievableby all analytical laboratories. Experiments which foryears have had to be carried out by TLC because ofthe limitations of conventional HPLC instrumentswill now be carried out by LC-MS.

The specific analysis techniques SIMS, XPS andLIMA are becoming increasing routine and, as aresult, cost effective for consultants to use incharacterisation and failure diagnosis work andtherefore an expansion of their use is guaranteed.

In the thermal analysis field, a number ofdevelopments have occurred in recent years, withmodulated temperature forms of TGA, DSC andTMA being brought out by manufacturers.Modulating the temperature enables these techniquesto deliver better, more informative data on samples.Another development within the thermal analysisgroup is the micro-thermal analysis (micro-TA)instrument. This technique combines thetopographical mapping capabilities of a scanningprobe microscope with the ability to performlocalised thermal analysis (DTA and TMA) on amicron scale. The instrument is also capable of beingconnected to a GC-MS via a heated interface for thechemical identification of specific features.

It is clear that, even with the development of newand more advanced techniques, the analysis of plasticcompounds and products will continue to present thepolymer analyst with complex and difficultchallenges.


39

Additional References

a.1 Surface Characterisation of AdvancedPolymers, Eds., L. Sabbatini and P.G.Zambonin, Wiley-VCH, 1993.

a.2 G. Lawson and J. Sidwell, Plastics and RubberInternational, 1983, 8, 6, 15.

a.3 J.L. Koenig, Spectroscopy of Polymers,Elsevier, 1999.

a.4 T.R Crompton, Manual of Plastics Analysis,Plenum, 1998.

a.5 T.R. Crompton, Practical Polymer Analysis,Plenum Press, 1993.

a.6 Polymer Spectroscopy, Ed., A.H. Fawcett,Wiley, 1996.

a.7 J. Haslam, H.A. Willis and D.C.M. Squirrell,Identification and Analysis of Plastics, 2nd

Edition, Butterworth, 1972.

a.8 P.J. Wyatt, Analytica Chimica Acta, 1992,272, 1.

a.9 D.O. Hummel, Atlas of Polymer and PlasticsAnalysis, Volume 2, Carl Hanser Verlag, 1984.

a.10 H.B.S Conacher and B.D. Page, Journal ofChromatographic Science, 1979, 17, 188.

a.11 P. Tittareli, T. Zerlia, A. Colli and G. Ferrari,Analytical Chemistry, 1983, 55, 220.

a.12 F. Lafferty and D.B. Stauffer, Wiley/NBSRegistry of Mass Spectral Data, John Wiley &Sons, 1989.

a.13 J. Udris, Analyst, 1971, 96, 130.

a.14 A. Groagova and M.A. Pribyl, AnalyticalChemistry, 1968, 234, 423.

a.15 F. Belpaire, Revue Belge des MatieresPlastiques, 1965, 6, 201.

a.16 D. Simpson and B.R. Currell, Analyst, 1971,96, 515.

a.17 L.N. Mal’kova, A.I. Kalanin and E.M.Derepletchikova, Zhurnal AnaliticheskoiKhimii, 1972, 27, 1924.

a.18 E. Schroeder and K. Thinius, Deutsche FarbenZeitschrift, 1960, 14, 146.

a.19 E. Schroeder and S. Malz, Deutsche FarbenZeitschrift, 1958, 5, 417.

a.20 Practical Surface Analysis, Eds., D. Briggs andM.P. Seah, John Wiley and Sons, 1988.

a.21 Handbook of X-Ray PhotoelectronSpectroscopy, Ed., G.E. Muilenberg, PerkinElmer Corporation, Eden Prarie, MN, 1979(update 1992-95).

a.22 D. Brigg, A. Brown and J.C. Vickerman, ALibrary of Standard Static SIMS Spectra,Wiley, 1989.


40


41

Appendix 1

Solubility Parameters of Plastics, Plasticisers and Typical Solvents

scitsalpfosretemarapytilibuloS

epyTcitsalP retemaraPytilibuloS

EFTP 2.6

EFTCP 2.7

enelyhteyloP 0.8

enelyporpyloP 0.8

yloP t etalyrcahtemlytub- 3.8

yloP n etalyrcahtemlyxeh- 6.8

yloP n etalyrcahtemlytub- 7.8

etalyrcalytubyloP 8.8

etalyrcahtemlyhteyloP 0.9

enerytsyloP 2.9

etalyrcahtemlyhtemyloP 2.9

CVP 5.9

etanobracylopAlonehpsiB 5.9

edirolhcenedilynivyloP 2.21-8.9

esolulleclyhtE 3.01-5.8

etartin-idesolulleC 55.01

TEP 7.01

sremyloplatecA 1.11

etateca-idesolulleC 53.11

6,6nolyN 6.31

lyhtemyloP α etalyrcaonayc- 1.41

elirtinolyrcayloP 1.41

sresicitsalpfosretemarapytilibuloS

resicitsalP retemaraPytilibuloS

sliociniffaraP 5.7

sliocitamorA 0.8

etapidalytcoiD 7.8

etacabeslytcoiD 7.8

etalahthplycediD 8.8

etacabeslytubiD 9.8

etalahthplytcoiD 9.8

etalahthplyhteyxotub-2iD 3.9

etalahthplytubiD 4.9

etahpsohplynehpirT 8.9

etahpsohplylotirT 8.9

etahpsohplylyxirT 9.9

rehtelyznebiD 0.01

etalahthplyhtemiD 5.01


42

stnevlosfosretemarapytilibuloS

tnevloS retemaraPytilibuloS

enatnep-oeN 3.6

n enaxeH- 6.6

rehtelyhteiD 4.7

enoteklyporposi-iD 0.8

enaxehocyC 2.8

ces etatecalymA- 3.8

edirolhcartetnobraC 6.8

enidirepiP 7.8

enelyX 8.8

rehtelyhtemiD 8.8

eneuloT 9.8

enaporporolhciD-2,1 0.9

FHT 1.9

etatecalyhtE 1.9

enezneB 2.9

mroforolhC 3.9

)KEM(enoteklyhtelyhteM 3.9

enelyhteorolhcirT 3.9

enelyhteorolhcarteT 4.9

enahteorolhcirT 6.9

)MCD(enahtemorolhciD 7.9

enonaxeholcyC 7.9

edirolhcidenelyhtE 8.9

N,N edimatecalyhteiD- 9.9

enotecA 9.9

o enezneborolhciD- 0.01

ediflusidnobraC 0.01

N,N edimamroflyhteiD- 6.01

n lonatuB- 4.11

lonaxehocyC 4.11

elirtinotecA 9.11

N,N edimamroflyhtemiD- 1.21

dicacitecA 6.21

lonahtE 7.21

edixofluslyhtemiD 9.21

dicacimroF 5.31

lonahteM 5.41

lonehP 5.41

locylgenelyhtE 6.41

lorecylG 5.61

retaW 4.32


43

Appendix 2

Specific Gravities of Plastics and Compound Ingredients

sremylopfoseitivargcificepS

remyloP ytivarGcificepS

enelyhteylopytisnedwoL 29.0

enelyhteylopytisnedhgiH 69.0

enelyporpyloP 09.0

edirolhclynivyloP 14.1

EFTP 2.2

EFTCP 1.2

ediroulfenedilynivyloP 5.1

edirolhcenedilynivyloP 7.1

enerytsyloplatsyrC 50.1

enerytsyloptcapmimuideM 50.1

enerytsyloptcapmihgihyreV 20.1

NAS 60.1

SBAtcapmimuideM 70.1-40.1

SBAtcapmihgiH 40.1-10.1

SBM 01.1-70.1

etalahthperetenelytubyloP 13.1

etalahthperetenelyhteyloP 73.1

nisercilonehpesopruplareneG 53.1

nisercilonehp-enimaleM 6.1-5.1

edyhedlamrof-aerU 6.1-5.1

enoflusyloP 42.1

etanobracyloP 2.1

edixoenelynehpyloP 60.1

remylopomohlatecA 34.1

remylopoclatecA 14.1

edimiyloP 24.1

6,4nolyN 81.1

6,6nolyN 41.1

6nolyN 31.1

01,6nolyN 90.1

21,6nolyN 70.1

11nolyN 40.1

21nolyN 20.1


44

stneidergnignidnuopmoccitsalpfoseitivargcificepS

tneidergnI ytivarGcificepS

etacilismuinimulA 01.2

edixoirtynomitnA 04.5

nemutiB 40.1

etaflusmuiraB 03.4

etacilismuiclaC 01.2

kcalbnobraC 08.1

xawabuanraC 99.0

yalcanihcdeniclaC 05.2

)niloak(yalcanihC 06.2

erbifnottoC 50.1

locylgenelyhteiD 21.1

etihparG 40.2

edixonorI 1.5-5.4

nilonaL 80.1

)emil(edixomuiclaC 91.2

egrahtiL 03.9

edixomuisengaM 06.3

etanobracmuisengaM 12.2

aciM 08.2

liolareniM 19.0

dicacielO 09.0

lioniffaraP 08.0

xawniffaraP 09.0

nisoR 70.1

aciliS 59.1

dicaciraetS 58.0

rufluS 50.2

)etacilismuisengam(claT 08.2

)esatana(edixoidmuinatiT 09.3

)elitur(edixoidmuinatiT 02.4

etanobracmuiclaC 56.2

edixocniZ 55.5

etaraetscniZ 01.1


45

Abbreviations and Acronyms

AAS atomic absorption spectroscopy

ABS acrylonitrile-butadiene-styrene

amu atomic mass units

APCI atmospheric pressure chemical ionisation

API atmospheric pressure ionisation

ATR attenuated total reflectance

BS British standard

DCM dichloromethane

DMTA dynamic mechanical thermal analysis

DOP dioctyl phthalate

DSC differential scanning calorimetry

Edax energy dispersive analysis

EI electron ionisation

ELS evaporative light scattering

EPA Environmental Protection Agency (US)

ESC environmental stress cracking

ESI electrospray ionisation

EVA ethylene-vinyl acetate copolymer

FID flame ionisation detector

FT Fourier transform

FTIR Fourier transform infrared spectroscopy

GC gas chromatography

GC-MS gas chromatography-mass spectrometry

GPC gel permeation chromatography

HDPE high density polyethylene

HIPS high impact polystyrene

HPLC high performance liquid chromatography

ICP inductively coupled plasma

IR infrared spectroscopy

ISO International Standards Organisation

KE kinetic energy

LALLS low angle laser light scattering

LAMMS laser microprobe mass spectroscopy

LC-MS liquid chromatography-mass spectroscopy

LDPE low density polyethylene

LIMA laser induced mass analysis

LLDPE linear low density polyethylene

MALLS multi-angle laser light scattering

MBS methylmethacrylate-butadiene-styrene


46

MEK methyl ethyl ketone

micro-TA micro-thermal analysis

Mn number average molecular weight

MSD mass selective detector

Mw weight average molecular weight

Mz Z average molecular weight

NIH National Institute of Health (US)

NIST National Institute of Standards and Technology (US)

NMR nuclear magnetic resonance

NPD nitrogen/phosphorus detector

OVA organic vapour analyser

PE polyethylene

PET polyethylene terephthalate

PMMA polymethylmethacrylate

PP polypropylene

PTFE polytetrafluoroethylene

PVC polyvinyl chloride

Rf Rf value is defined as ‘the distance from the start line on the plate to the analyte spot afterdevelopment, divided by the distance from the start line to the solvent front’ and is reasonablyconstant for a given TLC plate type and developing solvent

RI refractive index

SAN styrene-acrylonitrile copolymer

SEM scanning electron microscope

SFC supercritical-fluid chromatography

SIMS secondary ion mass spectrometry

SML specific migration limits

TAC triallyl cyanurate

TAIC triallyl isocyanurate

TEM transmission electron microscopy

Tg glass transition temperature

TGA thermogravimetric analysis

THF tetrahydrofuran

TLC thin layer chromatography

Tm melting temperature

TMA thermomechanical analysis

UV ultraviolet

VA vinyl acetate

Vis visible light

XPS X-ray photoelectron spectroscopy

XRD X-ray diffraction

XRF X-ray fluorescence

References and Abstracts

© Copyright 2002 Rapra Technology Limited 47

Abstracts from the Polymer Library Database

Item 1Polymer Testing21, No.5, 2002, p.591-5SPECTROSCOPIC BEHAVIOUR OF POLYVINYLALCOHOL FILMS WITH DIFFERENTMOLECULAR WEIGHTSAbd El-Kader K M; Orabi A SSuez Canal,University

Details are given of the preparation of PVAL films by acasting technique. Optical absorption and transmissionmeasurements were performed. The identification ofmolecular structures and assignments of energy bandswere also studied using FTIR and NMR. Correlationsbetween refractive index and molecular weight wereinvestigated. 17 refs.EGYPT

Accession no.856878

Item 2International Journal of Polymeric Materials51, No.4, 2002, p.315-23EFFECTS OF CURING TEMPERATURE ONPOLY(ETHYLENE TEREPHTHALATE)Al-Raheil I AMu’tah,University

The effect of cure temperature over the range from 280to 350C on PETP was investigated and changes in polymerstructure analysed by various techniques, including DSC,TGA, scanning electron microscopy and hot-stagemicroscopy. Changes in the crystallisation behaviour ofPETP at the different cure temperatures and themorphology of the PETP spherulites are discussed andmelting data of the melt crystallised PETP at 215C arepresented. 16 refs.JORDAN

Accession no.856733

Item 3Journal of Applied Polymer Science84, No.8, 23rd May 2002, p.1524-32KINETIC STUDY OF HINDERED AMINE LIGHTSTABILIZER UNDER NATURAL WEATHERINGCONDITIONSKaci M; Hebal G; Benhamida A; Boukerrou A;Djidjelli H; Sadoun TBejaia,University

The photografting kinetics of a hindered amine lightstabiliser (HALS) containing a polymerisable double bondin low density polyethylene (LDPE) films was studiedunder natural weathering conditions. The HALS (PBH-3, chemical structure shown) was added to the polymerat a concentration of 0.3 wt.%. The photografting kinetics

were determined by spectroscopic measurement of theabsorption band area of the stabiliser around 308 nm inthe UV spectra and 1605 cm -1 in the FTIR spectra,corresponding to benzylidene malonate and benzylidenemalonic groups respectively. Parallel measurements onthe free PBH-3 content after chloroform extraction of thephotostabiliser from the polymer matrix by UV and gaschromatography showed that in natural weatheringgrafting took place in the LDPE film after very shortexposure times of 127 and 168 hours as indicated by UVand FTIR respectively. The curves for the photograftingand the free HALS kinetics were similar. Thephotografting mechanism was thought to involve a quickphotoreaction between the methylene double bond of thestabiliser and the polymer macroalkyl radicals, withconsequent formation of polymer-bonded aminylstabiliser derivatives. 24 refs.ALGERIA

Accession no.853710

Item 4Polymer Bulletin48, No.1, March 2002, p.43-51PYROLYSIS OF GAMMA-IRRADIATEDBISPHENOL-A POLYCARBONATENavarro-Gonzalez R; Coll P; Aliev RCNRS; Mexico,Universidad Nacional Autonoma

This work shows the application of quantitative pyrolysis-gas chromatography coupled with infrared spectroscopyand electron impact mass spectrometry in the study ofradiation-induced scission of bisphenol-A polycarbonate(PC). PC under vacuum was gamma-irradiated using a60Co source in the dose range from 0.125 to 1.0 MGy.This was followed by flash pyrolysis under an inertatmosphere observed by GC-FTIR-MS. Pyrolysis of theirradiated PC gave different products depending on thedose. Yields of carbon dioxide and methane decreasedwith dose whereas those of phenol and 4-methylphenolincreased. The yields of benzene and toluene wereunaffected by irradiation. Analysis of the products in thisstudy helped to infer two main pathways for the radiation-induced scission of PC that involve carbonate bondrupture or aliphatic-aromatic bond rupture. 30 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;MEXICO; WESTERN EUROPE

Accession no.853698

Item 5Journal of Polymers and the Environment8, No.4, Oct. 2000, p.167-74SENSITIVE ELECTROCHEMICAL IMPEDANCESPECTROSCOPY METHOD FOR DETECTIONOF POLYIMIDE DEGRADATION BY


48 © Copyright 2002 Rapra Technology Limited

MICROORGANISMSGu J-G; Cheng S-P; Liu J; Gu J-DShenyang,Agricultural University; Nanjing,University;Beijing,University of Aeronautics & Astronautics;Hong Kong,University

An electrochemical impedance spectroscopy method wasevaluated for monitoring the microbial degradation ofpolyimides for electronic packaging. A mixed culture offungi isolated from degraded polyimides was used as themicrobial inoculum and scanning electron microscopywas employed to examine fungi growing on the surfaceof the inoculated polyimides. The data from themicroscopic analysis was utilised to further support therelationship between changes in the impedance spectraand microbial degradation of the polyimide. 30 refs.CHINA; HONG KONG

Accession no.853552

Item 6PVC 2002: Towards a Sustainable Future. Proceedingsof a conference held Brighton, 23rd-25th April 2002.London, IOM Communications Ltd., 2002. Paper 14,p.157-65, 21cm, 012PLATE-OUT IN PVC EXTRUSIONGilbert M; Varshney N; Van Soom K; Schiller MLoughborough,University; Honeywell; Chemson(Institute of Materials)

The results are reported of a study of plate-out in PVCextrusion carried out using several analytical techniques,including DSC, SEM-EDX, FTIR spectroscopy and laserionisation mass spectrometry. A special die and calibratorunit developed to investigate plate-out are illustrated andthe reproducibility of the method evaluated. The effectsof water content and anti-plate-out additives, such asalumina and silica, on plate-out are discussed andmechanisms explaining the formation of plate-out areproposed. 11 refs.AUSTRIA; BELGIUM; EUROPEAN COMMUNITY; EUROPEANUNION; UK; WESTERN EUROPE

Accession no.852750

Item 7PVC 2002: Towards a Sustainable Future. Proceedingsof a conference held Brighton, 23rd-25th April 2002.London, IOM Communications Ltd., 2002. Paper 9,p.116-23, 21cm, 012DETERMINING THE LEVEL OF GELATION BYODSC ON PVC WINDOW PROFILESKlingenfuss H; Zahn ASueddeutsches Kunststoff-Zentrum(Institute of Materials)

The degree of gelation of PVC window profiles and ofweld beads was investigated using oscillating differentialcalorimetry (ODSC). Tests carried out on a PVC dry blendrevealed that this analytical technique was capable ofdetermining the degree of gelation of very small samples

and permitted the determination of gelation at every pointof the profile and weld without the need for calibrationsamples. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;UK; WESTERN EUROPE

Accession no.852745

Item 8Polymer International51, No.5, May 2002, p.379-85STUDIES OF CURE KINETICS OFPOLYISOIMIDE BY DIFFERENTIAL SCANNINGCALORIMETRY IN THE SOLID STATEKim Y J; Son G I; Kim J-HSung Kyun Kwan,University

Detailed kinetic studies of the thermal imidisation ofpolyisoimide by DSC are described. Both isothermal anddynamic methods were used to obtain kinetic parametersand a phenomenological rate equation for estimating thedegree of imidisation as a function of time. 15 refs.KOREA

Accession no.851649

Item 9Journal of Adhesion76, No.1, 2001, p.55-74EVALUATING CURE OF A PMDI-WOODBONDLINE USING SPECTROSCOPIC,CALORIMETRIC AND MECHANICALMETHODSHarper D P; Wolcott M P; Rials T GWashington State,University; US,Dept.ofAgriculture,Forest Service

The cure of polymeric diphenylmethane diiso-cyanate(pMDI)/wood bondline in a controlled saturatedsteam environment was monitored using micro-dielectricanalysis(micro-DEA). Saturated steam environments wereproduced between 110 and 140C. The degree of curecalculated from micro-DEA was a basis for furtherspectroscopic, calorimetric and mechanical evaluation.Interpretation of calorimetric and spectroscopic analysisrevealed a high consumption of isocyanate early in cure.Mechanical strength, however, as revealed by lap sheartests, did not develop until late in cure. Low lap shearstrengths and a plateau in conversion rates were detectedfor samples pressed at 110 and 120C. Several componentsof the analysis suggested that low temperature cure couldresult in crystal formation, leading to diffusion controlledcure. 24 refs.USA

Accession no.851472

Item 10Journal of Advanced Materials34, No.2, April 2002, p.33-7



DEGREE OF CURE, HEAT OF REACTION ANDVISCOSITY OF 8552 AND 977-3 HM EPOXYRESINSNg S J; Boswell R; Claus S J; Arnold F; Vizzini AUS,Naval Air Warfare Center; Maryland,University

The heat of cure, degree of cure and viscosity of two epoxyresins (Hexcel 8552 and Cytec Fiberite 977-3 HM) wereinvestigated using a modulated differential scanningcalorimeter and a rheometric digital analyser.Mathematical models were developed to correlate the rateof the degree of cure and the viscosity with the degree ofcure and used to predict the kinetic behaviour of the epoxyresins, which was then compared with that of Hercules3501-6. A comparison was also made of cure modelsdeveloped based on neat and prepreg forms of theviscosity data. 6 refs.USA

Accession no.850900

Item 11Polymers & Polymer Composites10, No.3, 2002, p.237-48CURE BEHAVIOUR AND STRUCTURE OFDICYANATE-EPOXY NOVOLAC BLENDSGuo B; Fu W; Jia D; Qiu Q; Wang LSouth China,University of Technology

The objectives of this work are to investigate the curebehaviour and structure of bisphenol A dicyanate-novolacepoxy blends. The cure characteristics were investigatedby gel time determination and dynamic DSC. To disclosethe structural differences between cured cyanate-novolacepoxy blends and more traditional cyanate-diglycidylether systems, FTIR investigations were performed onthe two kinds of blends, and in situ FTIR was used toexamine the Bauer mechanism. The effects of epoxyconcentration in the blend on the cure kinetics wasinvestigated using two blends with different molar ratios,and in situ FTIR. 33 refs.CHINA

Accession no.850546

Item 12Macromolecular Chemistry & Physics203, No.4, 15th March 2002, p.653-62MISCIBILITY AND CRYSTALLIZATIONBEHAVIOUR OF POLYETHYLENETEREPHTHALATE/POLYVINYLIDENEFLUORIDE BLENDSRahman M H; Nandi A KIndian Association for the Cultivation of Science

The miscibility of PETP and PVDF was studied. The Tg,melting point, the crystallisation temperature and thecrystallinity values of the blends of differentcompositions, prepared at different conditions weremeasured. The polymer-polymer interaction parameter

was measured from equilibrium melting point depressiondata. 50 refs.INDIA

Accession no.850061

Item 13Chichester, John Wiley & Sons, 1999, pp.xiv,409.23cm. 911MICROSTRUCTURAL CHARACTERISATIONOF MATERIALSBrandon D; Kaplan W DHaifa,Technion Institute

This unreferenced book describes the technical andtheoretical aspects of a wide range of techniques for studyingthe microstructure of materials, including X-ray and electrondiffraction; optical microscopy, including polarised opticalmicroscopy and interference microscopy; transmission andscanning electron microscopy; X-ray microanalysis; electronenergy loss spectroscopy; and surface analysis byphotoelectron spectroscopy, Auger electron spectroscopy,and secondary ion mass spectrometry. The techniques aredescribed from sample preparation through informationacquisition to interpretation of results. A final chapterdescribes the derivation of quantitative structural data fromthe results of these techniques. Examples used in thebook mainly involve highly ordered materials such asmetals and inorganic crystalline materials, but many ofthe techniques used are applicable to polymers. Problemsfor the reader are included.ISRAEL

Accession no.849739

Item 14Polimeros: Ciencia e Tecnologia11, No.4, Oct./Dec.2001, p.213-21PortugueseNEAR-INFRARED SPECTRA OFPOLYSTYRENE, POLY(METHYLMETHACRYLATE) AND POLYCARBONATEDe Araujo S C; Kawano YSao Paulo,Instituto de Quimica

The near-infrared (NIR) spectra of amorphous polymersPS, PMMA and polycarbonate (PC) are studied. Thetentative assignment of the overtone and combinationfrequencies is made using the curve fitting calculations andthe local mode theory. Anharmonicity correction andmechanical frequency are determined from a Birge-Sponerplot. A tentative assignment of stretch overtone frequencyof CH2 and CH functional groups of PS; CH3 and COfunctional groups of PMMA; and CH, CH3 and COfunctional groups of PC is made. An anharmonicitycorrection of 57 and 58 cm-1 is obtained for CH2 and CHstretch modes of PS; 59 and 9 cm-1 for CH3 and CO stretchmodes of PMMA; and 53, 59 and 10 cm-1 for CH, CH3and CO stretch modes of PC, respectively. 21 refs.BRAZIL

Accession no.849333



Item 15Macromolecules35, No.7, 26th March 2002, p.2667-75THERMAL PROPERTIES OF CROSS-LINKEDPOLYISOPROPYLACRYLAMIDE,POLYMETHACRYLIC ACID, THEIR RANDOMCOPOLYMERS, AND SEQUENTIALINTERPENETRATING POLYMER NETWORKSDiez-Pena E; Quijada-Garrido I; Frutos P; Barrales-Rienda J MCSIC

The thermal properties of polyisopropyl acrylamide,polymethacrylic acid, isopropyl acrylamide-methacrylicacid copolymers and their blends were investigated byDSC and TGA. The state of the water was studied on thebasis of DSC traces of swollen samples. The Tg of thesame series of materials was also measured. 64 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.849122

Item 16Applied Spectroscopy56, No.2, Feb.2002, p.187-91RAMAN MICROSCOPY AND MAPPING AS APROBE FOR PHOTODEGRADATION INSURFACE RELIEF GRATINGS RECORDED ONLAYER-BY-LAYER FILMS OF CONGO RED/POLYELECTROLYTEConstantino C J L; Aroco R F; He J A; Zucolotto Z; LiL; Olveira O N; Kumar J; Tripathy S KWindsor,University; Lowell,Massachusetts University

Raman microscopy, mapping and surface-enhancedRaman scattering techniques are applied to investigatethe degradation of Congo Red (CR) in a surface reliefgrating (SRG) recorded on electrostatically assembledlayer-by-layer film of CR alternated with polydimethyldiallylammonium chloride (PDAC). Photoinduceddegradation is suggested by a decrease in the Raman bandsassigned to CR with a concomitant increase in thebackground signal. More degradation is observed in thevalleys of the SRG, which correspond to the mostilluminated areas. In a line mapping across the SRG, theRaman intensity of CR bands follows the modulation ofthe grating, which indicates that photodegradation of CRcontributes at least partially to the SRG formation.Surface-enhanced resonance Raman scattering (SERRS)indicates that the phenyl ring groups are located at thefilm surface. Mapping of the Raman signal over manyperiods of SRG shows that, within the limits of detection,the chromophores appear to be oriented in much the sameway throughout the film. They have no preferredorientation in the peaks and valleys of the SRG after therecording process is completed. 23 refs.CANADA; USA

Accession no.848921

Item 17Injection Molding10, No.1, Jan. 2002, p.40-4THE MATERIALS ANALYST: PART 50. THECASE OF THE DISAPPEARING CONTAMINANTSepe MDickten & Masch Mfg.

A report is presented on the diagnosis of the failure of acomponent made from a 33% glass-reinforced nylon 66on the assembly line with the aid of DSC, thermalgravimetric analysis, which was utilised to determine fillercontent and type, X-ray fluorescence and IR spectroscopy.The analytical procedures employed indicated that failureof the component could be attributed to the presence ofchlorine probably arising from contamination of theprocess by PVC.USA

Accession no.848744

Item 18Journal of Polymer Science: Polymer Physics Edition40, No.5, 1st March 2002, p.434-53FREE VOLUME, GLASS TRANSITION, ANDDEGREE OF BRANCHING IN METALLOCENE-BASED PROPYLENE/ALPHA-OLEFINCOPOLYMERS: POSITRON LIFETIME,DENSITY, AND DIFFERENTIAL SCANNINGCALORIMETRIC STUDIESDlubek G; Bamford D; Rodriguez-Gonzalez A;Bornemann S; Stejny J; Schade B; Alam M A; Arnold MBristol,University; ITA Institut fuer InnovativeTechnologien GmbH; Martin-Luther-Universitat Halle

Results of the above studies are presented and arediscussed with particular reference to Tg and degree ofbranching, local free volume and degree of branching,local free volume and Tg, specific volume and degree ofbranching, and number density of holes and degree ofbranching. 56 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;UK; WESTERN EUROPE

Accession no.848572

Item 19Polymer Preprints. Volume 42. Number 2. Fall 2001.Proceedings of a conference held Chicago, Il., 7th-11thApril 2002.Washington, D.C., ACS,Div.of Polymer Chemistry,2001, p.13-4POSITRON ANNIHILATION SPECTROSCOPYAS A NOVEL SURFACE PROBE OF POLYMERSJean Y C; Zhang R; Mallon P; Chen H; Huang C-M; LiY; Zhang J; Huang Y Y; Sandreczki T C; Wu YMissouri-Kansas City,University(ACS,Div.of Polymer Chemistry)

Positron annihilation spectroscopy (PAS) is a special non-destructive evaluation (NDE) technique for materials



characterisation, which uses the positron (anti-electron).Positron-electron annihilation gamma-rays reveal usefulinformation about the electronic and defect properties ofmaterials under study. The unique repulsive force betweenthe positron and the ion cores of materials makes thepositron ideal for probing defects at the atomic andmolecular levels. In recent years, PAS was developed as auseful tool to probe the microscopic properties of polymericmaterials. One of the great successes in this line of researchis the direct determination of polymer free volume and holeproperties at an atomic scale (0.2-2 nm). Most existing PASstudies emphasise the bulk of polymers in measuringpositron annihilation lifetime. Recently, another methodof positron annihilation radiation, Doppler broadening ofenergy spectra, coupled with a slow positron beam, hasbeen developed to examine the defect profile near thesurface. The results of experiments on the photodegradationof polymer-based coatings induced by 313 nm UVirradiation as studied by slow positron annihilationspectroscopy are reported and correlated with glossmeasurements. The sub-nanometer defect S parameter isfound to decrease with exposure time. Current resultssuggest that the slow positron technique is a sensitive toolfor detecting degradation of polymers in a time much earlierthan for any existing testing methods. It is particularlysensitive to the surface defect properties. Applications ofPAS to systems of polymers and fillers appear to beinteresting to investigate in the near future. 6 refs.USA

Accession no.847946

Item 20Adhesives & Sealants Industry9, No.1, Feb. 2002, p.38-40ENHANCED DSC INSTRUMENTATIONIMPROVES DESIGN ANDCHARACTERIZATION OF ADHESIVESCassel R BTA Instruments

The use of differential scanning calorimetry (DSC) for thecharacterisation and development of adhesive products isdiscussed. The Q Series DSC with Advanced TzeroTechnology from TA Instruments is described, withreference to the advantages it affords as a new and enhancedtool for improved design and characterisation of adhesives.The development incorporates a new measurementprinciple with an additional sensor that together providecompensation for intrinsic instrument distortion of the DSCsignal. With distortion virtually eliminated, it is possibleto measure specific-heat capacity directly in a single scan,and to achieve greater sensitivity and accuracy. Analysistime is also reduced, especially for modulated temperaturedifferential scanning calorimetry. It’s use in curing analysisof a two-part epoxy, and of pressure-sensitive adhesives isdemonstrated. 3 refs.USA

Accession no.847415

Item 21Macromolecules35, No.5, 26th Feb. 2002, p.1797-804LIQUID CHROMATOGRAPHY OF SYNTHETICPOLYMERS UNDER CRITICAL CONDITIONS.THE CASE OF SINGLE ELUENTS AND THEROLE OF THETA CONDITIONSMacko T; Hunkeler D; Berek DSwiss Federal Institute of Technology; SlovakAcademy of Sciences

PMMA, polybutyl methacrylates and polystyrenes invarious solvents were investigated with bare silica geland silica C18 bonded phases. The effect of variations ineluent nature on polymer retention is discussed. Criticalconditions were identified in some single eluents whichare thermodynamically poor solvents for the polymers.37 refs.SLOVAK REPUBLIC; SLOVAKIA; SWITZERLAND; WESTERNEUROPE

Accession no.847047

Item 22Macromolecules35, No.5, 26th Feb. 2002, p.1677-84LOW-TEMPERATURE CRYSTALLIZATION OFETHYLENE-RAN-PROPYLENE COPOLYMERS.CONFORMATIONAL REARRANGEMENT OFSEQUENCES DURING THE FORMATION OFTHE AGGREGATESBracco S; Comotti A; Simionutti R; Camurati I;Sozzani PMilan,University; Basell Spa

Low-temperature crystallisation of ethylene-propylenecopolymers was followed by DSC and solid-state NMR.The trans conformation fraction identifying the aggregateswas detected for all temperatures independent of thermalhistory. 41 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.847031

Item 23Macromolecular Materials and Engineering286, No.7, 27th July 2001, p421-8THERMOGRAVIMETRY OF THERMOPLASTICPOLYIMIDE POWDERS UNDER FOURDIFFERENT ATMOSPHERESXin-Gui Li; Mei-Rong Huang; He Bai; Yu-Liang YangTongji,University; Tianjin Customs Central Laboratory;Fudan,University

The high resolution thermogravimetry technique uses avariable heating rate response to changes in the weightloss rate to both reduce test times and improve definition.The thermal degradation of a thermoplastic polyimidepolymer in nitrogen, helium, argon and air was analysedusing both conventional and high resolution



thermogravimetric analysis techniques. It was concludedthat the thermal degradation results varied with bothatmosphere and test technique with the high resolutiontechnique providing more precise data in the inertatmosphere tests but less resolution in air.Thermogravimetric analysis data for a number ofpolyimide polymers is tabulated. The thermoplasticpolyimide polymer evaluated was more thermally stablethan many other polyimides. Complete details of the testtechniques are given with full discussion of the results.40 refs.CHINA

Accession no.846773

Item 24Journal of Applied Polymer Science83, No.12, 2002, p.2522-7CRYSTALLIZATION AND CROSSLINKING OFPOLYAMIDE-1010 UNDER ELEVATEDPRESSUREJun Yang; Wenfei Dong; Yucheng Luan; Jingjiang Liu;Shue Liu; Xingguan Guo; Xudong Zhao; Wenhui SuChangchun,Institute of Applied Chemistry;Jilin,University

This study looked at the structural changes to polyamide-1010 (PA1010) when it was treated at 250 degC for 30min at a pressure of 0.7-2.5 GPa. Crystals grew when thepressure was below 1.0 GPa or above 1.2 GPa.Crosslinking occurred in the pressure range 1.0-1.2 GPa.DSC and wide angle x-ray diffraction showed that PA1010lost its crystallisation ability after treatment at pressuresof 1.0-1.2 GPa. Crystallised PA1010 had a greater thermalstability than crosslinked PA1010 at 400 degC. 20 refs.CHINA

Accession no.846587

Item 25Kautchuk und Gummi Kunststoffe55, No.1-2, 2002, p.9-14GermanANALYSIS OF TECHNICAL POLYMER BLENDSWITH COUPLING OF LIQUIDCHROMATOGRAPHY WITH FTIRSPECTROSCOPYPasch H; Rode K; Kloninger C; Esser EDeutsches Kunststoff-Institut

The coupling of liquid chromatography with FTIRspectroscopy provides a new and interesting method forthe detailed analysis of complex polymer systems. Theapplication of this hyphenated technique to the analysisof polymer blends shows that it is possible to identify thedifferent blend components by their spectralcharacteristics. Components of different chemicalcompositions are determined selectively and theirchemical structure is analysed through well-resolvedFTIR spectra. For structure elucidation, all facilities of

state-of-the-art FTIR spectroscopy can be used. From thechromatographic and spectroscopic data, contourdiagrams are generated that present the molecularheterogeneity of the sample in the coordinates molar massand chemical composition. 17 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.846265

Item 26Polymer43,No.6,2002,p.1835-47THERMAL DEGRADATION OF PET ANDANALOGOUS POLYESTERS MEASURED BYTHERMAL ANALYSIS-FOURIER TRANSFORMINFRARED SPECTROSCOPYHolland B J; Hay J NBirmingham,University

The thermal degradation of two commercial PET samplesand two laboratory prepared polyesters, poly(ethyleneisophthalate) and poly(diethylene glycol terephthalate),was studied using thermogravimetry and thermal analysis-FTIR. The commercial PET samples were copolymerisedwith diethylene glycol and isophthalic acid groups indifferent proportions, and their thermal stabilities werefound to differ. Through a study of the thermal degradationof poly(diethylene glycol terephthalate) and poly(ethyleneisophthalate), it was found that diethylene glycol andisophthalate units promoted thermal degradation throughincreased chain flexibility and more favourable bondangles, respectively. The thermal degradation of all thepolyesters tested led to the formation of non-volatileresidue. IR spectroscopic analysis indicated that theresidue consisted almost exclusively of interconnectedaromatic rings. 21 refs.EU; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE; WESTERN EUROPE-GENERAL

Accession no.846155

Item 27Progress in Organic Coatings43, No.4, Dec.2001, p.226-32SIMPLE RAMAN TECHNIQUE TO MEASURETHE DEGREE OF CURE IN UV CURABLECOATINGSNichols M E; Seubert C M; Weber W H; Gerlock J LFord Research Laboratory

The curing of four UV-curable clearcoats was studied byconfocal Raman microscopy. The disappearance of theC:C line near 1636/cm provided the signature for thecuring of the samples, but quantification of the degree ofcure by standard peak fitting and baseline subtractionmethods did not work well because of samplefluorescence, baseline shifts and overlapping peaks. Asmoothed second-derivative processing approachovercame all of these difficulties and provided a simple,



rapid and objective quantification procedure. Steep curegradients through the thickness of the clearcoat, due toscreening of the bottom of the clearcoat by both the UVAand photoinitiator, were observed. Cure gradients at thetop of the clearcoat due to oxygen inhibition were alsoobserved. The most complete cure throughout the filmthickness was obtained with a mixture of standard andred-shifted photoinitiators. 9 refs.USA

Accession no.846135

Item 28Polymer43, No.5, 2002, p.1587-97FULL COPOLYMER CHARACTERIZATION BYSEC-NMR COMBINED WITH SEC-MALDIMontaudo M SCNR

Random copolymers with units of methyl methacrylate,butyl acrylate, styrene and maleic anhydride were studiedby fractionating the copolymer by size exclusionchromatography(SEC), collecting 30 to 40 fractions andthen recording both the NMR and MALDI spectra of thefractions. In a successive step, bivariate distribution ofchain sizes and composition maps were derived fromknowledge of the molar mass, weight and compositionof the copolymer fractions. The compositional distributionwas obtained by summation of the sections of the bivariatedistribution which belonged to a narrow compositionalrange. A model for SEC fractionation of copolymers wasdeveloped which allowed prediction of the compositionand D(x) of the SEC fraction, D(x) being the ratio betweenthe number-average and the weight-average molar mass,with x being the fraction number. Off-line SEC-MALDImeasurements were performed in order to measure D(x)experimentally for the random copolymers. 31 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.846119

Item 29Polymer Testing21, No.2, 2002, p.155-61BISPHENOL A-BASED POLYCARBONATES:CHARACTERIZATION OF COMMERCIALSAMPLESDelpech M C; Coutinho F M B; Habibe M E SRio de Janeiro,Universidade Federal; Rio deJaneiro,Universidade Estadual; Polialden Petroquimica SA

Samples of bisphenol A polycarbonate were characterisedby DSC, TGA, FTIR spectroscopy, size exclusionchromatography(SEC), vapour pressure osmometry(VPO) and viscometry. The samples exhibited the sameFTIR spectrum profile and almost the same values of Tgand initial temp. of degradation. Slight differences were,however, observed in differential TGA curves, whichcould be due to the presence of additives. The number-

average molec.wts. of the samples, as received andpurified, were determined by VPO in two differentsolvents, trichloromethane and THF. Viscometric averagemolec.wts. were obtained in trichloromethane at 25C. Fivedifferent equations were used to calculate intrinsicviscosities and viscometric constant values. Relativemolec.wts. and polydispersities were determined by SEC,in THF at 35C and in trichlorobenzene at 135C. It wasconfirmed that the results obtained in the latter solventwere in better agreement with those obtained by the othertechniques. 25 refs.BRAZIL

Accession no.845967

Item 30Plastics Engineering58, No.2, Feb. 2002, p.40/55PLASTICS ANALYSIS - THE ENGINEERSRESOURCE FOR TROUBLESHOOTINGPRODUCT AND PROCESS PROBLEMS ANDFOR COMPETITIVE ANALYSISEzrin MConnecticut,University

Methods for competitive analysis, troubleshooting processand product problems, plastics analysis, analysis of failedproducts and analysis of polymeric formulations arediscussed. Procedures covered include FTIR spectroscopy,Raman spectroscopy, NMR spectroscopy, surface analysisby spectroscopy, gas chromatography/mass spectrometry,atomic force microscopy and techniques for analysingunidentified formulations. 47 refs.USA

Accession no.845139

Item 31Journal of Applied Medical Polymers5, No.2, Autumn 2001, p.77-9NOVEL TECHNIQUE FOR THE DETECTION OFA HINDERED AMINE LIGHT STABILIZER,BASED ON SILICON TECHNOLOGYNarayan S; Lee R E; Hallberg D; Malatesta VGreat Lakes Chemical Corp.; Great Lakes ChemicalItalia

Details are given of the development of a novel methodto detect the presence of a hindered amine light stabiliserin PP, based on silicon technology. The method consistedof extracting the stabiliser from the PP matrix followedby detection and quantification using proton NMR. 3 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY; USA;WESTERN EUROPE

Accession no.844622

Item 32Adhasion Kleben & Dichten45, No.12, 2001, p.34-8German



NON-DESTRUCTIVE NUCLEAR MAGNETICRESONANCE CONTACT TECHNIQUE -EXAMPLES AND POSSIBILITIESHartwig A; Wolter BFraunhofer-Institut fuer Ang.Materialforschung;Bundesministerium fuer Wirtschaft; DECHEMA

On page 25 of the November 2001 issue of Adhaesion,Kleben & Dichten, the nuclear magnetic resonancecontact technique was introduced as a new sort of methodfor non-destructive characterisation of polymers. Thisarticle uses examples from the area of epoxy resins andthick-layer bondings to give an impression of typical,potential applications for this new non-destructive testingmethod. 2 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.844288

Item 33Applied Spectroscopy55, No.12, Dec.2001, p.1729-32FORENSIC ANALYSIS OF SINGLE FIBRES BYRAMAN SPECTROSCOPYMiller J V; Bartick E GWashington G.,University; US,FBI

Microscopical analysis by FT-IR spectroscopy has beenthe preferred method for obtaining additional informationon the polymeric composition of a fibre. It allowsunequivocal determination of the generic class andfrequently permits sub-classification. FT-IR analysiscannot be conducted while the fibre is mounted due tothe strong absorption of IR radiation by glass. The fibremust be removed from the slide and rinsed to clean offthe mounting medium before preparing the fibre. Thisincreases sample preparation time and the chance forsample loss. Glass produces little response to Ramanspectroscopy. Therefore, Raman analysis of fibres can beconducted while the fibre remains mounted on a glassslide under coverslips. The theoretical beam width of thelaser is 0.8 mu m; thus, Raman will potentially permitmeasurement of microfibres used in some fabrics in thecurrent market. The samples do not need to be thinned orflattened, as with IR, because the photons are scatteredfrom the surface and not transmitted through the sample.The current literature contains limited reports and citationson the use of Raman microprobe spectroscopy for forensicanalysis of fibres. It has previously been shown that it ispossible to scan fibres while they are taped onto a glassslide. By the same sample preparation method, it has beendemonstrated that it is possible to differentiate betweenseveral generic and sub-generic classes of fibres. It isillustrated that it is possible to scan through a glasscoverslip and mounting medium to obtain polymericidentification of non-dyed fibres. 14 refs.USA

Accession no.843701

Item 34Journal of Applied Polymer Science83, No.5, 31st Jan.2002, p.956-66SAFETY ASSESSMENT OF POLYMERICADDITIVES FOR FOOD PACKAGING:HYDROLYSIS OF POLYMERIC PLASTICISERSBY DIGESTIVE FLUIDSHamdani M; Thil L; Gans G; Feigenbaum A EInstitut National de la Recherche Agronomique; BASF AG

The safety of polymeric plasticisers capable of migratinginto food was assessed by an in vitro study of the hydrolysisof poly(1,2-propylene adipate) (PPA) by digestive fluidliquids. Freshly prepared simulated intestinal fluid solutionsproduced a high degree of hydrolysis. As indicated by highperformance size exclusion chromatography, the bulkplasticiser disappeared completely, and low molecularweight oligomers were produced within 4 hours. Gas-phasechromatography indicated no significant conversion to freemonomers after hydrolysis, and NMR tests showed thatthe cleavage selectivity occurred selectively at primary esterlinkages. Silica gel fractionation of the hydrolysate gavesix oligomeric fractions, which were recovered andanalysed. Proton NMR was used to evaluate the absolutemolecular weight of the plasticisers and the hydrolysisproducts. Under simulated gastric and saliva conditions thedegree of hydrolysis was less than 2%. 3 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;GERMANY; WESTERN EUROPE

Accession no.842741

Item 35Journal of Applied Polymer Science81, No.7, 15th Aug.2001, p.1588-94CHARACTERIZATION OF BRANCHEDPOLYMERS BY SIZE EXCLUSIONCHROMATOGRAPHY COUPLED WITHMULTIANGLE LIGHT SCATTERINGDETECTOR. I. SIZE EXCLUSIONCHROMATOGRAPHY ELUTION BEHAVIOR OFBRANCHED POLYMERSPodzimek S; Vlcek T; Johann CWyatt Technology Corp.; Pardubice,University; WyattTechnology Deutschland GmbH

The elution behaviour of randomly branched PS and star-branched poly(benzyl methacrylate) with different levelsof branching was studied by size exclusionchromatography (SEC) coupled with a multiangle lightscattering detector. The highly branched polymers showedabnormal SEC elution behaviour. After normal elution atsmall elution volumes, the molar mass and root meansquare radius of the eluting molecules increased withincreasing elution volume. Reasons for this were exploredand discussed. SEC separation was compared withseparation by thermal field flow fractionation. 8 refs.CZECH REPUBLIC; EUROPEAN COMMUNITY; EUROPEANUNION; GERMANY; USA; WESTERN EUROPE

Accession no.842695



Item 36Revista de Plasticos Modernos81, No.538, April 2001, p.461-6SpanishAPPLICATION OF INFRARED SPECTROSCOPYAND THERMAL ANALYSIS IN MONITORINGTHE CURE OF THERMOSETTING RESINSUSED IN THE AIRCRAFT INDUSTRYSanchez-Blazquez ACASA

The amine cure of Hexcel 8552 epoxy resin, for use asthe matrix in carbon fibre-reinforced composites forapplication in aircraft construction, was monitored bynear-infrared spectroscopy. This technique was validatedby comparison of the results with those obtained bymodulated DSC. 18 refs.

HEXCEL COMPOSITESEUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.842573

Item 37Progress in Colloid & Polymer ScienceVol.117, 2001, p.167-71SURFACE CHARACTERISATION OFPOLYLACTIDE/POLYGLYCOLIDECOPOLYMERSKiss E; Lam C N C; Due T M; Vargha-Butler E IBudapest,Eotvos Lorand University;Toronto,University; Biophy Research

The wettability and the surface composition ofbiodegradable polymers used as drug delivery particlesare determined and compared. Films of polylactic acid,polyglycolic acid and their copolymers with four differentlactide, glycolide ratios of 85/15, 75/25, 65/35 and 50;50 are formed by solvent-casting on polar (silicone waferglass and silica) substrates. Advancing and receding watercontact angles are measured goniometrically and also byusing the automated axisymmetric drop shape analysismethod. Both the advancing and the receding watercontact angles of the copolymers are higher than expectedfrom the values obtained for the two homopolymersconsidering the increasing glycolide content of thecopolymers. Surface analysis of the polyester films isperformed by X-ray photoelectron spectroscopy at varioustake-off angles to get information on the depth distributionof the components. Surface enrichment of the nonpolar(lactide) component in the outermost layer of thecopolymer films is detected. The wettability behaviour isin accordance with the surface composition, resultssuggesting a surface activity effect resulting in theorientation of the nonpolar segments of the copolymerchains towards the surface of the film and hence producingmore hydrophobic character for the copolymer films thanshould be due to their bulk composition. 20 refs.

Accession no.842190

Item 38Synthetic Metals124, No.2-3, 22nd Oct.2001, p.407-14STUDY OF THE SURFACE POTENTIAL ANDPHOTOVOLTAGE OF CONDUCTINGPOLYMERS USING ELECTRIC FORCEMICROSCOPYBarisci J N; Stella R; Spinks G M; Wallace G GWollongong,University

The effect of the polymer composition, preparationmethod and nature of the substrate on the surface potential(SP) of conducting polymer films is investigated. Boththe average value and the distribution of SP across thepolymer surface are influenced by these factors.Polythiophenes, potentially useful for solar energyconversion, are used to examine the generation of light-induced changes in SP. Results suggest the possibility ofdetermining the local variations of the surfacephotovoltage and the photovoltaic properties of polymerfilms intended for use in photovoltaic devices. 16 refs.AUSTRALIA

Accession no.842093

Item 39Polymer Degradation and Stability75, No.1, 2002, p.185-91STUDY ON METHANOLYTICDEPOLYMERIZATION OF PET WITHSUPERCRITICAL METHANOL FORCHEMICAL RECYCLINGYong Yang; Yijun Lu; Hongwei Xiang; Yuanyuan Xu;Yongwang LiChinese Academy of Sciences

Polyethylene terephthalate (PET) was subjected tomethanolytic depolymerisation with supercriticalmethanol in a stirred stainless steel autoclave attemperatures of 523-543 deg.C, pressure 8.5-14.0 MPa,and a 3-8 methanol to PET weight ratio. The solid productsobtained, consisting mainly of dimethyl terephthalate andsmall amounts of methyl-(2-hydroxyethyl) terephthalate,bis(hydroxyethyl) terephthalate, dimers, and oligomers,were analysed by high performance liquidchromatography (HPLC), and the liquid products, mainlyethylene glycol and methanol were analysed by gaschromatography (GC). The temperature, weight ratio ofmethanol to PET, and the reaction time had a very markedeffect on dimethyl terephthalate yield and the degree ofPET depolymerisation, but the effect of pressure wasinsignificant above the methanol critical point. Theoptimum PET depolymerisation conditions were:temperature 533-543 K, pressure 9.0-11.0 MPa, and amethanol to PET weight ratio of 6-8. Thedepolymerisation of several PET wastes from the Chinesemarket was studied under the optimum conditions. 28 refs.CHINA

Accession no.841527



Item 40Polymer Degradation and Stability75, No.1, 2002, p.153-9THE EFFECT OF ULTRAVIOLET STABILISERSON THE PHOTODEGRADATION OFPOLY(ETHYLENE TEREPHTHALATE)Fechine G J M; Rabello M S; Souto-Maior R MPernambuco,Federal University; Paraiba,UniversidadFederal

The weathering behaviour of polyethylene terephthalate(PET) samples obtained by bi-axial tension in thelaboratory over a period of up to about 1100 hours wasstudied. The mechanical properties of films obtained fromthe samples having different types of UV stabilisers, e.g.a triazine ultraviolet absorber (Tinivin 1577), carbonblack, or a TiO2/BaSO4 mixture, were tested, and thefilms were examined by UV-VIS spectroscopy, titration,size exclusion chromatography, and FTIR. The resultsshowed that the unstabilised films were easily degraded,resulting in considerable deterioration in mechanicalproperties and a molecular weight decrease. The triazinewas the most effective stabiliser. 38 refs.BRAZIL

Accession no.841524

Item 41Polymer Degradation and Stability75,No.1, 2002, p.123-9INITIAL STEPS AND EMBRITTLEMENT INTHE THERMAL OXIDATION OF STABILISEDPOLYPROPYLENE FILMSFayolle B; Audouin L; Verdu JEcole Nationale Superieure des Arts et Metiers

Physicochemical and mechanical characterisationmethods were used to study the oxidation of 100 micronstabilised polypropylene films at 130 deg.C in air.Stabiliser consumption (UV spectrophotometry) andmolecular weight decrease (steric exclusionchromatography) could be observed during the inductionperiod, when no carbonyl build-up could be detected byIR spectroscopy. These structural modifications had aneffect on the fracture properties, as indicated by theessential work of fracture (EWF) method, whereas theultimate tensile elongation showed no significant changes.The results show that the EWF method is useful forcharacterising the degradation induced embrittlement ofinitially ductile polymers. The experimental data reportedsuggest that the problem of the spatial heterogeneity ofthe oxidation process requires further discussion. 21 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.841521

Item 42Biomaterials23, No.6, March 2002, p.1439-46

EFFECTS OF THE STERILISATION METHODON THE WEAR OF UHMWPE ACETABULARCUPS TESTED IN A HIP JOINT SIMULATORAffatato S; Bordini B; Fagnano C; Taddei P; Tinti A;Toni ABologna,Istituti Ortopedici Rizzoli; Bologna,Universita

Details are given of the effects of sterilisation methodson the wear and changes in physical properties of ultra-high molecular weight PE acetabular cups. Thecrystallinity of the cups was evaluated by micro-Ramanspectroscopy as a function of the inner surface position.The partial least square calibration was used to correlatethe Raman spectra with the crystallinity of the polymermeasured by DSC. 52 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.840964

Item 43Polymer Preprints. Volume 41. Number 2. Conferenceproceedings.Washington, D.C., 20th-24th Aug.2000, p.1792-3CHARACTERISATION OF PLANT FIBRES BYINFRA-RED SPECTROSCOPYGarside P; Wyeth PSouthampton,University(ACS,Div.of Polymer Chemistry)

The application of IR spectroscopy with respect to thecharacterisation of cellulosic (plant) fibres isdemonstrated. The ability to characterise fibres is ofimportance to textile conservators, as this information aidsin the determination of the age and origin of the artefactfrom which they are taken, and may influence the choiceof treatment. The fibres under examination are takenlargely from the bast group (flax, hemp, jute and ramie);in addition, sisal and cotton are compared. FT-IRmicrospectroscopy and ATR techniques are employed. Tocomplement the conventional use of these methods, theinherent polarisation effects of the equipment areexploited to record polarised IR spectra. Jute, sisal andcotton are readily differentiated, but flax, hemp and ramieprove more difficult to distinguish. Peak ratio techniquesare applied in the latter case. 2 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.840045

Item 44Journal of Coatings Technology73, No.923, Dec. 2001, p.43-50ON THE USE OF THE ATOMIC FORCEMICROSCOPE TO MONITOR PHYSICALDEGRADATION OF POLYMERIC COATINGSURFACESVanLandingham M R; Nguyen T; Byrd W E; Martin J WUS,National Inst.of Standards & Technology



Changes in the surface properties of a model thermosettingacrylic melamine polymeric coating system similar tosystems widely used as automotive clearcoats werefollowed using atomic force microscopy (AFM). Thesamples were exposed to a range of relative humidities,different temperatures and various UV wavelengths anda full factorial experimental design was utilised. Amechanism for the formation of pits in the surface of thecoatings, as observed by AFM, was developed and therelationship between the chemical and physicaldegradation of the coatings discussed. 21 refs.USA

Accession no.839365

Item 45Polymer Plastics Technology and Engineering40, No.5, 2001, p.767-81STABILISATION OF FREE RADICALS INFILLED OLIGOESTER ACRYLATESKadossov E B; Kovarski A L; Kasparov V V;Zapadinski B I; Tikhonov A PRussia,Academy of Science; Mendeleev University ofChemical Technology

The results are reported of a study of the formation anddecay of free radicals during the photocrosslinking of anoligocarbonate methacrylate filled with two types of silicadiffering in particle size or hydroxyapatite using ESRspectroscopy. The data are correlated with those obtainedfor molecular mobility using a spin probe and the kineticsof radical accumulation during photocrosslinking arediscussed along with the kinetics of termination ofradicals. 17 refs.RUSSIA

Accession no.839176

Item 46Revista de Plasticos Modernos81, No.537, March 2001, p.345-52SpanishANALYSIS OF SYNTHETIC POLYMERS BYCAPILLARY ELECTROPHORESISSimo C; Barbas C; Cifuentes AInstituto de Fermentaciones Industriales; San Pablo-CEU,Universidad

The principles of the various modes of capillaryelectrophoresis are examined, and applications of thesetechniques in the molecular weight characterisation ofpolymers are discussed. 40 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.839085

Item 47Applied Spectroscopy55, No.11, Nov. 2001, p.1514-22

RAMAN SPECTROSCOPY DETERMINATIONOF THE THERMOPLASTIC CONTENT WITHINEPOXY RESIN-COPOLYETHERSULFONEBLENDSvan Overbeke E; Devaux J; Legras R; Carter J T;McGrail P T; Carlier VLouvain,Universite Catholique; ICI

Details are given of the possibility of using Ramanspectroscopy to determine the local thermoplastic contentwithin an epoxy resin/copolyethersulphone blend. Therequired calibration of the Raman data is presented. Theapplicability of the calibrations to blends containingchlorine-ended copolyethersulphone is discussed. Resultsobtained with small or large Raman confocal holes werealso compared. 40 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; WESTERN EUROPE

Accession no.838755

Item 48Polymer Degradation and Stability74, No.2, 2001, p.321-6XPS CHARACTERIZATION OF FRIEDEL-CRAFTS CROSS-LINKED POLYSTYRENEJianqi Wang; Jianxin Du; Hongyang Yao; Wilkie C ABeijing,Institute of Technology; Marquette,University

The combination of a difunctional alkylating agent, eitherhydroxymethylbenzyl chloride or alpha,alpha’-dichloroxylene, with PS or high-impact PS together witha Friedel-Crafts catalyst, 2-ethylhexyldiphenylphosphate,and an amine for reaction with hydrogen chloride wasstudied by X-ray photoelectron spectroscopy. The resultsconfirmed the theories proposed from previousinvestigations using TGA, i.e. crosslinking of the polymeroccurred as the temp. was raised and the alcohol-containing alkylating agent gave a greater amount ofcrosslinking than did the dichloro compound. 13 refs.CHINA; USA

Accession no.838285

Item 49Macromolecular Chemistry & Physics202, No.16, 7th Nov. 2001, p.3228-33CHARACTERIZATION OF THECROSSLINKING KINETICS OF A THINPOLYMERIC LAYER BY REAL-TIMEDIELECTRIC RELAXATION SPECTROSCOPYSchonhals A; Fritz A; Pfeiffer KBerlin,University; Micro Resist Technology GmbH

The crosslinking kinetics of a thin polymeric layer on aprepolymer of a phthalic acid diallyl ester was studied byreal-time dielectric spectroscopy. Activation energies wereestimated for the reaction using the temperaturedependence of the time constant. The change of therelaxation rate of the dynamic Tg with the reaction timewas obtained from dielectric loss data. 20 refs.



EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.838158

Item 50LCGC Europe14, No.12, Suppl., Dec.2001, p.8/21CONSIDERATIONS ON COLUMN SELECTIONAND OPERATING CONDITIONS FOR LC-MSSandra P; Vanhoenacker G; Lynen F; Li L; Schelfaut MKortrijk,Research Institute for Chromatography;Ghent,University

Mass spectrometry is slowly, but surely becoming thedetection system of choice for liquid chromatographyanalysis in many areas. An overview is presented ofcolumn and mobile phase selection for LC-MS. Relativelysimple guidelines are advanced to successfully optimiseLC-MS for several applications. This article discusses thefundamentals of LC related to MS hyphenation, adaptingLC to LC-MS methods, normal-phase liquidchromatography, supercritical fluid chromatography,reversed-phase liquid chromatography, size exclusionchromatography, ion-exchange chromatography, affinitychromatography and capillary electrophoresis. 25 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;WESTERN EUROPE

Accession no.837996

Item 51Polymer42, No.20, 2001, p.8461-7STATES OF WATER IN DIFFERENTHYDROPHILIC POLYMERS - DSC AND FTIRSTUDIESPing Z H; Nguyen Q T; Chen S M; Zhou J Q; Ding Y DFudan,University; Rouen,University

Differential scanning calorimetry and Fourier transforminfrared spectroscopy techniques were used to study thestructure of water molecules in polyvinyl alcohol andpolyethylene grafted acrylate hydrophilic polymers.Varying amounts of water were added to test samples andthe samples conditioned to the sorption equilibrium statein sealed containers for 24 hours prior to evaluation. It wasconcluded that below a threshold water content, dependingon the polymers physical and chemical structure, watermolecules absorbed in hydrophilic polymer cannot formice crystals in the polymer matrix. Above this thresholdcontent, the water crystallises but below zero. It was alsodemonstrated that the absorbed water in hydrophilicpolymers develops differing hydrogen bonds in the firstand second hydration layers. It was concluded that thepotential influence of these intermolecular interactionsshould therefore be taken into account whenever a polymeris used with a solvent. 25 refs.CHINA; EUROPEAN COMMUNITY; EUROPEAN UNION;FRANCE; WESTERN EUROPE

Accession no.837027

Item 52Polymer42, No.20, 2001, p.8425-34PHYSICAL AND MECHANICAL PROPERTIESOF POLYETHYLENE FOR PIPES IN RELATIONTO MOLECULAR ARCHITECTURE. PART I.MICROSTRUCTURE AND CRYSTALLISATIONKINETICSHubert L; David L; Seguela R; Vigier G; Degoulet C;Germain YInstitute Nationale des Sciences Appliquees; Atofina

Five high density polyethylene bimodal copolymers withvarying molecular architectures designed for pipeapplications were tested to evaluate the relationshipsbetween structure properties contributing towardsimproved end use properties. Crystallisation kinetics werestudied in relation to molecular architecture usingchromatography, density columns, differential scanningcalorimetry, X-ray scattering, rising temperature elutionfractionation and infrared spectroscopy. From the testresults, it was concluded that the normal correlationbetween kinetics, molecular structure and moleculartopology found with unimodal copolymers does not applywith bimodal copolymers as the crystal surface free energywas sensitive to topological changes resulting fromarchitectural molecular changes. Complete details of theexperimental procedures and test results are given withextensive discussion of the background theory and results.60 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;FRANCE; WESTERN EUROPE

Accession no.837023

Item 53LCGC Europe14, No.9, Sept. 2001, p.564/9INVESTIGATION OF A NOVEL SOL-GELDERIVED STATIONARY PHASE FOR GASCHROMATOGRAPHYCervini R; Day G; Hibberd A; Sharp G; Froud ASGE International Pty Ltd.; SGE Europe Ltd.

The effectiveness of using a novel, sol-gel materialincorporating PEG or wax as a capillary column stationaryphase is described. Chromatograms demonstratinginertness, partitioning capability and robustness for arange of applications are presented. 10 refs.AUSTRALIA; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; WESTERN EUROPE

Accession no.836916

Item 54Polymer Engineering and Science41, No.10, Oct.2001, p.1714-30TEMPERATURE MODULATED DSC STUDIESOF MELTING AND RECRYSTALLIZATION INPOLY(OXY-1,4-PHENYLENEOXY-1,4-



PHENYLENECARBONYL-1,4-PHENYLENE)(PEEK)Kampert W G; Sauer B BDuPont Central Research & Development

The thermal and crystal morphological properties ofamorphous and melt-crystallised PEEK were investigated.Two different molec.wts. were studied by temp.-modulated DSC(TMDSC) over a broad range of annealingtimes and temps. The lower molec.wt. PEEK under allcrystallisation conditions was found to exhibit secondarycrystal melting in the low endotherm region, followed bymelting of primary crystals superimposed with a largerecrystallisation contribution. Primary crystal meltingbroadly overlapped with melting of the recrystallisedspecies and contributed to the broad highest endotherm.Recrystallisation contributions and the interpretation ofTMDSC were partially confirmed by independent rapidheating rate m.p. determinations and variable heating rateDSC. The higher molec.wt. PEEK showed manysimilarities but generally had smaller levels ofreorganisation above the annealing temp. under mosthigher temp. crystallisation conditions. TMDSC providedgood resolution of recrystallisation and related eventscompared with standard DSC. The broad and substantialexothermic recrystallisation in amorphous samples wasalso examined, showing that recrystallisation continuedthrough the final melting region. 42 refs.USA

Accession no.836355

Item 55Macromolecular SymposiaVol.174, Aug.2001, p.413-34STRATEGIES IN TWO-DIMENSIONAL LIQUIDCHROMATOGRAPHIC SEPARATION OFCOMPLEX POLYMER SYSTEMSBerek DSlovak,Academy of Sciences

The separation of complex polymer systems by two-dimensional liquid chromatography is discussed. Methodsare reviewed in which the effect of polymer molec.wt. onpolymer retention is suppressed. The resulting ‘oneparameter separation systems’ can be on-line or off-lineconnected to another separation system such as sizeexclusion chromatography in order to provide more detailedcharacterisation of complex polymers. Selected proceduresfor the re-concentration of diluted polymer solutions arealso considered. These could be used for increasing theconcentration of sample(s) leaving the first dimensionseparation column. Some arrangements for controlledsample re-introduction into the second dimensionseparation column are outlined. 48 refs. (World PolymerCongress, IUPAC MACRO 2000, 38th MacromolecularIUPAC Symposium, Warsaw, Poland, July 2000)SLOVAK REPUBLIC; SLOVAKIA

Accession no.836231

Item 56Revista de Plasticos Modernos81, No.536, Feb.2001, p.244-8SpanishPERMEABILITY OF METHANOL, TOLUENE,FUELS AND OXYGENATED FUELS IN ANETHYLENE-VINYL ALCOHOL COPOLYMERUSED AS A BARRIER COMPONENT TO GASES,AROMAS AND HYDROCARBONSLagaron J M; Powell A KJaume I,Universitat; BP Chemicals Ltd.

Measurements were made of the permeation rates ofmethanol, toluene, a 50/50 toluene/isooctane fuel (fuelC) and fuel C with 10% ethanol or 15% methanol throughEVOH films. Large scale methanol and water inducedplasticisation was suggested by large solvent uptakes andconfirmed by the observation of considerable decreasesin Tg. The permeability of fuel C increased significantlywhen methanol was present, while the high barrierproperties of EVOH to hydrocarbons was maintained forfuel C containing ethanol. 9 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;WESTERN EUROPE

Accession no.835449

Item 57Revista de Plasticos Modernos81, No.536, Feb.2001, p.236-43SpanishETHYLENE-VINYL ALCOHOL COPOLYMERSAND THEIR APPLICATIONS IN FOODPACKAGINGCerrada M LInstituto de Ciencia y Tecnologia de Polimeros

The gas barrier properties of ethylene-vinyl alcoholcopolymers are examined as a function of ethylene andvinyl alcohol content, and their use in combination withother plastics in films, bottles and other containers forfood packaging is discussed. Results are presented of astudy of the crystal structure of three copolymers havingdifferent compositions. 11 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.835448

Item 58Polymer Preprints. Volume 41. Number 2. Conferenceproceedings.Washington, D.C., 20th-24th Aug.2000, p.1423-4MAPPING CHEMICALLY HETEROGENEOUSPOLYMER SYSTEM USING CHEMICALMODIFICATION AND ATOMIC FORCEMICROSCOPYRaghavan D; Gu X; VanLandingham M; Nguyen TWashington,Howard University; US,National Inst.ofStandards & Technology



(ACS,Div.of Polymer Chemistry)

Interactions between a film and its external environmentare strongly influenced by the surface chemistry andmorphology of the film. Extensive research has beenconducted to provide in-depth microstructural informationof thin polymer films using analytical techniques such assmall-angle X-ray scattering, X-ray photoelectronspectroscopy, neutron scattering and secondary ion-massspec trometry. However, these techniques lack the lateralresolution to detect and map the heterogeneity in polymerfilms. With the advent of atomic force microscopy (AFM),it is possible to provide direct spatial mapping of surfacetopography and surface heterogeneity at nanometerresolution. A combination of tapping mode and forcemode AFM techniques has been effective in mappingmechanically heterogeneous regions in multi-componentpolymer systems. Recent developments in chemicallyfunctionalised AFM tips have allowed mapping ofchemically heterogeneous lithographically patternedsurfaces by AFM at the molecular scale. This techniqueis known as chemical force microscopy. However,mapping chemical heterogeneity in a polymer system bychemical force microscopy pose difficulties because ofchain length variation and irregular packing of chains atthe probe surface. The objective is to chemically degradeone component of a model blend and then identify thedegraded component by AFM. A model blend consistingof polyethylene acrylate (PEA) and PS is selected due tothe difference in the hydrolysis characteristics of PEAand PS. Acid is selected as the aggressive chemicalmedium so as to accelerate the hydrolysis of onecomponent in the model blend film. 9 refs.USA

Accession no.835296

Item 59Polymer Preprints. Volume 41. Number 2. Conferenceproceedings.Washington, D.C., 20th-24th Aug.2000, p.1409-10OVERVIEW OF STATE-OF-THE-ART SPM OFCRYSTALLINE POLYMERSMiles M J; Hobbs J K; McMaster T J; Baker A A;James P J; Blakely S T; Aissaoui M-NBristol,University(ACS,Div.of Polymer Chemistry)

Scanning probe microscopy is a family of a dozen or moremicroscopies essentially based on the concept andtechnology of the founding member, scanning tunnellingmicroscopy. The most appropriate and widely-used ofthese microscopies in the study of polymer systems isatomic force microscopy (AFM), which in many of itsmodes of operation is suitable for imaging relatively softsolids such as polymers and biological materials. In thesimplest AFM modes of operation (contact and ‘tapping’),topographic images representing the surface of thepolymer specimen can be obtained. At the lamellar crystallevel, such images have generally confirmed morphology

and crystalline structures deduced from transmissionelectron microscopy (TEM) or X-ray studies. However,the resolution of the AFM can go beyond that easilyachievable with TEM imaging of polymers. At higherresolution, AFM has, in some cases, revealed unpredictedsurface structures. 26 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.835289

Item 60Polymer43, No.1, 2002, p.159-70QUANTIFYING SHORT CHAIN BRANCHINGMICROSTRUCTURES IN ETHYLENE 1-OLEFINCOPOLYMERS USING SIZE EXCLUSIONCHROMATOGRAPHY AND FOURIERTRANSFORM INFRARED SPECTROSCOPY(SEC-FTIR)Deslauriers P J; Rohlfing D C; Hsieh E TChevron Phillips Chemical Co.

Ethylene-1-olefin copolymers are used to demonstrate anSEC-FTIR method for the analysis of short chainbranching distribution (SCBD) across the molecularweight distribution (MWD). The chromatograms wereobtained using the root mean square absorbance in the3000-2700 cm power -1 spectral range (with FTIR servingas a concentration detector). The spectra from individualtime sections of the chromatogram were then analysedfor comonomer branch levels using a chemometricmethod, and the error in the reported SCB content of eachsection was estimated. By using the appropriate trainingsets, chemometric models for giving SCB versuschemometric models were constructed for obtaining SCBversus MWD profiles of enough accuracy for detectingtrends resulting from catalysis and process changes in low-and high-density polyethylene samples. The model wasused for accurate quantification of branching levels inpolyolefins within plus or minus 0.5/1000 total carbons(i.e. about 0.1 mol percentage) in samples havingrelatively low SCB levels, i.e. less than 10 SCB/totalcarbons and mixed branch types. 20 refs.USA

Accession no.835164

Item 61Journal of Applied Polymer Science82, No.7, 14th Nov.2001, p.1677-90SURFACE MODIFICATION OF LOW DENSITYPOLYETHYLENE (LDPE) FILM ANDIMPROVEMENT OF ADHESION BETWEENEVAPORATED COPPER METAL FILM ANDLDPEJu-Shik Kong; Dong-Jin Lee; Han-Do KimPusan,National University

The effects of chromic acid treatment for periods of timebetween 1 and 60 minutes and oxygen plasma treatment



for periods of time between 30 and 90 seconds on thesurface of low density polyethylene films were examinedby attenuated total reflectance fourier transform infraredspectroscopy, electron spectroscopy for chemical analysis(ESCA), scanning electron microscopy and water contactangle. The effect of chromic acid treatment on the tensilestrength of the samples was evaluated and tensile strengthreduced with increasing treatment time. Adhesion ofcopper film to the treated surface was evaluated by ascratch test. It was found that both surface roughness andnumber of polar groups on the surface increased withincreasing treatment times of both chromic acid andoxygen plasma, resulting in lowered water contact angle.Blackening of a film sample occurred after 30 minutestreatment in chromic acid. Adhesion of copper filminitially increased with increasing treatment times, butoptimum adhesion properties consistent with tensilestrength retention were established with 30 minuteschromic acid treatment followed by 30 seconds oxygenplasma treatment. 14 refs.KOREA

Accession no.834851

Item 62Advanced Materials & Processes159, No.10, Oct.2001, p.66-7SURFACE ENGINEERING TECHNOLOGIESSudarshan T SMaterials Modification Inc.

The 15th International Conference on SurfaceModification Technologies will be held in November inIndianapolis. This article presents a few paper abstractsand lists the titles of the sessions. Papers include: structureand properties of HVOF sprayed amorphous polymermatrix nanocomposite coatings; field experience withadvanced soft-metal surfaces on carbon steel boltingmaterials used in gall-prone gasketed joints that operateat elevated temperatures; characterisation of industrialcoatings with atomic force microscopy; characterisingaluminium pretreatments for structural adhesive bonding;the Air Force manufacturing technology laser peeninginitiative; and iron aluminide based coating deposited byhigh energy density processes.USA

Accession no.834668

Item 63Journal of Applied Polymer Science82, No.6, 7th Nov.2001, p.1382-90PROPERTIES AND MORPHOLOGY OFPOLY(ETHYLENE TEREPHTHALATE) ANDHIGH-DENSITY POLYETHYLENE BLENDGuerrero C; Lozano T; Gonzalez V; Arroyo ENuevo Leon,Universidad Autonoma

Blends of polyethylene terephthalate (PET) and highdensity polyethylene (HDPE), widely used in the soft

drinks industry, were studied with and without acompatibiliser. The compatibilising agent was a surlyncopolymer of ethylene and methacrylic acid partiallyneutralized with zinc, the olefinic segment of which iscompatible with HDPE, whereas the carboxylic acidgroups form hydrogen bonds with the PET carbonylgroups. Infrared spectroscopy, differential scanningcalorimetry, scanning electron microscopy, and themechanical properties were used to assess theeffectiveness of the compatibiliser. 29 refs.MEXICO

Accession no.832040

Item 64Polymer Degradation and Stability73, No.3, 2001, p.467-70CORRELATION BETWEEN THERMALPROPERTIES AND CONFORMATIONALCHANGES IN POLY(ETHYLENETEREPHTHALATE)/POLY(ETHER IMIDE)BLENDSRuvolo-Filho A; de Fatima Barros ASao Carlos,Universidade Federal

Virgin and recycled polyethylene terephthalate (PET) wasblended with polyether-imide (PEI) in proportionsbetween 0 and 50 percent PEI content and samples wereexamined by differential scanning calorimetry and Fouriertransform infrared spectroscopy. All blends werecompletely miscible, as indicated by a single glasstransition temperature which is dependent on blendcomposition. Crystallisation rates of PET were retardedstrongly at 20 percent PEI content and above, but degreeof crystallinity was easily determined from a linearcorrelation between a structural parameter measuredspectroscopically and enthalpy of fusion. Trans conformeractivation energy measurement confirmed the effects ofPEI content on crystallisation of PET. 9 refs.BRAZIL

Accession no.831829

Item 65Polymer Degradation and Stability73, No.3, 2001, p.463-6EFFECT OF INTERFACE MODIFICATION ONTHE PHOTO-STABILITY OF PIGMENTEDPOLYETHYLENE FILMSAnna P; Bertalan G; Marosi G; Ravadits I; Maatoug MABudapest,University of Technology & Economics

Examination of the ageing characteristics of high densitypolyethylene films containing phthalocyanine green andtitanium white and other pigments with those of lightlystabilised polymer film without pigments was carried outusing tensile analysis, differential scanning calorimetryand ultraviolet spectroscopy. The early failure of thephthalocyanine pigmented sample, and subsequent UV



spectroscopic examination showed that the cause wasadsorption of stabilisers onto the pigment surface.Reactive surfactant coating of pigments was shown toconsiderably extend the film stability by reducing theiradsorbency. 9 refs.EASTERN EUROPE; HUNGARY

Accession no.831828

Item 66Polymer Degradation and Stability73, No.3, 2001, p.387-92MECHANISM OF PHOTOSTABILIZATION OFPERFLUOROPOLYETHER COATINGS BYHINDERED AMINE STABILISERSLuda M P; Camino G; Laurenti E; Novelli S;Temtchenko T; Turri STorino,Universita; Centro Ricerche Ausimont

The mechanism of operation of hindered amine stabilisers(HAS) against photodegradation in perfluoro polyethersincorporated into a coating material of polyurethane hasbeen studied by infrared spectroscopy, gaschromatography-mass spectrometry and electron spinresonance spectroscopy. Under curing conditionsnormally utilised for coil coating (280 degrees Centigradefor 1 minute in air), the HAS was found to increase thenumber of urea bridges in the polyurethane network, andreduce the amount of unreacted isocyanate, giving astructure which is more resistant to photooxidation.Byproducts of the high temperature cure process, causedby partial transformation of the HAS into -NH derivativesact as antioxidants. The unreacted HAS was found toslowly evaporate from the test film, but whilst presentacted as a radical scavenger. 8 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.831816

Item 67Plast’ 21No.101, April 2001, p.77-9SpanishINFRARED THERMOGRAPHY: THE COLOURSOF HEATASCAMM

The use of IR thermography in the study of injectionmoulds and injection moulded plastics parts is discussed,and details are given of research and development projectsbeing undertaken by ASCAMM of Spain using thistechnique.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.831329

Item 68Polymers for Advanced Technologies12, No.9, Sept, 2001, p.515-23

HIGH RESOLUTION SOLID-STATE CARBON 13NMR STUDY OF AS-CURED AND IRRADIATEDEPOXY RESINSNgono-Ravache Y; Foray M-F; Bardet MGrenoble,University

Details are given of the effects of strong ionisingradiations on the physico-chemical modifications ofepoxy resins. The sensitivity of the epoxy resins toradiation was determined using carbon 13 NMR. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.831124

Item 69Applied Spectroscopy55, No.8, Aug. 2001, p.984-91RAMAN AND INFRAREDMICROSPECTROSCOPIC MAPPING OFPLASMA-TREATED AND GRAFTED POLYMERSURFACESKeen I; Rintoul L; Fredericks P MQueensland,University of Technology

A section of the surface of a predominantly PP substratecontaining a small amount of PE copolymer and a smallamount of blended EPM was characterised before andafter plasma treatment and after graft copolymerisationwith PS by means of Raman and ATR/IR mapping. Themaps constructed indicated variations in crystallinityacross the surface, the distribution of EPM and thedistribution of hydroxy groups introduced onto the surfaceby plasma treatment. 24 refs.AUSTRALIA

Accession no.830453

Item 70POLYMER PROCESSING ENGINEERING. 01.Proceedings of a conference held June 2001.London, IOM Communications Ltd., 2001, Paper 5,p.46-58, 012AT-PROCESS RAMAN SPECTROMETRY OFPOLYMER MELTSDhamdhere M; Li J; Deshpande B; Patil P; Hansen M GTennessee,University(Institute of Materials; Interdisciplinary ResearchCentre)

In-line monitoring of EVA extrusion was carried out usingin-line fibre optic Raman spectroscopy. Vinyl acetatecontent in the random copolymer and melt indices ofvarious grades of the EVA were determined and vinylacetate content in the samples correlated using linear leastsquares and PLS analysis. Hierarchical Cluster analysis wasemployed as a pattern recognition technique to follow thenatural clustering tendencies of the EVA samples. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK; USA;WESTERN EUROPE

Accession no.830358



Item 71Polymer Testing20, No.7, 2001, p.729-40DIRECT SOLID SAMPLING METHODS FORGAS CHROMATOGRAPHIC ANALYSIS OFPOLYMER/ADDITIVE FORMULATIONSBart J C JMessina,University

The present ‘state of the art’ in direct solid samplingmethods for gas chromatographic analysis of additivesencapsulated in polymers is reviewed. Techniquesconsidered are static and dynamic headspace methods,thermal desorption and solid phase microextraction.Applications for each method are discussed. 54 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.830211

Item 72Antec 2001.Conference proceedings.Dallas, Texas, 6th-10th May, 2001, paper 620DETERMINATION OF CONDENSABLEVOLATILES DURING POLYMER PROCESSINGUSING AN ANALYTICAL EXTRUDERBuzanowski W C; Gunderson J; Froelicher SDow Chemical Co.(SPE)

A method of collecting and analysing the volatiles createdduring extrusion is described, in which the extruder is partof the analytical instrumentation. A non-vented 19 mm (3/4 in) single screw extruder was fitted with a right angle 3.2mm single strand die, which in turn carried a glass tubewith a bulb near the die exit to allow for polymer swell,and a side arm for attachment of the sampling system. Thepolymer extruded into the glass tube, the less volatilematerials condensing in the tube, and the more volatilematerials being withdrawn by the side arm and trapped ina set of three impingers containing an appropriate chilledtrapping solution. The volatiles from the glass tube wereremoved by rinsing and analysed by Fourier transforminfrared spectroscopy and gas chromatography-massspectrometry. The trapping solutions were analysed directly.The equipment was used to determine the influence ofextrusion time on volatile emissions from polycarbonate,the influence of melt temperature on volatile loss from apolycarbonate/styrene-acrylonitrile copolymer blend, andthe influence of additives on volatile loss from a glass-filled polymer. 6 refs.USA

Accession no.830052

Item 73Journal of Applied Polymer Science81, No.8, 22nd August 2001, p.1902-13DYNAMIC MECHANICAL ANALYSIS STUDYOF THE CURING OF PHENOL-

FORMALDEHYDE NOVOLAC RESINSMarkovic S; Dunjic B; Zlatanic A; Djonlagic JBelgrade,University

Using dynamic mechanical analysis the curing reactionsof typical phenol-formaldehyde novolac resins werefollowed. The evolution of various rheological parameterswas recorded for samples of the resins on cloth. A third-order phenomenological equation described the curingreaction. The influences of the structure, composition andphysical treatment on the curing kinetics were evaluated.20 refs.EASTERN EUROPE; YUGOSLAVIA

Accession no.829458

Item 74Journal of Applied Polymer Science81, No.11, 12th Sept.2001, p.2779-85RIGID AMORPHOUS PHASE AND LOWTEMPERATURE MELTING ENDOTHERM OFPOLY(ETHYLENE TEREPHTHALATE)STUDIED BY MODULATED DIFFERENTIALSCANNING CALORIMETRYSong MLoughborough,University

Three similar samples of polyethylene terephthalate (PET)prepared by isothermal cold crystallisation in thedifferential scanning calorimetry (DSC) cell (PET1), meltcrystallisation at a steady cooling rate and annealing forvarious times in the DSC cell (PET2), and quenching from300 degrees centigrade to -20 degrees over a period of 5minutes (PET3) were used to study the glass transitioneffects in the rigid amorphous phase and the lowtemperature melting endotherm using modulated DSC.As annealing time increased in PET2 the increment ofheat capacity (IHC) at annealing temperature increasedand the IHC at the glass transition temperature decreased.It was deduced that the low temperature meltingendotherm originated with transitions in the rigidamorphous fraction, and it was noted that the glassliketransition of this fraction occurred between glass transitionand melting temperatures. 23 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.829381

Item 75Journal of Applied Polymer Science81, No.10, 6th Sept.2001, p.2387-98COMPARISON OF THERMAL DEGRADATIONCHARACTERISTICS OF POLY(ARYLENESULFONE)S USING THERMOGRAVIMETRICANALYSIS/MASS SPECTROMETRYLi-Hsiang PerngTa Hwa,Institute of Technology

Thermogravimetric analysis with gas chromatography andmass spectrometry were used in the analysis of the thermal



degradation of polyether sulphone (PES) andpolysulphone (PSF). Evolution of sulphur dioxide andphenol from random chain scission in a one stagepyrolysis was observed in both cases with apparent initialthermal stability of the PES being lower than PSF, butfire retardation of PES was better due to reduction of thesulphone group by hydrogen radicals. More pyrolysisproducts were identified from the PSF than from the PES.Thermal stability of ether and sulphone groups appearedsimilar in PES but in PSF the sulphone groups provedthe more stable. A simple kinetic model was developedwhich showed good agreement between theoretical andexperimental pyrolysis curves for both polymers. 20 refs.TAIWAN

Accession no.829337

Item 76Journal of Applied Polymer Science81, No.12, 19th Sept.2001, p.3064-8TEMPERATURE AND ATMOSPHEREINFLUENCES ON SMOKE COMPOSITIONDURING THERMAL DEGRADATION OFPOLY(ETHYLENE TEREPHTHALATE)Malgorzata Dzieciol; Jerzy TrzeszczynskiSzczecin,Technical University

The less volatile compounds formed during the thermaldegradation of polyethylene terephthalate (PET) underdifferent conditions at 200-700 deg.C in nitrogen and airatmospheres were studied. The compounds were trappedon a glass fibre filter and analysed by capillary gaschromatography using a mass spectrometer (GC-MS), andhigh performance liquid chromatography. The resultswere tabulated, and plots were drawn of the degradationtemperatures in nitrogen and air atmospheres versus theweight changes of terephthalic acid and monovinylterephthalate evolved from PET. The effects of theatmosphere and temperature on smoke emission andcomposition during PET thermal degradation wereconsidered. 28 refs.EASTERN EUROPE; POLAND

Accession no.826911

Item 77Macromolecules34, No.15, 17th July 2001, p.5224-8STUDIES OF MISCIBILITY BEHAVIOUR ANDHYDROGEN BONDING IN BLENDS OFPOLYVINYLPHENOL ANDPOLYVINYLPYRROLIDONEKuo S W; Chang F CTaiwan,National Chiao Tung University

Blends of polyvinyl phenol with polyvinyl pyrrolidonewere prepared by solution casting from DMF solutions.DSC, FTIR, and NMR were used to investigate thehydrogen bonding and miscibility of the blend. The Tgof the blend was determined. 22 refs.

CHINA

Accession no.825682

Item 78Journal of Thermal Analysis and Calorimetry64, No.2, 2001, p.549-55CRYSTALLIZATION AND MELTING OFPOLYCARBONATE STUDIED BYTEMPERATURE-MODULATED DSC (TMDSC)Schick C; Wurm A; Merzlyakov M; Minakov A;Marand HRostock,University; Moscow,General Physics Institute;Virginia,Polytechnic Institute & State University

TMDSC measurements conducted at reasonably highfrequencies for bisphenol-A polycarbonate(PC, Lexan)allowed for the determination of base-line heat capacity.Vitrification and devitrification of the rigid amorphousfraction(RAF) could be directly observed. 0.01 Hzappeared to be a reasonably high frequency for PC. TheRAF of PC was established during isothermalcrystallisation. Devitrification of the RAF seemed to berelated to the lowest endotherm. For PC, the melting ofsmall crystals between the lamellae was expected to yieldthe lowest endotherm. 27 refs.

GENERAL ELECTRIC CO.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;RUSSIA; USA; WESTERN EUROPE

Accession no.825045

Item 79Shawbury, Rapra Technology Ltd., 2001, p.iv, 174,25cm, 91TEASY IDENTIFICATION OF PLASTICS ANDRUBBERSVERLAYE G A L; ROEGES N P G; DE MOOR MOKaHo Sint-Lieven

This book presents an identification scheme developedover the last thirty years for thermoplastics, commonthermosets, a few copolymers and elastomers. Thetechniques used are based on simple tests such as thebehaviour of polymers in liquids and in a flame. The bookalso covers Infrared spectroscopy. Main headings are:Simple tests (melting, solubility, burning characteristics,odour recognition, dripping, flotation, halogen test,nitrogen- and sulphur-test); Recording an IR spectrum;Identification flow charts; Thermoplastics; Cellulose andstarch; Thermosets; Elastomers. (15 Refs)BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; WESTERN EUROPE

Accession no.824868

Item 80UTECH 2000. Proceedings of a conference held TheHague, Netherlands, 28th-30th March 2000.London, 2000, Other Rigid Foam DevelopmentsSession, Paper 1, pp.4, 012



LONG-TERM ENERGY EFFICIENCY OF PU-INSULATION FOR REFRIGERATIONSeifert H; Biedermann AElastogran GmbH(Crain Communications Ltd.; European IsocyanateProducers’ Association)

The ageing behaviour of rigid PU foams was investigatedusing gas chromatographic quantitative evaluation of thecell gas composition in the foams. The change in thermalconductivity of the foams during ageing was alsoexamined as was the dimensional stability of the foamsunder diffusion open conditions and the results obtainedcorrelated with the K x A-values from refrigerator cabinetsvia the change in cell gas composition. The data obtainedrevealed that the ageing process of appliances could besimulated in a tenth of the time by measuring diffusionopened PU foams. 2 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;NETHERLANDS; WESTERN EUROPE

Accession no.824859

Item 81International Polymer Science and Technology28, No.5, 2001, p.T/79-80STUDY OF POLYMER-FILLER INTERACTIONBY INVERSE GAS CHROMATOGRAPHYGukasyan S Z

The surface modification of fillers with polymericsubstances is discussed with reference to improvementof the properties of filled polymers. When the fillers aremodified with polymers, the boundary layer contains notonly the matrix filler, but also the modifying polymer,and when the modifying polymer interacts with the surfacefiller, the properties of both the mineral component andthe modifier are altered. One characteristic which reflectsthe result of polymer-filler interaction is the glasstransition temperature of the modifier. To determine thisparameter for a very low content of polymer, the methodof inverse gas chromatography was used using themodified filler as the stationery phase. The studyinvestigated the use of travertine and tuff, the surfaces ofwhich were modified with latices of a copolymer ofstyrene and methacrylic acid. 3 refs. (Article translatedfrom Plasticheskie Massy, No.8, 2000, p.36)RUSSIA

Accession no.824324

Item 82Molecular Crystals & Liquid CrystalsVol.353, 2000, p.95-108COMPOSITES MADE FROMLIGNOCELLULOSICS AND THERMOSETPOLYMERSAramguren M I; Marcovich N E; Reboredo M MINTEMA

Preparation and testing of composites from a styrene/unsaturated polyester thermoset matrix and wood flours

from different wood species was carried out. Studies werecarried out on Pine (Pino Eliottis), eucaliptus (EucaliptusSaligna) and marmelero (Ruprechia Laviflora), asoftwood and two semi-hard woods, respectively. Theparticles were used untreated and chemically modifiedwith maleic anhydride. For the characterisation ofuntreated and treated flours, thermogravimetric analysisand analytical techniques were utilised. Dispersion of thefibrous particles, in addition to maximum fibreconcentration (accompanied by complete wetting of thewood fibres) was dependent on the treatment and on thewood species utilised. Bending and compression testssuggested some improvement in the performance of thecomposites, if the wood flour was previously esterified.Changes in the fracture surfaces due to maleic anhydridetreatment of the fibres were observed using scanningelectron microscopy. 12 refs.ARGENTINA

Accession no.824162

Item 83Polymer Degradation and Stability73, No.2, 2001, p.251-7THERMAL CHARACTERISTICS OF ADDITION-CURED PHENOLIC RESINSReghunadhan C P; Bindu R L; Ninan K NVikram Sarabhai Space Centre

The thermal cure characteristics, kinetics of thermaldegradation and pyrolysis of four different addition curedphenolic resins were investigated using varioustechniques, including DSC, DMA, FTIR spectroscopy,TGA and X-ray diffraction. Resins investigated werepropargyl ether resins and phenyl azo-, phenyl ethynyl-and maleimide-functional resins. A comparison of the dataobtained for all the phenolic resins was made as a functionof molecular structure. 12 refs.INDIA

Accession no.824043

Item 84UTECH 2000. Proceedings of a conference held TheHague, Netherlands, 28th-30th March 2000.London, 2000, Innovations: Flexible FoamDevelopments Session, Paper 5, pp.4, 012VOC DETECTION IN POLYURETHANEFLEXIBLE FOAMSOcchiello E; Tavan M; Pannocchia P; Fava FEniChem(Crain Communications Ltd.; European IsocyanateProducers’ Association)

The detection of volatile organic compounds in polyolsand PU foams using SPME, gas chromatography and gaschromatography-mass spectroscopy is demonstrated.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;NETHERLANDS; WESTERN EUROPE

Accession no.823982



Item 85Polymer Degradation and Stability73, No.1, 2001, p.163-7THERMAL, PHYSICAL AND CHEMICALSTABILITY OF POROUS POLYSTYRENE-TYPEBEADS WITH DIFFERENT DEGREES OFCROSSLINKINGYanhong Li; Yunge Fan; Jianbiao MaNankai,University

The thermal decomposition of porous polystyrene beadswith differing crosslinking degrees using divinyl benzenewere evaluated using thermogravimetry and differentialscanning calorimetry techniques. The test results showedthat the thermal stability of the beads increased with higherdegrees of crosslinking. DSC analysis revealed that theglass transition temperatures gradually increased withcrosslinking levels up to 30% crosslinking by weight, butabove this level beads were thermally stable as the glasstransition temperature was replaced by an exothermicpeak. Complete details of the testing procedures andresults are given 15 refs.CHINA

Accession no.823950

Item 86Polymer Degradation and Stability73, No.1, 2001, p.69-74EXAMINATION OF A LOW DENSITYPOLYETHYLENE (LDPE) FILM AFTER 15YEARS OF SERVICE AS AN AIR AND WATERBARRIERMoller K; Gervert T; Holmstrom ASweden,National Testing & Research Institute

Comparisons between accelerated ageing tests and testson polymeric materials aged in actual service conditionsto identify possible degradation mechanisms appear tobe the only reliable method of predicting long term servicelifetimes. A low density polyethylene film used as an airand water barrier for 15 years in an exterior wallconstruction was characterised using tensile testing,spectroscopy and chromatography techniques. Althoughthe mechanical properties of the film were unaffected byageing, its antioxidant stabilisers were severely degraded.Full details of the ageing conditions, test methods andresults are given. 16 refs.EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERNEUROPE

Accession no.823940

Item 87Polymer Degradation and Stability73, No.1, 2001, p.47-67VACUUM PYROLYSIS OF COMMINGLEDPLASTICS CONTAINING PVC. PART II.PRODUCT ANALYSISMiranda R; Pakdel H; Roy C; Vasile C

Quebec,Universite Laval; Pyrovac Institute Inc.; PetruPoni,Institute of Macromolecular Chemistry

Vacuum pyrolysis was performed on HDPE, LDPE, PP,PS and PVC materials individually, and also on a mixedplastics sample containing the five polymers. The maingaseous and liquid products, including chlorinatedhydrocarbons, were identified by chromatography, andthe yields and pyrolysis products were compared for theindividual and mixed runs. The results suggested that thepyrolysis yields of the plastics mixtures were similar tothose calculated from the pyrolysis of the individualpolymers. However, the chlorine content was lower thanexpected indicating limited interaction during pyrolysis.Full details of the experimental procedures are givenincluding a detailed tabulation of all the pyrolysisproducts. 54 refs.CANADA; EASTERN EUROPE; RUMANIA

Accession no.823939

Item 88Polymer Degradation and Stability73, No.1, 2001, p.15-22THERMO-OXIDATIVE STABILITY OF PPWASTE FILMS STUDIED BY IMAGINGCHEMILUMINESCENCE

The spread of oxidation in artificially recycled PPmaterials, with and without stabilisation, was monitoredusing imaging chemiluminescence techniques. The resultswere compared with estimates made using Fouriertransform infrared spectroscopy and differential scanningcalorimetry techniques. It was concluded that althoughthe conventional techniques gave residual lifetimes of fivecycles, imaging chemiluminescence showed that asignificant reduction in oxidative stability had occurredafter only two cycles. Full details of the imagingchemiluminescence technique used are given withdetailed results. 12 refs.

Accession no.823934

Item 89DEVELOPMENTS IN POLYMER ANALYSIS ANDCHARACTERISATION Proceedings of a conferenceheld Shawbury, UK, 10th May 1999.Shawbury, 1999, Paper 4, p.1-15, 012CHEMICAL CHARACTERISATION OFPOLYURETHANESForrest M JRapra Technology Ltd.(Rapra Technology Ltd.)

Polyurethane chemistry is briefly outlined, additivesgenerally used in polyurethanes are indicated and theanalytical techniques used to characterise the structure,composition and properties of PUs and PU-based productsare discussed in a comprehensive manner. Techniquescovered include spectroscopic, chromatographic techniquesand miscellaneous techniques, such as wet chemistry



techniques. Sections are included dealing with thecharacterisation of polymer structure and starting materials,molecular weight determinations, characterisation ofadditives and cure reaction studies. 14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.822952

Item 90Macromolecular SymposiaVol. 169, May 2001, p.45-55CHARACTERIZATION OF THEINTERACTIONS IN POLYMER/SILICASYSTEMS BY INVERSE GASCHROMATOGRAPHYVoelkel A; Milczewsk K; Jeczalik JPoznan,University of Technology

The inverse gas chromatography technique, (IGC) ispresented as a method of characterisation of theinteractions in polymer-modified silica systems. Theauthors propose to express the magnitude of modifiedfiller/polymer interactions by means of the Flory-Hugginsparameter. Polyether-urethane/modified silica systemscontaining different amounts of filler were investigated,and information relating to the physicochemical propertiesof oligomer and modified silicas were presented by meansof the solubility factor to describe the properties of thepolymer layer, and the Flory-Huggins parameter whichdescribes the polymer-solute or mixture polymer/silica-solute interactions. These parameters are obtained frominverse gas chromatography experiments. The influenceof the IGC experiment temperature, the content ofmodified silica, and the nature of test solute on theevaluated parameters are presented and discussed. 7 refs.EASTERN EUROPE; POLAND

Accession no.822644

Item 91Journal of Applied Polymer Science80, No.8, 23rd May 2001, p.1305-11EFFECT OF RECYCLED POLYPROPYLENE ONPOLYPROPYLENE/HIGH DENSITYPOLYETHYLENE BLENDSBonelli C M C; Martins A F; Mano E B; Beatty C IRio de Janeiro,Universidade Federal;Florida,University

A study was made of the effects of addition of recycledpolypropylene on the incompatible blends of virginpolypropylene with high-density polyethylene. Thecharacteristics of the recycled polypropylene weredetermined by spectrographic and thermal analysis means.The mechanical properties of the blends were determined.The 50/50 blend of the two virgin polymers benefited mostfrom the addition of the recycled polypropylene. 9 refs.BRAZIL; USA

Accession no.821546

Item 92Polymer Degradation and Stability72, No.1, 2001, p.175-86CHEMICAL AND MORPHOLOGICALMODIFICATIONS OF IRRADIATED LINEARLOW DENSITY POLYETHYLENE (LLDPE)Guadagno L; Naddeo C; Vittoria V; Camino G;Cagnani CSalerno,University; Turin,University; Montell ItaliaSpA

Spherilene technology produced films of linear lowdensity polyethylene which were exposed to UVirradiation to simulate accelerated weathering.Comparison was made with a set of films annealed at60C and no irradiation. The resulting chemical structureswere examined using FTIR. The findings were that thedegradation is dominated by the formation of carbonyland vinyl species. 22 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.820850

Item 93Polymer Degradation and Stability72, No.1, 2001, p.31-45FACTORS AFFECTING THE ADSORPTION OFSTABILISERS ON TO CARBON BLACK (FLOWMICRO-CALORIMETRY STUDIES). IV.SECONDARY ANTIOXIDANTSPena J M; Allen N S; Edge M; Liauw C M; Valange BManchester,Metropolitan University; Cabot Corp.

Using flow micro-calorimetry, X-ray photoelectronspectroscopy and Fourier transform infra-redspectroscopy techniques the surface activity of differenttypes of carbon black with secondary antioxidants (arylphosphites and phosphonites) have been examined. Bothin the overall adsorption activity and the levels of probeadsorption significant differences were observed. Twofactors were reported which were found to influence thebehaviour of phosphite stabilisers. 29 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; WESTERN EUROPE

Accession no.820835

Item 94Polymer International50, No.6, June 2001, p.635-42DEGRADATION OF HIGH BARRIERETHYLENE-VINYL ALCOHOL COPOLYMERUNDER MILD THERMAL-OXIDATIVECONDITIONS STUDIED BY THERMALANALYSIS AND INFRARED SPECTROSCOPYLagaron J M; Gimenez E; Suara J JJaume I,Universitat

The thermooxidative degradation of a solution castethylene-vinyl alcohol copolymer (containing 32



mol.percent ethylene) used in barrier applications wasstudied at three temperatures immediately above themelting point using thermogravimetric analysis, DSC andFTIR spectroscopy. The weight loss measured bythermogravimetric analysis was fast at short times andslowed down progressively. The weight loss of about 3.6percent measured by thermogravimetric analysis resultedfrom chemical alterations in the polymer. DSC showedsmall changes in crystallinity, melting point and glasstransition and broadening of the melting endotherms insamples exposed to the more severe thermooxidativetreatments. FTIR showed a transformation of the vinylalcohol hydroxyl groups into carbonyl groups and thecreation of double bonds. Changes in degradation kinetics,and possibly mechanisms, were thought to occur withincreasing time. FTIR measurements indicated thattransformation of the hydroxyl groups led to a weakeningof the overall hydrogen bonding strength in the degradedsamples so a reduction in the intermolecular cohesion,and hence the barrier properties of the copolymer, couldbe anticipated. 19 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.819207

Item 95Polymer Science Series B43, Nos. 3-4,March/April 2001, p.105-8TRANSFORMATIONS OF ANTIMONY-HALOGEN- AND NITROGEN-PHOSPHORUS-BASED FLAME RETARDANTS INPOLYOLEFINS AND THEIR PERFORMANCEBogdanova V VBelorussian,State University

Degradation products from both antimony-halogen basedand nitrogen-phosphorus based flame retardants werestudied using X-ray diffraction and atomic emissionanalysis. Evidence of the retardation mechanisms in useagainst combustion was obtained for each system and ineach case emission of volatile combustion inhibitors atthe degradation temperature of the polymer matrix wasthe critical factor. 11 refsBELARUS; BELORUSSIA

Accession no.818458

Item 96Polimery45, Nos.11-12, 2000, p.51-8PolishPYROLYSIS GAS CHROMATOGRAPHY ANDNEW POSSIBILITIES OF ITS USE IN THEANALYSIS OF POLYMERSHetper J

Major conditions are formulated to ensure that pyrolysisgas chromatography yields reliable and repeatable results,particularly when non-volatile substances such as

polymers are analysed. The author’s own modificationof PGC is presented, involving the use of a pyrolysisattachment with the mobile reaction zone. Resulting dataare compared with those obtained by conventionalpyrolysis gas chromatography. 34 refs.

Accession no.816530

Item 97New York, John Wiley & Sons, Inc., 1999, pp.xv,752CHEMICAL SEPARATIONS- PRINCIPLES,TECHNIQUES, AND EXPERIMENTSMELOAN, C EKANSAS STATE UNIVERSITY

This combination laboratory manual and reference sourceprovides a working knowledge of an array of separationmethods. In forty-two chapters, it explores all majorcategories of separation. With an emphasis upon everydaypractice rather that theory, this book explains theprinciples and parameters of these methods and provides59 specific experiments to demonstrate proper procedures.These experiments feature step-by-step protocols for eachseparation scheme, precise instructions on setting up theapparatus, and checklists for essential chemicals andsupplies. Main Headings include Separations involvingphase changes; Separations involving extraction;Separations involving chromatography; Separationsinvolving ion exchange resins; Separations involvingelectric fields; Separations involving flotation;Separations involving membranes; Separations involvingmiscellaneous techniques.USA

Accession no.816497

Item 98Polymer Bulletin46, No.2-3, April 2001, p.191-6MISCIBILITY OF POLYETHERIMIDE ANDPOLYBUTYLENE NAPHTHALATE BLENDSLin C H; Wang C STaiwan,Kung Shan Institute of Technology;Taiwan,National Cheng Kung University

DSC, optical microscopy, and SEM were performed tocharacterise the miscibility of a blend of polybutylenenaphthalate and polyetherimide. Data were compared withtheoretical predictions. 6 refs.CHINA

Accession no.816205

Item 99Journal of the National Institute of Materials andChemical Research8, No.4, 2000, p.149-59JapanesePOSITRONIUM FORMATION AND DIFFUSIONIN POLYMERS



Hirata K; Kobayashi Y

High-energy positrons injected into condensed matterquickly lose their energy, become thermalised andannihilate with one of the electrons of the medium intogamma rays. In polymers, some of the positrons form ahydrogen-like bound state between a positron and anelectron prior to the annihilation. This bound state is calledpositronium (Ps). Ps is formed by recombination of apositron and one of the electrons released from themolecules in terminal positron spur. Positron-electronrecombination in the positron spur competes with otherreactions, so that the Ps formation probability dependson various factors. The influence of additives, polargroups and external field on Ps formation in polymers isdiscussed. A possibility of using Ps as a radiation chemicalprobe for polymers is described. Ps formed as a result ofpositron-electron recombination interacts with asubnanometer-size free volume hole, and diffuses over acertain distance before annihilation. The diffusioncoefficient of Ps is determined using a chemical reactionbetween Ps and an additive, and its diffusion length inamorphous polymers is estimated to be ca.1 nm. Thisresult is of fundamental importance to apply Ps as a probefor studying free volume in polymers. 68 refs.JAPAN

Accession no.815833

Item 100Journal of Applied Polymer Science80, No.11, 13th June 2001, p.2120-2SOLID-STATE NMR AND XPS STUDIES OF PVA/SUGARCANE COMPOSITESTavares M I B; Stael G C; Gorelova M M; de MenezesS M CRio de Janeiro,Cidade Universitaria

Bagasse, taken directly from the sugarcane mills, wasdried, cut to lengths of 5 mm, and blended withpoly(ethylene-co-vinyl acetate) in proportions up to 60wt%. The composites were characterised by solid-statenuclear magnetic resonance spectroscopy and X-rayphotoelectron spectroscopy. A homogeneous copolymercovering on the surface of the fibres was achieved, thesamples exhibiting homogeneity at the molecular level.The best physical interaction between the fibres and thematrix was achieved with the sample containing 60 wt%fibre. 10 refs.BRAZIL

Accession no.814366

Item 101Journal of Polymer Science: Polymer Physics Edition39, No.3, 1st Feb.2001, p.337-41PHYSICAL AGING OF POLYCARBONATEINVESTIGATED BY DYNAMICVISCOELASTICITYApaki O; Horie M; Masuda T

Kyoto,University

Dynamic viscosity measurements were used to determinethe physical ageing at 110C of polycarbonate usingsamples quenched from the molten state. The test resultsshowed that there was a memory effect in thepolycarbonate of the quenching processes, but asequilibrium is reached then the memory becomes lost.Evidence is shown that the structure of the polymericchain in the glassy state relaxes over larger segment scalelengths because the scale of the movable segments isrelated to temperature. 29 refs.JAPAN

Accession no.814126

Item 102Polymer42, No.13, 2001, p.5523-9SEC-FTIR CHARACTERIZATION OF SEMI-CRYSTALLINE HDPE AND PPVerdumen-Noel L; Baldo L; Bremmers SDSM Research

A pressure transducer in combination with the sizeexclusion chromatography-FTIR technique was used tocharacterise semi-crystalline materials such as HDPE andrandom PP copolymers. The comonomer content (butenefor HDPE and ethylene for PP) decreased with increasingmolar mass. For two HDPE samples produced by the dualreactor process, this decrease occurred stepwise with aconstant comonomer amount on either side of the step.For all the HDPE samples, the amount of endunsaturations decreased with molar mass. Theconcentration of side and trans unsaturations was too lowto be determined. 8 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.813974

Item 103Macromolecular Materials and Engineering286, No.3, 30th March 2001, p.161-7MATRIX-ASSISTED LASER DESORPTION/IONIZATION MASS SPECTROMETRY OFSYNTHETIC POLYMERS, 5A. ANALYSIS OFPOLY(PROPYLENE OXIDE)S BY COUPLEDLIQUID CHROMATOGRAPHY AT THECRITICAL POINT OF ADSORPTION ANDMALDI-TOF MASS SPECTROMETRYKeil C; Esser E; Pasch HDarmstadt,Deutsches Kunststoff-Institut

Poly(propylene oxide)s were analysed efficiently bycoupled liquid chromatography and MALDI-TOF massspectrometry. The techniques were coupled via a roboticinterface where the matrix was coaxially added to theeluate and spotted dropwise onto the MALDI target. Sizeexclusion chromatography and liquid chromatography atcritical conditions of adsorption coupled to MALDI-TOF



gave useful structural information on oligomer massesand chemical composition; The technique showed thepresence of diols and monools in addition to the triols inpoly(propylene oxide) triols. The oligomer distributionsof all functionality fractions were determined. 23 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.813967

Item 104Polimery45, No.10, 2000, p.701-6PolishOXIDATION AND DESORPTION OF OXYGENFROM THE UPPER LAYER OF ACTIVATEDPOLYPROPYLENE FILMZenkiewicz M

Photoelectron spectroscopy was used to study oxidationof biaxially oriented polypropylene film. X-rays andultrahigh vacuum associated with the method of studywere found to promote oxygen desorption from the upperlayer. 6 refs. Articles from this journal can be requestedfor translation by subscribers to the Rapra producedInternational Polymer Science and Technology.

Accession no.813667

Item 105Macromolecules34, No.8, 10th April 2001, p.2667-72SELF-FOCUSING IN GRADIENT LIQUIDADSORPTION CHROMATOGRAPHY OFPOLYMERSDegoulet C; Perrinaud R; Ajdari A; Prost J; Benoit H;Bourrel MTotalFinaElf; Atofina; Elf Atochem North AmericaInc.; ESPCI; Institut Curie; Institut Charles Sadron

The separation process occurring during liquidchromatography of polymers in a gradient of compositionof the eluent was examined. The main feature was that,after a transient regime, the concentration profile tendedto move as a front, i.e. without diffusive spreading in time.This results in relatively sharp peaks and the observationthat long columns were useless. A simple analytical modelwas proposed for this self-focussing process that allowedoptimal conditions of operation to be determined. Thisanalysis was supported by experimental tests. 13 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;USA; WESTERN EUROPE

Accession no.813456

Item 106Macromolecules34, No.8, 10th April 2001, p.2395-7NONDESTRUCTIVE MEASUREMENT OF AGLASS TRANSITION TEMPERATURE AT SPIN-CAST SEMICRYSTALLINE POLYMER SURFACES

Hyun J; Aspnes D E; Cuomo J JNorth Carolina,State University

A non-destructive technique for characterisation of thesurface Tg in PETP is described which involves analysisof the variation of the ellipsometrically measuredrefractive index with temp., using the spectral dependenceof the penetration depth of light to discriminate betweensurface and bulk transitions. The surface Tg is shown tobe lower than that of the bulk for spin-cast semicrystallinePETP films because of density variation and Tg is foundto be lowered further by plasma processing. 18 refs.USA

Accession no.813421

Item 107Macromolecular SymposiaVol.165, March 2001, p.91-8RECENT DEVELOPMENTS IN POLYOLEFINCHARACTERISATIONPasch HDeutsches Kunststoff-Institut

A brief review is presented on techniques for the analysisof polyolefins and additives in polyolefins. Techniquesconsidered include high-temperature GPC combined withFTIR spectroscopy for the analysis of chemicalcomposition as a function of molar mass, crystallisationfractionation for the analysis of short-chain branching inLLDPE and of polyolefin blends and pyrolysis-gaschromatography-mass spectrometry for the determinationof additives, such as antioxidants, in polyolefins. 13 refs.(3rd Annual UNESCO School & IUPAC Conference onMacromolecules and Materials Science, Stellenbosch,South Africa, 2000)EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.813085

Item 108Vinyltec 2000. Conference proceedings.Philadelphia, Pa., 11th-12th Oct.2000, p.198-202USE OF ADVANCED ANALYTICAL METHODSTO ENHANCE THE PERFORMANCE OF VINYLMATERIALSIsner J D; Eiden R WPolymer Diagnostics Inc.(SPE,Vinyl Div.; SPE,Philadelphia Section)

Analytical laboratories are asked to perform a variety oftest methods in order to solve problems relating to theperformance or otherwise of vinyl materials, and whilstthere are many individual problems that need to be solved,they can be categorised, it is argued, by a relatively smallnumber of questions. Five of these questions areaddressed, and ways in which a laboratory may answerthem are discussed. Suggestions are made for techniquesthat may be used for each question, and examples ofproblems are given. Recent advances in analytical



techniques can be used to address topics such as lifetimeprediction and failure analysis. Questions related toidentification, commercialisation, competitiveness, failureand performance.USA

Accession no.811310

Item 109Journal of Materials Science Letters20, No.3, 1st Feb.2001, p.257-8COMMENTS ON A NEW RAMAN PEAK IN AHIGH-DENSITY POLYETHYLENERodriguez A B; Young R JNavarra,Universidad Publica; Manchester,University;UMIST

Raman spectroscopy yields information about themolecular structure of materials based on the observationof scattered light spectra, and has been used extensivelyin the investigations of polymer structure andcomposition: chemical structure and interactions,morphology, crystalline and amorphous structure,processing effects and orientation, etc. As an analyticaltechnique, however, it is not free from artefacts, i.e.apparent experimental results that are not actually realbut are due to the experimental methods or conditions.One factor that may be responsible for the presence ofartefacts in Raman spectroscopy is external backgroundlight. There are numerous potential sources of externalbackground light that lead to sharp spectral peaks. If theyare not excluded from the collection optics of the Ramaninstrument, they can lead to noise, or artefacts,superimposed on the Raman spectrum from the sample.This background light can come from either the sampleor from the environment around the sample. A study ofthe latter is reported. 14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; UK;WESTERN EUROPE

Accession no.811165

Item 110Journal of Applied Polymer Science80, No.7, 16th May 2001, p.1071-84PHASE BEHAVIOUR AND MOLECULARMOBILITY IN POLYURETHANE/STYRENE-ACRYLONITRILE BLENDSVatalis A S; Kanapitsas A; Delides C G; Viras K; Pissis PKozani,Technological Education Institute;Athens,University; Athens,Kapodistrian University

The molecular mobility and microphase separation inblends of crosslinked polyurethane (PUR) and styrene-acrylonitrile (SAN) copolymer were investigated. ThePUR and SAN copolymer were prepared by reactiveblending with polymer polyols. DSC, thermallystimulated depolarisation currents (TSDC) techniques,dielectric relaxation spectroscopy (DRS) and dynamicmechanical thermal analysis over a wide range of

temperatures and frequencies were used in theinvestigation. Results by each technique indicated thatthe degree of microphase separation of PUR into hard-segment (HS) microdomains and soft-segment (SS)microphase increases on addition of SAN. The varioustechniques used were initially compared with each other.Results showed that for the dynamic glass transition ofthe PUR SS microphase the characteristic time scales atthe same temperature are similar for DSC, TSDC andDMTA and shorter for DRS. The PUR/SAN blends areclassified as fragile systems. 40 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;WESTERN EUROPE

Accession no.810314

Item 111Macromolecular Rapid Communications22, No.2, 8th Feb.2001, p.51-67EVANESCENT WAVE LIGHT SCATTERING.FUSION OF THE EVANESCENT WAVE ANDLIGHT SCATTERING TECHNIQUES TO THESTUDY OF COLLOIDS AND POLYMERS NEARTHE INTERFACEMatsuoka HKyoto,University

The evanescent wave light scattering technique, which isproduced by a fusion of the evanescent wave techniqueand light scattering technique, is a very powerful an usefultool for investigation of colloidal particles and polymersnear the surface and interfaces. Two kinds of evanescentwave light scattering apparatuses are developed. One isthe evanescent wave dynamic light scattering (EVDLS)technique and the other is the evanescent wave lightscattering microscope (EVLSM). By EVDLS, the diffusionbehaviour of a colloidal particle near the interface can beextracted quantitatively as a function of the distance fromthe interface. The diffusion coefficient is smaller than thosefor particles in bulk, reflecting electrostatic andhydrodynamic interactions. By EVLSM, the interactionpotential profile between a colloidal particle and the surfacein dispersion can be directly evaluated. EVLSM will playan import role in colloidal interaction studies, especially ata low ionic strength. It is also shown that a particle dynamicsstudy is possible by the EVLSM technique. A new fieldwill be developed in colloid science and polymer scienceby application of the evanescent wave light scatteringtechnique, i.e. fusion of the evanescent light and a scatteringtechniques. 41 refs.JAPAN

Accession no.809623

Item 112Journal of Applied Polymer Science79, No.6, 7th Feb.2001, p.1101-12ULTRASONICATION AND MICROWAVEASSISTED EXTRACTION OF DEGRADATIONPRODUCTS FROM DEGRADABLE



POLYOLEFIN BLENDS AGED IN SOILContat-Rodrigo L; Haider N; Ribes-Greus A; KarlssonSStockholm,Royal Institute of Technology;Valencia,Polytechnical University

Degradation in soil of samples of a polyolefin blendtreated with two different biodegradable additives (astarch/iron mixture and a commercial product (Mater-BiAF05H)) was studied using two non-conventionalextraction techniques. The period studied was from 0 to21 months, and extracted products were analysed by gaschromatography mass spectroscopy. Molecular weightchanges were monitored using high-temperature sizeexclusion chromatography. Extraction techniques wereultrasonication and microwave assisted extraction (MAE).Reproducibility of ultrasonification was found better withimproved extraction of carboxylic acids and otherproducts than MAE methods, but both were found fasterthan conventional (soxhlet) extraction techniques. Tablesindicate the relative amounts of different extractionproducts and molecular weight changes in the polymerblend found over the 21-month period for bothbiodegradable additive types. 17 refsEUROPEAN COMMUNITY; EUROPEAN UNION;SCANDINAVIA; SPAIN; SWEDEN; WESTERN EUROPE

Accession no.808785

Item 113Polimeros: Ciencia e Tecnologia10, No.4, Oct./Dec.2000, p.202-8PortugueseETHYLENE COPOLYMERS ANALYSIS BYFRACTIONATION TECHNIQUESEscher F F N; Silva L P; Galland G B; Benetti ARio Grande do Sul,Universidade Federal; IpirangaPetroquimica SA

Ethylene-butene copolymers were fractionated accordingto molecular size by direct extraction by different solventsand at different temperatures. Samples were alsofractionated by differences in crystallinity using DSC.Fractions were characterised using carbon 13 NMR, FTIR,GPC and DSC. 9 refs.BRAZIL

Accession no.808128

Item 114Journal of Polymer Science: Polymer ChemistryEdition39, No.5, 1st March 2001, p.630-9NEW SEGMENTED POLYESTER-URETHANESFROM RENEWABLE RESOURCESLiu Y; Lindblad M S; Ranucci E; Albertsson A-CSweden,Royal Institute of Technology

The physical and mechanical properties of aliphaticpolyesters from propanediol and succinic acid wereimproved by their combination with aromatic urethane

segments capable of establishing strong intermolecularhydrogen bonds. Characterisation was carried out usingproton NMR, size exclusion chromatography, DSC, anddynamic mechanical analysis. The influence of the ratioof hard and soft segments on degree of crystallinity, Tg,melting point, tensile strength, elongation and Young’smodulus was examined. 24 refs.EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERNEUROPE

Accession no.808057

Item 115Journal of Applied Polymer Science80, No.1, 4th April 2001, p.1-9CROSSLINKING AND ITS EFFECTS ONPOLYANILINE FILMSTan H H; Neoh K G; Liu F T; Kocherginsky N; Kang E TSingapore,National University

Polyaniline base films with varying degrees ofcrosslinking were cast from methylpyrrolidone solutionsat different processing temperatures. The effects ofcrosslinking on solubility, morphology, tensile strength,doping characteristics and transport of ions across thefilms were investigated. Characterisation was undertakenusing UV visible spectroscopy, atomic force microscopy,and elemental analysis. 18 refs.SINGAPORE

Accession no.807643

Item 116Macromolecular SymposiaVol.162, Dec.2000, p.227-33STUDY OF POLYMER COMPLEXES BYEXCLUSION CHROMATOGRAPHY COUPLEDWITH LIGHT SCATTERING IN COMBINATIONWITH FLUORESCENCE SPECTROSCOPYMrkvickova L; Pokorna V; Pecka JCzech Republic,Academy of Sciences

PMMA stereocomplexes prepared at differentconcentration in dilute tetrahydrofuran solutions are studiedby size exclusion chromatography coupled with refractiveand light scattering detectors in combination withfluorescence spectroscopy. A considerable increase insegment density due to complexation compared with freePMMA chain is only slightly affected by the polymerconcentration in solution where stereocomplexes areformed. At polymer concentrations up to 3 x 10-3 g cm-3,an increase in non-uniformity of polymer complexmolecular weight and size and a shift to higher values ofboth are observed. In semidilute solutions stereocomplexesvirtually do not become heavier and larger. 6 refs.CZECH REPUBLIC

Accession no.806260

Item 117Polymer42, No.8, 2001, p.3859-66



STRUCTURE FORMATION DURING THEISOTHERMAL CRYSTALLISATION OFORIENTED AMORPHOUS POLY(ETHYLENETEREPHTHALATE) FILMSRadhakrishnan J; Kaito AJapan,National Institute of Materials & ChemicalResearch

A study was made of structure formation during theisothermal crystallisation of oriented, amorphous PETPfilm from the glassy state using in situ FTIR spectroscopy,in situ wide-angle X-ray diffraction and small angle X-ray scattering. The PETP films were prepared by rollingmelt quenched films to a draw ratio of 2 and an evaluationmade of the changes in the conformation and orientationorder of the PETP chains during crystallisation along withthe development of crystalline structure. Structureorganisation before and during isothermal crystallisationis discussed and a comparison made of the crystallisationbehaviour of oriented with that of isotropic PETP. 27 refs.JAPAN

Accession no.806185

Item 118Antec 2000.Conference proceedings.Orlando, Fl., 7th-11th May, 2000, paper 678USE OF CONTACT-ATOMIC FORCEMICROSCOPY IN PLASTIC MATERIALSURFACESReyes E; Guerrero CNuevo Leon,Universidad Autonoma(SPE)

Using thin films of isotactic polypropylene, poly(ethyleneterephthalate) and polystyrene, the range of atomic forcemicroscopy contact forces and the scanning frequenciesrequired to obtain sharp and clear 3-D images of polymersurfaces was determined, by systematically varying theseparameters, starting with typical values used for rigidsurfaces. The optimum values were determined to be acontact force of 88-150 nN, and a scanning frequency of1.0-1.5 Hz. 12 refs.MEXICO

Accession no.805686

Item 119Journal of Applied Polymer Science79, No.3, 18th Jan.2001, p.473-8PYROLYSIS GAS CHROMATOGRAPHICANALYSIS OF POLYACRYLONITRILEMinagawa M; Onuma H; Ogita T; Uchida HYamagata,University

In the pyrolytic gas chromatographic analysis (PGCA) ofacrylonitrile polymer under an inert atmosphere at 500-900deg.C, lower nitriles, including methyl cyanide, HCN, andacrylonitrile were the main degradation products, but lowerhydrocarbons, e.g. methane and ethylene, resulting fromsecondary decomposition, were also detected. Thermo-

analytical data, including data on the relation betweenretention time and nitrile polarity, and the limiting yield onpyrolysis as a function of temperature were obtained. Onthe basis of these results, specific applications of PGCA andthe usefulness of this method for studying the thermaldegradation of acrylonitrile polymer are indicated. 20 refs.JAPAN

Accession no.804442

Item 120West Conshohocken, Pa., 2000, pp.3. NALOANASTM D 3465-. TEST METHOD FOR PURITY OFMONOMERIC PLASTICISERS BY GASCHROMATOGRAPHYAmerican Society for Testing & MaterialsASTM D 3465-

Version 2000. Photocopies and loans of this documentare not available from Rapra.USA

Accession no.801052

Item 121Polymer News25, No.10, Oct.2000, p.359-60ANALYSIS OF AIRCRAFT COATING BYSECONDARY ION MASS SPECTROSCOPYUsmani A M; Donley MUDC; Wright-Patterson Air Force Base

An analysis was made of a flat aircraft coating usingsecondary ion mass spectroscopy, which revealed that thecoating was a polyurethane C type based on isophoronediisocyanate, diethylene glycol and adipic acid. X-rayphotoelectron spectroscopy was employed to determinepigments and extenders. 10 refs.USA

Accession no.800157

Item 122Antec 2000.Conference proceedings.Orlando, Fl., 7th-11th May, 2000, paper 441THERMODYNAMIC AND KINETIC ANALYSISOF SEMICRYSTALLINE RECYCLATES BY DSCCassel R B; Li LPerkin-Elmer Inc.(SPE)

Developments in differential scanning calorimetry (DSC)for the characterisation of semicrystalline thermoplastics,including mixed recyclates are discussed. The techniquesinclude stepwise DSC for the accurate determination ofspecific heat capacity, rapid determination of crystallinityusing the Gray-Mathot total enthalpy technique, andanalysis of crystallisation kinetics. The techniques showthe influence of impurities on the glass transitiontemperature, crystallinity and crystallisation. 6 refs.USA

Accession no.799956



Item 123Antec 2000.Conference proceedings.Orlando, Fl., 7th-11th May, 2000, paper 439NOVEL TECHNIQUE FOR THE DETECTION OFA HINDERED AMINE LIGHT STABILIZER(HALS), BASED ON SILICON TECHNOLOGYNarayan S; Lee R E; Hallberg D; Malatesta VGreat Lakes Chemical Corp.; Great Lakes ChemicalItalia(SPE)

A technique for the determination of HALS inpolypropylene was developed. The HALS, based on apolysiloxane backbone with tetramethyl piperidine sidechains, was melt blended with the polypropylene whichwas then spun into fibres. The chopped fibres weredissolved in toluene, the polymer precipitated usingmethanol, and the filtrate dried. A solution of the filtratewas then prepared and analysed by proton nuclearmagnetic resonance spectroscopy. The peak at 0.1 ppmwas attributed to the methyl group on the silicon atom ofthe HALS, and was used for quantitative purposes.Polypropylene pellets were also prepared containing alower concentration of HALS, which was subsequentlysubjected to direct extraction to prevent the loss whichmay occur during polymer reprecipitation. 3 refs.USA

Accession no.799954

Item 124Antec 2000.Conference proceedings.Orlando, Fl., 7th-11th May, 2000, paper 438ANALYTICAL METHODOLOGIES EMPLOYEDIN A COMPREHENSIVE FDA FOOD CONTACTCOMPLIANCE INVESTIGATION: ANALYSISFOR RESIDUAL MONOMERS, RESINOLIGOMERS, ADDITIVES AND MODIFIERS INSEVERAL FOOD SIMULATING SOLVENTSEberhard J S; McCort-Tipton M MCovance Laboratories(SPE)

The FDA considers that materials which come into contactwith food, such as processing machinery and packaging,to be indirect food additives, and the potential migrationof materials into the food requires determination. Ethanol/water solutions and food oils are commonly used as foodsimulating solvents when determining migration. Thesubsequent determination of the migrating species (whichmay include residual monomers, oligomers, additives andmodifiers) may be by liquid and gas chromatography, andmass spectroscopy.USA

Accession no.799953

Item 125Polymer42, No.4, 2001, p.1449-59

PHASE SEPARATION IN MISCIBLE POLYMERBLENDS AS DETECTED BY MODULATEDTEMPERATURE DIFFERENTIAL SCANNINGCALORIMETRYDreezen G; Groeninckx G; Swier S; Van Mele BLeuven,Catholic University; Brussels,Free University

The phase separation of two partially miscible polymerblends was studied using modulated temp.DSC(MTDSC). The lower critical solution temp.demixing behaviour of PEO blended with polyethersulphone(PES) and with poly(3,4'-diphenylene etherisophthaloyl amide), as determined by cloud point temps.with optical microscopy, was in good agreement withresults obtained from non-isothermal MTDSCmeasurements. The non-isothermal MTDSC apparentheat capacity evolution was time-dependent. It wasinfluenced by the endothermic demixing enthalpy and,in the case of PEO/PES blends, by the vitrification of ahigh-Tg phase formed. Quasi-isothermal MTDSCmeasurements contained information on the kinetics ofdemixing and remixing, emphasising the added valueof MTDSC to follow in situ the diffusion-controlledphase separation processes of partially miscible polymerblends. 32 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;WESTERN EUROPE

Accession no.798922

Item 126Macromolecular Materials and EngineeringVol.283, Nov.2000 p.153-62CHARACTERIZATION OF FLAME-SPRAYEDPEEK COATINGS BY FTIR-ATR, DSC ANDACOUSTIC MICROSCOPYSimonin L; Liao HCREST; Belfort-Montbeliard,Universite deTechnologie

Poly (aryl ether ether ketone) (PEEK) was utilised as aname-sprayed coating because of its good mechanicalproperties, low friction coefficient and high thermalstability. Fine polymeric powders were warmed up inoxyacetylene flame and sprayed onto a previously heatedaluminium substrate. Investigation of the degree ofcrystallinity of PEEK coatings was carried out usingdifferential scanning calorimetry (DSC), according tothe rate of cooling after the spraying process. Structuralmodifications were revealed by FTIR-ATR, attributedto interactions between the flame and the polymericpowders. Ultrasonic methods were developed, especiallyacoustic microscopy, to study the variations ofmechanical properties at the surface and the defectsinside the material. In general terms, flame-sprayedcoatings contain a large amount of porosity. Particularlysuited to the observation of large defects (exceeding 50microns) inside the polymeric materials is low-frequencymicroechography, a non-destructive technique. 19 refs.

Accession no.798668



Item 127Polymer Preprints, Volume 40, Number 2, August1999, Conference proceedings.New Orleans, La., August 1999, p.1043-4MALDI/TOF/MS STUDY OF HOMOPOLYMERSAND AMPHIPHILIC DIBLOCK COPOLYMERSBASED ON SULPHONATED POLYSTYRENEYang A; Nonidez W K; Mays J WBirmingham,University of Alabama(ACS,Div.of Polymer Chemistry)

Matrix-assisted laser desorption ionisation time of flightmass spectroscopy (MALDI/TOF/MS) provides a newway to probe polymers; it can provide information onmolecular weight, molecular weight distribution, massof end groups and mass of repeating units. Furtherinformation, such as reactivity ratios, individual blockchain length and its distribution, etc., can be obtainedbased on mass information. Polystyrene sulphonic acidand its sodium salt form have been successfullycharacterised by MALDI/TOF/MS, but no MALDI/TOF/MS study of diblock copolymers containing a polystyrenesulphonic acid block appears to be evident. The resultsof such a study of amphiphilic diblock copolymers,NaPSS-b-PtBS, and their precursors, PSb-PtBS, arereported. Number-average and weight-average molecularweights (Mn and Mw), polydispersity indices and extentsof sulphonation are obtained. 13 refs.USA

Accession no.798428

Item 128Polymer Degradation and Stability71, No.1, 2001, p.123-34QUALITY-DETERMINATION OF RECYCLEDPLASTIC PACKAGING WASTE BYIDENTIFICATION OF CONTAMINANTS BY GC-MS AFTER MICROWAVE ASSISTEDEXTRACTION (MAE)Camacho W; Karlsson SSweden,Royal Institute of Technology

The resulted are reported of an investigation into thequality of recycled HDPE and PP separated from mixedmunicipal solid waste carried out using gaschromatography-mass spectrometry. The development ofa simple and rapid microwave assisted extraction methodfor the systematic analysis of low molec.wt. compounds,such as decomposition products and additives, inpolymers is also reported and successfully applied to theanalysis of contaminants in the above recycled plastics.15 refs.EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERNEUROPE

Accession no.796627

Item 129Polymer Degradation and Stability70, No.2, Nov.2000, p.269-75

RAMAN SPECTRAL MAPPING OFPHOTOOXIDISED POLYPROPYLENEBlakey I; George G AQueensland,University of Technology

The photooxidation of unstabilised, isotactic PP wasinvestigated using Raman spectral mapping incombination with SEM/energy dispersive X-ray analysis,which permitted the determination of Ziegler-Nattacatalyst residue distribution throughout the PP. It wasfound that oxidation was heterogeneous at a microscopicscale and that a high local concentration of catalystresidues resulted in the stabilisation of the polymer in theimmediate vicinity and the formation of mobile reactivespecies, which initiated oxidation at sites away from thecatalyst. 30 refs.AUSTRALIA

Accession no.795269

Item 130Macromolecules33, No.19, 19th Sept.2000, p.7088-92SOLUTION CARBON-13 NMRCHARACTERIZATION OF NYLON 66:QUANTITATION OF CIS AMINECONFORMERS, ACID AND AMINE GROUPS,AND CYCLIC UNIMERSSouthern Mississippi,UniversityEdited by: Davis R D; Steadman S J; Jatterr W L;Mathias L J

Using a mixed 2,2,2-trifluoroethanol/deuteriochloroformsolvent system, well-resolved solution carbon-13 NMRspectra of nylon-66 samples were obtained which showedseveral low intensity peaks which were not seen in moreacidic solvents. The low intensity peaks were correlatedwith the methylene carbons near cis amide conformers,acid and amine end groups and within cyclic oligomers.The quantitative contents of these components for atypical nylon-66 sample were 1.1 mol% cis amideconformers, 1.0 mol% acid end groups and 0.5 mol%amine end groups. From end group concentrations, thenumber-average molecular weight of the nylon-66 wascalculated to be 30 177 g/mol. The chemical shift valuesof methylene carbons in the end groups and in cyclicoligomers was pH sensitive and thus depended on therelative concentrations of acid and amine groups in eachsample. 12 refs.USA

Accession no.794402

Item 131Polymer Engineering and Science40, No.11, Nov.2000, p.2442-55EVALUATION OF THREE METHODS FOR THEMEASUREMENT OF CRYSTALLINITY OF PETRESINS, PREFORMS, AND BOTTLESBashir Z; Al-Aloush I; Al-Raqibah I; Ibrahim M



SABIC R & D

The crystallinity of PETP resins, preforms and bottles wasinvestigated using DSC, modulated DSC and densitymeasurements. The PETP employed was a bottle-gradePETP copolymer containing 1.5% isophthalic acid. Theaccuracy, precision and validity of the techniquesemployed were evaluated and problems encountered ininterpreting the results assessed. 47 refs.SAUDI ARABIA

Accession no.793608

Item 132Kautchuk und Gummi Kunststoffe53, No.10, Oct.2000, p.574/81GermanDIRECT ANALYSIS OF ADDITIVES INPOLYMERIC MATERIALS BY PYROLYSIS-GASCHROMATOGRAPHY-MASS SPECTROMETRYMeyer-Dulheuer T; Pasch H; Geissler MDeutsches Kunststoff-Institut

This article describes the direct analysis of additives bypyrolysis-gas chromatography-mass spectrometry. Usingthis method it is possible to identify additives quicklyand reliably without separation of the polymer matrix. Asmall specimen of the sample is pyrolysed, i.e. degradedunder inert gas atmosphere. The pyrolysis products areseparated by gas chromatography and ionised in the massspectrometer by electron-impact ionisation. By comparingthe results with library data it is possible to identifyunknown additives unambiguously and with highaccuracy. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.792613

Item 133Journal of Thermal Analysis and Calorimetry61, No.2, 2000, p.589-96CALORIMETRIC ANALYSIS OF AN ISOTACTICPOLYPROPYLENE GAMMA-IRRADIATED INVACUUMSpadaro G; Valenza APalermo,University

The molecular modifications induced in an isotactic PPgamma-irradiated in vacuum under a complete set ofexperimental conditions are studied by means of calorimetricanalysis. The influence of the irradiation parameters, the totalabsorbed dose, D, and the dose rate, I, has previously beenanalysed and a simple kinetic model based on the rates ofthe main reactions occurring during irradiation, i.e. beta-scission, addition to double bonds and termination, was alsodiscussed. It is shown how thermal analysis confirms themodel forecasts and in particular the existence of the‘inversion conditions’: below them the main effect ismolecular degradation, while above them the main effectsare chain-branching and crosslinking. 12 refs.

EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.792350

Item 134ICAC 99. Conference proceedings.Bristol, UK, 23rd-24th Sept.1999, p.133-43IDENTIFICATION OF KEY CURE STAGES INLIQUID MOULDING PROCESSES BYPARALLEL PLATE DIELECTRIC ANALYSISMcIlhagger A T; Matthews S T; Brown D; Hill BUlster,University(IOM Communications Ltd.; Ulster,University;IMechE)

The aerospace industry has recognised the major benefitsassociated with fibre reinforced composite materials. Themore popular techniques available for compositeproduction are the traditional wet lay-up or autoclave andresin transfer moulding (RTM). Efforts to further reduceprocessing time and improve part quality have focusedon improved process control. To date this has been basedon off-line techniques. The need for on-line curemonitoring is widely recognised and this will require thedevelopment of suitable in-mould sensors. TheEngineering Composites Research Centre (ECKE) hasinvestigated and concentrated on the specific problemsencountered in the aerospace industry. Of the availablecure monitoring methods, parallel plate dielectric analysis(DEA) appears to offer the greatest potential fordetermining the through-thickness cure state of the resinduring cure. A laboratory dielectric instrument is utilisedto simulate RTM and autoclave cure cycles for compositestructures containing non-conductive and conductivefibres and for different resin systems used in the aerospaceindustry. Key resin cure stages are identified by anappropriate dielectric signal and correlated with data fromother thermal and mechanical techniques. Insulatedparallel plate dielectric sensors are being developed foruse in the laboratory instrument with the potential forincorporation into composite production tooling. 26 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.790059

Item 135Polymer Journal (Japan)32, No.7, 2000, p.610-5INFRARED SPECTROSCOPIC ANDMODULATED DIFFERENTIAL SCANNINGCALORIMETRY STUDY OF PHYSICAL AGINGIN BISPHENOL A POLYCARBONATEJin Lu; Yong Wang; Deyan ShenAcademia Sinica

FTIR spectroscopy was used to study the conformationalchanges in quenched bisphenol A polycarbonate filmsduring physical ageing. The conformation changedgradually from the high energy trans-cis conformation to



the low energy trans-trans conformation on sub-glasstransition temperature annealing. In-situ FTIR studies onthe conformational changes of films quenched from therubbery and sub-glass transition temperature annealed fordifferent times were carried out while increasing thetemperature through the glass transition region. Theresults indicated that incremental changes in thepopulation of trans-cis conformers in the quenched samplewere gradual, whereas rather abrupt changes occurred inthe sub-glass transition temperature annealed samples.The energy absorbed during the abrupt conformationalchange represented only part of the endothermic peakobserved by modulated DSC. The authors concluded thatsome new cohesional entanglements may be formedduring physical ageing. 28 refs.CHINA

Accession no.789734

Item 136Polymer Journal (Japan)32, No.7, 2000, p.560-6CALORIMETRIC AND INFRAREDSPECTROSCOPIC ANALYSIS OF MULTIPLEMELTING ENDOTHERMS OFPOLY(ETHYLENE TEREPHTHALATE)Yong Wang; Jin Liu; Deyan ShenChinese Academy of Sciences

The multiple melting behaviour of PETP was studiedusing DSC, FTIR spectroscopy and temperaturemodulated DSC by examining PETP samples subjectedto special schemes of crystallisation and annealingtreatment at different temperatures. On one-step and two-step annealing, a series of multiple endothermic minorpeaks was observed, resulting from the melting ofimperfect crystals during crystallisation. Both dualmorphology and melting-recrystallisation-remeltingmechanisms were probably responsible for the observedmultiple melting behaviour which was dependent on thethermal history of the PETP samples. 34 refs.CHINA

Accession no.789727

Item 137Analytical Chemistry72, No.19, 1st Oct.2000, p.4550-4GPC SEPARATION OF POLYMER SAMPLESFOR MALDI ANALYSISHanton S D; Liu X MAir Products & Chemicals Inc.; Lab Connections Inc.

MALDI mass spectrometry was combined with GPCanalysis for broad polydispersity polymers with the useof liquid chromatography interface. Results for PMMAwere compared with a blend of five narrow PMMAstandards that mimic the broad dispersed material. 24 refs.USA

Accession no.789529

Item 138Polymers Paint Colour Journal190, No.4432, Sept.2000, p.25-6WATCHING PAINT DRYMiddleton J

The development of nuclear magnetic resonance imaging,a technique previously only used in medicine, to providevarious information, including the drying rate, positionof water and curing in waterborne coatings, is discussed.The principles of magnetic resonance imaging are outlinedand work conducted at Surrey University in conjunctionwith Resonance Instruments to design equipment forcoatings analysis is described.

SURREY,UNIVERSITY; RESONANCEINSTRUMENTSEUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.789465

Item 139Journal of Applied Polymer Science78, No.5, 31st Oct.2000 p.1009-16CRYSTALLIZATION OF LOW-DENSITYPOLYETHYLENE- AND LINEAR LOW-DENSITYPOLYETHYLENE-RICH BLENDSDrummond K M; Hopewell J L; Shanks R ARMIT University

Using differential scanning calorimetry (DSC) thecrystallisation of a series of low-density polyethylene(LDPE)- and linear low-density polyethylene (LLDPE)-rich blends was examined. After continuous slow coolingDSC analysis showed a broadening of the LLDPE meltpeak and subsequent increase in the area of a secondlower-temperature peak with increasing concentration ofLDPE. Melt endotherms following stepwisecrystallisation (thermal fractionation) detailed the effectof the addition of LDPE to LLDPE, showing a nonlinearbroadening in the melting distribution of lamellae, acrossthe temperature range 80-140 degrees Celsius, withincreasing concentration of LDPE. A rise in the populationof crystallites melting in the region between 110 and 120degrees Celsius, a region was observed where as a purecomponent LDPE does not melt. A decrease in thecrystallite population over the temperature range whereLDPE exhibits its primary melting peaks (90-110 degreesCelsius) was noted, indicating that a proportion of thelamellae in this temperature range (attributed to eitherLDPE or LLDPE) were shifted to a higher melttemperature. 30 refs.

Accession no.789066

Item 140Polymer International49, No.9, Sept.2000, p.1007-13USING SPECTROSCOPY WITHCHEMOMETRICS TO MEASURE POLYMER



MOLAR MASSShenton M J; Herman H; Stevens G CSurrey,University

The ability to determine the molar mass of a polymer isof fundamental importance to describe polymer molecularcharacteristics. Conventional methods for measuringmolar mass include viscometry, osmometry, lightscattering and analytical gel permeation chromatography.Although high quality data can be obtained by thesemethods, the results can be significantly affected bysample preparation, and they are often time consumingand unsuitable for real-time on-line processing. Thepotential of determining polymer molar mass using opticalspectroscopy combined with chemometric analysis isdemonstrated. This is technically attractive becauseoptical spectroscopy is routinely used to collect processdata on-line and some refineries routinely monitor andcontrol blending using near-infrared spectroscopy. Acomparable development to monitor polymer molarmasses on-line from systems already being used tomeasure density and melt index, would be of potentialvalue to many sectors of the polymer production andprocessing industry. Chemometrics is a multivariatemethodology that allows the information from entirespectra to be used; it can be considered as a maximalcompression technique. Extracted ‘factors’ can then beregressed against property data by using a well-characterised set of ‘training’ samples to producepredictive regression models. It is shown that simplespectroscopic methods, such as the Raman techniquediscussed, when coupled with chemometrics, are capableof providing molar mass and distribution information.This is illustrated with reference to polydimethylsiloxanesin the liquid phase. 18 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.787562

Item 141Composite Interfaces7, No.2, 2000, p.81-92INVESTIGATING INTERPHASEDEVELOPMENT IN WOOD-POLYMERCOMPOSITES BY INVERSE GASCHROMATOGRAPHYRials T G; Simonsen JUSDA; Oregon,State University

The influence of secondary interactions on thedevelopment of interfacial structure in composites ofwood and amorphous thermoplastic polymers is not wellunderstood. Inverse gas chromatography is used toinvestigate the effect of different polymers on the surfaceenergy of partially or fully coated white pine wood meal.In this way, the development of the interphase ismonitored as a function of polymer depth on the woodsurface. The polymers are selected to provide a range offunctional groups and include PS, PMMA, PVC,

polymethacrylic acid and polymethacrylonitrile. Theoverall variation of the dispersive component of thesurface energy and the ratio of acceptor to donorcoefficients appear to group themselves into twocategories based upon the polarity of the polymer’sfunctional groups. In addition, the high loadings requiredfor stabilisation of the less polar polymers suggest that arelatively large volume of the matrix phase isaffected bythe wood filler. 20 refs.USA

Accession no.786897

Item 142Polymer Science Series B42, Nos.5-6, May-June 2000, p.169-74IR SPECTROSCOPY STUDY OF POLYMERPOROSITYPakhomov P M; Kruglova E V; Khizhnyak S DTver,State University

IR spectroscopic method is developed for evaluating theporosity (concentration and size of pores) in polymers.PE and PAN films of various porosity are prepared fromthe solutions in liquid and solid paraffins. Theconcentration and maximum pore size in the bulk and ina surface layer of the samples are determined by IRspectroscopy in the transmission and reflection modes,respectively. The results obtained are in agreement withthe data of optical and atomic force microscopy. 12 refs.RUSSIA

Accession no.786845

Item 143Iranian Polymer Journal9, No.2, April 2000, p.117-24STUDY OF CRYSTALLINITY OF HIGH-DENSITY POLYETHYLENE BY INVERSE GASCHROMATOGRAPHYGhaemy M; Hadjmohammadi M R; Tabaraki RMazandaran,University

The crystallinity of HDPE (Poliran-HD0035 and Irapol-5620) was investigated using inverse gas chromatography.The effects of flow rate of carrier gas and sample size onpeak retention volume and of the amount of injection onretention volume were evaluated. Retention diagrams anddegrees of crystallinity of the HDPEs were determinedand compared with those of LDPE. 15 refs.IRAN

Accession no.786383

Item 144Journal of Applied Polymer Science77, No.7, 15th Aug.2000, p.1419-31CURE MODELING AND MONITORING OFEPOXY/AMINE RESIN SYSTEMS. 1. CUREKINETICS MODELING



Karkanas P I; Partridge I KCranfield,University

An investigation using differential scanning calorimetrywas carried out under both isothermal and dynamic curingconditions to determine the cure kinetics of four epoxy/amine resins. Various cure kinetic models were used tocompare them with the results of the DSC results. Goodfits were found, in good agreement with the experimentalresults for the resin systems. 22 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.786048

Item 145International Polymer Science and Technology27, No.6, 2000, p.T/7-T/9. (Translation of Muanyag esGumi, No.3, 2000, p.89)APPLICATION OF STATE-OF-THE-ARTMETHODS IN ADHESION TECHNOLOGY. 1Vabrik R; Czajlik I; Bertoti I; Keresztes Z; Ille A;Rusnak I; Vig A; Kalman E

The use is demonstrated of microscopic analysistechniques for the investigation of adhesive failure. PVCsheet was bonded to glass using a M35R hybrid UVcurable adhesive based on epoxy resin. Atomic forcemicroscopy and X-ray induction photoelectronspectroscopy were used for the chemical characterisationof of failure surfaces. 11 refs.EASTERN EUROPE; HUNGARY

Accession no.785593

Item 146Journal of Applied Polymer Science78, No.1, 3rd Oct. 2000, p.166-72EFFECT OF POLY(VINYL CHLORIDE)/CHLORINATED POLYETHYLENE BLENDCOMPOSITION ON THERMAL STABILITYKlaric I; Vrandecic N S; Roje USplit,University

The miscibility of PVC and chlorinated PE and the effectof the blend composition on the heat stability of the PVCwere investigated using several techniques, includingTGA and DSC. The apparent activation energy of PVCdehydrochlorination in the blends was calculated andexperimental TGA curves compared with those predictedusing the additivity rule. It was found that the blends wereheterogeneous and that addition of chlorinated PE in aspecific temperature range resulted in an improvementin the heat stability of the PVC. 22 refs.CROATIA

Accession no.784861

Item 147Polymer41, No.22, Oct.2000, p.8161-5

APPLICATION OF MODULATED-TEMPERATURE DIFFERENTIAL SCANNINGCALORIMETRY TO THE STUDY OFCRYSTALLISATION KINETICS IN POLY(E-CAPROLACTONE)-POLY(STYRENE-COACRYLONITRILE) BLENDSSong M; Hourston D JLoughborough,University

In order to evaluate the application of modulated-temperature differential scanning calorimetry (M-TDSC)to the study of the crystallisation kinetics of semi-crystalline polymers, isothermal crystallisation kineticsin poly(e-caprolactone)-SAN blends are investigated. Thetemperature dependence of d ln G/dT (G =crystal growthrate), determined by M-TDSC agrees approximately withprevious experimental data and theoretical values. Thesewere obtained from direct measurements of spherulitegrowth rate by optical microscopy. Here, theoretical andM-TDSC experimental results show that the d ln G/dTversus temperature plots are not sensitive to the non-crystalline component in the poly(e-caprolactone)-SANblends. 15 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.784242

Item 148Polymer41, No.22, Oct.2000, p.8151-4PORE DIMENSION OF WATER TREES IN PE:NMR STUDIESJudeinstein P; Carmo Lanca M; Marat-Mendes J; Rault JParis-Sud,Universite; Portugal,Universidade Nova deLisboa

In PE films aged under electric field the crystallisation ofwater (and melting of ice) is studied by quadrupolar NMR,this technique allows determination of water concentrationas low as 10 -4. It is shown that the pore dimensions ofthe tracks forming the water trees of the order of 2.5 nmare independent of the ageing time. The mobility of waterin these water trees and in porous glass, of similar poredimensions, are compared. 17 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;PORTUGAL; WESTERN EUROPE

Accession no.784240

Item 149Journal of Applied Polymer Science77, No.10, 6th Sept.2000, p.2178-8CURE MODELLING AND MONITORING OFEPOXY/AMINE RESIN SYSTEMS. II.NETWORK FORMATION ANDCHEMOVISCOSITY MODELLINGKarkanas P I; Partridge I KCranfield,University

The glass transition temperature (Tg) advancement andthe chemoviscosity development under isothermal



conditions are investigated for four epoxy/amine systems,including commercial RTM6 and F934 resins. Differentialscanning calorimetry is the thermoanalytical techniqueused to determine the Tg advancement, and rheometryfor determination of the chemoviscosity profiles of theseresin systems. The complex cure kinetics are correlatedto the Tg advancement via a one-to-one relationship usingDi Benedetto’s formula. It is revealed that the three-dimensional network formation follows a single activatedmechanism independent of whether the cure kineticsfollow a single or several activation mechanisms. Theviscosity profiles show the typical characteristics ofepoxy/amine cure. A modified version of the Williams-Landel-Ferry equation (WLF) is adequate to model theviscosity profiles of all the resin systems, in thetemperature range 130 to 170 deg.C, with a very gooddegree of accuracy. The parameters of the WLF equationare found to vary in a systematic manner with curetemperature. Further correlation between Tg and viscosityshows that gelation, defined as the point where viscosityreaches 10 4 Pas, occurs at a unique Tg value for eachresin system, which is independent of the cure conditions.16 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.784172

Item 150Fire & Materials24, No.2, March/April 2000, p.101-12SMOKE GAS ANALYSIS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY -SUMMARY OF THE SAFIR PROJECT RESULTSHakkarainen T; Mikkola E; Laperre J; Gensous F;Fardell P; Le Tallec Y; Bajocchi C; Paul K; SimonsonM; Deleu C; Metcalfe EVTT Building Technology; Centexbel; Elf AtochemSA; UK,Building Research Establishment; CEMATE;LSF SUD srl; Rapra Technology Ltd.; Sweden,NationalTesting & Research Institute; Ghent,University;Greenwich,University

The determination of toxic components from fire gasesis difficult because the environment is hot, reactions areoften temperature dependent, and a lot of soot may beproduced. Due to the different properties of the gascomponents, a different time-consuming procedure foreach species has traditionally been used. The use of FTIR(Fourier transform infrared) spectrometers as a continuousmonitoring technique overcomes many of the problemsin smoke gas analyses. FTIR offers an opportunity to setup a calibration and prediction method for each gasshowing a characteristic spectral band in the infraredregion of the spectrum. The objective of the SAFIR projectwas to further develop the FTIR gas analysis of smokegases to be an applicable and reliable method for thedetermination of toxic components in combustion gasesrelated to fire test conditions. The optimum probe design,

filter parameters and the most suitable sampling lines interms of flow rate, diameter, construction material andoperating temperature have been specified. In the largescale, special concern was given to the probe design andthe effects of the probe location as well as practicalconsiderations of the sampling line length. Quantitativecalibration and prediction methods have been constructedfor different components present in smoke gases.Recommendations on how to deal with interferents, non-linearities and outliers have been provided and averification method for the spectrometer for unexpectedvariations and for the different models have beendescribed. FTIR measurement procedures in different firetest scenarios are studied using the recommendations ofthis project for measurement techniques and analysis andan interlaboratory trial of the FTIR technique in smokegas analysis is carried out to define the repeatability andreproducibility of the method in connection with a smallscale fire test method, the cone calorimeter. 9 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;FINLAND; FRANCE; ITALY; SCANDINAVIA; SWEDEN; UK;WESTERN EUROPE

Accession no.784096

Item 151Polymer41, No.23, Nov.2000, p.8241-5USE OF RAMAN SPECTROSCOPY TO STUDYTHE REACTION BETWEEN AN AMINE-TERMINATED THERMOPLASTIC AND EPOXYRESINSvan Overbeke E; Carlier V; Devaux J; Carter J T;McGrail P T; Legras RLouvain,Universite Catholique; ICI Plc

Reactive thermoplastics are often used as tougheningmodifiers for epoxy resins. Raman spectroscopy was usedto follow the reaction of aromatic amines with epoxidemonomers through the evolution of an amine-substitutedaromatic vibration. A double shift of this peak was correlatedwith the formation of secondary and tertiary amines. Bandassignment was confirmed by the study of modelcompounds. Using this method, qualitative observation ofthe reaction between an amine-terminated copolyether-sulphone thermoplastic and epoxide was performed.Unfortunately, in the blend studied containing the curingagent, a band appearing upon curing overlapped with theband characterising the end group reaction. 17 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; WESTERN EUROPE

Accession no.783075

Item 152Polymer Degradation and Stability68, No.3, 2000, p.437-43SEMI-QUANTITATIVE ANALYSIS OFTHERMAL DEGRADATION INPOLYPHENYLENE ETHER



Kinoshita M; Nemoto T; Souda T; Takeda KKoito Mfg.Co.Ltd.; Shibaura,Institute of Technology

The use of simple computer simulation and analysis ofthe thermal degradation products of differently thermallyaged samples of melt processed polyphenylene ether filmgave information on possible degradation routes for thispolymer. An increase in dimeric products was noted withincreased thermal ageing, but not in monomeric products.To explain the distribution of scission products foundexperimentally, the simple computer model was arrangedto simulate cleavage rates of methylene bridge, ether andsidechain links. Although results were not totallyconclusive, it was noted that both ether bridge and sidechain cleavage rates were similar, and approximately ninetimes lower than cleavage rates of the methylene bridge.It is suggested that quantitative results determined willgive detailed information on flame retardance due to theunderstanding of rates of volatile product generation atthe polymer surface. 28 refs.JAPAN

Accession no.782776

Item 153Polymer Degradation and Stability68, No.3, 2000, p.321-6COMPARATIVE ANALYSIS OF THE PHOTO-OXIDATION OF POLYSTYRENE ANDPOLY(ALPHA-METHYLSTYRENE)Mailhot B; Jarroux N; Gardette J-LEnsemble Universitaire des Cezeaux

Fourier transform infrared spectroscopy (FTIR) and massspectroscopy were used to study the photo-oxidation ofboth poly(alpha-methylstyrene) (PMS) and polystyrene(PS) films which had been irradiated at differenttemperatures and with different radiation sources underan oxygen atmosphere. The oxidised films were treatedwith ammonia or sulphur tetrafluoride and photolysiscarried out under vacuum. Photoproducts from bothpolymers were broadly similar, but aromatic ketoneconcentration was higher from the PMS and a new ketonewas also identified from this source. Routes for formationof identified photoproducts are proposed. 13 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.782763

Item 154ACS, Polymeric Materials Science & Engineering FallMeeting 1999. Volume 81. Conference proceedings.New Orleans, La., 22nd-26th Aug.1999, p.242-3ANALYSIS OF THE NANOPHASE STRUCTUREOF SEMICRYSTALLINE POLYMERS WITHATOMIC FORCE MICROSCOPY (AFM),MICROCALORIMETRY (MC) ANDTEMPERATURE-MODULATEDCALORIMETRY (TMC)

Wunderlich BTennessee,University; Oak Ridge National Laboratory(ACS,Div.of Polymeric Materials Science & Engng.)

Semicrystalline, polymeric materials consist usually ofmetastable aggregates of strongly coupled microphases ornanophases with their constituent, micrometre-long, flexiblemolecules traversing multiple phase domains. Some 40 yearsago it was established that well-formed crystals are oftenlamellar with a thickness of only about 10 nm. Between theselamellae one can find the remaining amorphous phase witheven smaller dimensions. Less perfect crystallisation candecrease the crystal dimensions to as little as 1-2 nm in alldimensions. An operational definition of the microphase isits having at least one dimension smaller than a micrometre,while nanophases are approached when the small dimensionapproaches 10 nm. Characteristic of the microphases is theneed to consider the surface properties for their description,i.e. the melting temperature depends on the surface freeenergy. Nanophases, in turn, show an interaction betweenopposing surfaces, i.e. they may show no bulk properties. Ifthe dimensions decrease below 1 nm, the macroscopic phasedescription has reached its limit. Many macromolecules can,however consist of alternating sequences of nanometer-length chain segments that are immiscible, so that in all theirphase structures there is a strong tendency of nanophaseseparation. It is shown that special tools must be developedto probe the nanophase structures and properties of polymers.Some new information available by using three rather newtechniques their combinations are described. 10 refs.USA

Accession no.780666

Item 155ACS, Polymeric Materials Science & Engineering FallMeeting 1999. Volume 81. Conference proceedings.New Orleans, La., 22nd-26th Aug.1999, p.236-7CRYSTALLISATION AND MELTING OFPOLYMER CRYSTALS REVEALED BY T-M DSCToda A; Oda T; Tomita C; Hikosaka M; Arita T;Saruyama YHiroshima,University; Kyoto,Institute of Technology(ACS,Div.of Polymeric Materials Science & Engng.)

Temperature-modulated differential scanning calorimetry(T-MDSC) applies a thermal modulation in temperatureto a conventional DSC run and determines a dynamic heatcapacity from the relationship between the modulationcomponents of temperature and of heat flow. Primaryapplication of this technique has been the measurementof specific heat capacity and the examination of theanomaly in a relaxation process such as alpha processrelated to the glass transition. An application to the first-order phase transitions of crystallisation and melting ofpolymer crystals has recently been suggested. The methodand typical results are described. 13 refs.JAPAN

Accession no.780663



Item 156ACS, Polymeric Materials Science & Engineering FallMeeting 1999. Volume 81. Conference proceedings.New Orleans, La., 22nd-26th Aug.1999, p.173-4FILM FORMATION IN POLYMER LATEXBLENDS: MICROSPECTROSCOPIC 3D STUDIESZhao Y; Urban M WNorth Dakota State University(ACS,Div.of Polymeric Materials Science & Engng.)

A series of previous studies on latex films indicates thatmobility of low molecular weight species in particularsurfactant molecules, may be affected by latex glasstransition temperature, and subsequently, by free volumeof a polymer matrix, surface tension at the film/air andfilm/substrate interfaces, compatibility and coalescencetimes, to name just a few. It appears that there are otherfactors that not only influence distribution of individualcomponents including distribution of surfactants, but alsomay significantly affect film formation. In an effort toenhance understanding of these multi-phase latex blendsand their coalescence, a series of experiments on latexescontaining PS and poly-n-butyl acrylate (p-nBA) blendsis presented. An attempt is made to identify factorsaffecting film formation of PS/p-nBA latex blends usingmulti-dimensional vibrational spectroscopic methods, andthese findings are compared with respective copolymers.The effects of SDOSS exudation by latex composition,particle and annealing temperatures are also addressed interms of phase separation and dynamics ofmacromolecular segments. 21 refs.USA

Accession no.780632

Item 157ACS, Polymeric Materials Science & Engineering FallMeeting 1999. Volume 81. Conference proceedings.New Orleans, La., 22nd-26th Aug.1999, p.387-8FAILURE STUDIES OF ADHESION BY UVREFLECTION AND FLUORESCENCETECHNIQUESKim N-J; Jeong C N; Sung C S P; Sung N-HConnecticut,University; Tufts University(ACS,Div.of Polymeric Materials Science & Engng.)

Various techniques such as optical and electron microscopy,IR-ATR ESCA and SIMS have been used for failure modeanalysis in polymeric adhesive joints. However, thesetechniques are not amenable for in situ, non-destructiveexamination of the failure surfaces as failure occurs. Inorder to develop in situ techniques, UV reflection andfluorescence methods are evaluated, as they can be appliedvia optical fibres to the actual failure surface. Failuresurfaces of two types of adhesive joints are examined byUV reflection and fluorescence, complemented by FT-IRATR studies. The first joint studied is PU on epoxy-coatedsteel. The second is PETP/PE/PETP. 8 refs.USA

Accession no.780560

Item 158Analytical Chemistry72, No.11, 1st June 2000, p.2490-8CHARACTERISATION OF POLYETHER ANDPOLYESTER POLYURETHANE SOFT BLOCKSUSING MALDI MASS SPECTROMETRYMehl J T; Murgasova R; Dong X; Hercules D M;Nefzger HVanderbilt University; Bayer Corp.

Selective degradation reactions combined with MALDIanalysis were applied for molecular weight determinationof polyether and polyester polyurethane soft blocks. Sizeexclusion chromatography was combined with MALDI toprovide accurate molecular weight determination. 44 refs.USA

Accession no.778970

Item 159Macromolecular SymposiaVol.152, March 2000, p.267-78ANALYSIS OF COMPLEX POLYMERS BYMALDI-TOF MASS SPECTROMETRYPasch H; Ghahary RGerman Plastics Institute

The results are reported of an analysis of the functionality,molar mass and chemical composition of complexpolymers, using MALDI-TOF mass spectrometry and acombination of MALDI-TOF mass spectrometry andliquid chromatography. Polymers investigated includedpolyamide-12, bisphenol A polycarbonate, methoxylatedmelamine-formaldehyde resin, carboxy-terminated PSand PMMA. 33 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.778702

Item 160Journal of Injection Molding Technology4, No.2, June 2000, p.84-91ANALYSIS OF STYRENE PLASTIC RESIDUESON INJECTION MOULDING TOOLSMakinen M; Astola J; Poutanen J; Alen R; Paakkonen ETampere,University of Technology;Jyvaskyla,University

The contaminating substances formed during the injectionmoulding of ABS and PS parts were removed from themould surface. The residues were characterised usingFTIR, gas chromatography, pyrolysis gaschromatography, elemental analysis, detection reactiontest of bromine, and different dissolving tests. Thechemical composition of the contamination was clarifiedand suitable solvents for dissolving these products wereselected. 6 refs.EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERNEUROPE

Accession no.776471



Item 161Polymer41, No.15, 2000, p.5949-55UNDERSTANDING VITRIFICATION DURINGCURE OF EPOXY RESINS USING DYNAMICSCANNING CALORIMETRY ANDRHEOLOGICAL TECHNIQUESLange J; Altmann N; Kelly C T; Halley P JQueensland,University

The gelation and vitrification transitions during cure ofan epoxy resin-amine system were examined usingrheological, modulated DSC and FTIR techniques. Theresults of DMA showed that gelation was observed beforevitrification at all temps. where it could be rheologicallydefined. By comparing different rheological criteria forvitrification, it was seen that the vitrification transitionwas a gradual process that extended over a large part ofcure at all temps. where it occurred. Results frommodulated DSC measurements showed that thecalorimetric vitrification times were longer than thevitrification times obtained from rheologicalmeasurements at cure temps. above 100C, but that at lowertemps. calorimetric vitrification occurred before, or at thesame time as, rheological vitrification. Theoreticalgelation times, estimated from FTIR conversion data,were found to be consistently shorter than the observedgelation times. Theoretical vitrification times agreed wellwith the observed times. The magnitude of the vitrificationtransition, expressed either as amount of change in heatcapacity or as maximum value of loss tangent, was foundto decrease approximately linearly with increasing curetemp. 34 refs.AUSTRALIA

Accession no.776348

Item 162Macromolecules33, No.8, 18th April 2000, p.3180-3COMPLETE ASSIGNMENT OF PROTON ANDCARBON 13 NMR SPECTRA OFPOLYVINYLCARBAZOLEKarali A; Froudakis G E; Dais P; Heatley FCrete,University; Manchester,University

Details are given of the assignment of the proton andcarbon 13 spectra of polyvinylcarbazole by using anumber of modern gradient two-dimensional NMRexperiments. The relationship between the assignmentsand the conformational and dynamic properties of thepolymer is discussed. 13 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE; UK;WESTERN EUROPE

Accession no.776167

Item 163Journal of Thermal Analysis and Calorimetry59, Nos.1-2, 2000, p.409-24

CHARACTERISATION OF POLYURETHANECOATINGS USING THERMOANALYTICALTECHNIQUESGinic-Markovic M; Choudhury N R; Matisons J G;Williams D R GSouth Australia,University; Adelaide,University

A two-pack PU coating was analysed usingthermoanalytical techniques. The curing reaction wasmonitored using pressure differential calorimetry,rheometry and dynamic mechanical analysis. Thedecomposition behaviour was examined using TGA. 13refs.AUSTRALIA

Accession no.776090

Item 164Injection Molding8, No.6, June 2000, p.42/50MATERIALS ANALYST: PART 33 -DETERMINING COMPOSITIONSepe MDickten & Masch Mfg.

This article focuses on the problems associated withidentifying a polymer. There are three major techniquesthat are particularly helpful in identifying the type ofpolymer used in a compound. These are DSC, TGA andIR spectroscopy. Each of these techniques has itsstrengths, and in determining the composition of thepolymer, the task is to highlight properties and behaviourthat are distinctive.USA

Accession no.775805

Item 165Polymer41, No.11, 2000, p.4361-5RAPID MICROWAVE INDUCEDDEPOLYMERISATION OF POLYAMIDE 6Klun U; Krzan ALjubljana,National Institute of Chemistry

Polyamide 6 depolymerisation was performed usingmicrowaves as the energy source for the acid catalysedhydrolysis, with phosphoric acid as the catalyst. Theproduct mixture was analysed by chromatographic andspectroscopic methods. 19 refs.SLOVENIA

Accession no.774158

Item 166Polymer41, No.11, 2000, p.4039-46MATRIX-ASSISTED LASER DESORPTION/IONISATION MASS SPECTROMETRY OFSYNTHETIC POLYMERS. IV. COUPLING OFSIZE EXCLUSION CHROMATOGRAPHY AND



MALDI-TOF USING A SPRAY-DEPOSITIONINTERFACEEsser E; Keil C; Braun D; Montag P; Pasch HDarmstadt,Deutsches Kunststoff-Institut

Size exclusion chromatography and MALDI-TOF massspectrometry was coupled via a robotic interface. Forpolydisperse synthetic polymers a continuous track ofmatter was deposited onto the matrix surface. Spectrawere taken from different positions of the polymer track.Data are presented for PS, PMMA and butyl methacrylate-methyl methacrylate copolymers. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.774127

Item 167Muanyag es Gumi37, No.3, 2000, p.89-91HungarianAPPLICATION OF STATE-OF-THE-ARTMETHODS IN ADHESION TECHNOLOGY. I.Vabrik R; Czajlik I; Bertoti I; Keresztes Zs; Ille A;Rusznak I; Vig A; Kalman E

Atomic force microscopy (AFM) and X-ray photoelectronspectroscopy (XPS) were used to study the nature of thefailure interface and the failure mechanism in a PVC film/adhesive/glass system. The failure mode was found to bemostly interfacial, occurring at the glass/adhesive interface,and also partially cohesive, located in the adhesive layervery close to the interface. The results are discussed inrelation to the chemical nature of the interface and thefailure mechanism. 11 refs. Articles from this journal canbe requested for translation by subscribers to the Rapraproduced International Polymer Science and Technology.

Accession no.773793

Item 168Revista de Plasticos Modernos78, No.521, Nov.1999, p.541-6SpanishSTRUCTURAL CHARACTERISATION OFMULTILAYER POLYMERIC MATERIALS BYMICRORAMAN SPECTROSCOPYSanz R; Martin B; Merino J C; Pastor J MValladolid,Universidad

Results are presented of a study in which confocalmicroRaman spectroscopy was used to determine thestructure of the individual polymers present in a series ofmultilayer food packaging films. 8 refs.

AMCOR FLEXIBLES ESPANA SAEUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.773260

Item 169Iranian Journal of Polymer Science & Technology12, No.2, Summer 1999, p.1-8

PersianKINETIC STUDY OF THE AUTO-OXIDATIONOF POLYURETHANESemsarzadeh M A; Salehi HTarbiat Modarres University

Gel permeation chromatography was used to study thekinetics of the auto-oxidation of polyurethane. Thestationary state rate and the induction time weredetermined at various temperatures. FTIR and H NMRwere used to determine the alcohol, acetate and formatecompounds in the auto-oxidation products.IRAN

Accession no.773140

Item 170Journal of Macromolecular Science BB39, No.2, 2000, p.279-96TIME-RESOLVED FTIR STUDY OFCRYSTALLISATION BEHAVIOUR OF MELT-CRYSTALLISED POLYPHENYLENE SULPHIDEYu J; Asai S; Sumita MTokyo,Institute of Technology; China,TextileUniversity

The crystallisation behaviour of polyphenylene sulphidewas studied using time-resolved FTIR spectroscopy andthe results obtained correlated with DSC measurements.The 1073 cm/1 amorphous band was selected for the time-resolved measurements. The procedure provided detailson the microstructure of the PPS, including heterogeneityof the amorphous phase above and below Tg. A methodis proposed for calculating the rigid, amorphous fractionin terms of the increase in the slope of the absorbancevariation with temperature at the glass transition. 43 refs.CHINA; JAPAN

Accession no.772147

Item 171Journal of Applied Polymer Science76, No.6, 9th May 2000, p.938-46OPTIMIZATION OF EXPERIMENTALPARAMETERS FOR THE QUANTIFICATION OFPOLYMER ADDITIVES USING SFE/HPLCThilen M; Shishoo RSwedish Institute for Fibre & Polymer Research

A study was conducted with the aim of extracting theantioxidants Irganox 1010 and Irgafos 168 from a PPmatrix by using the supercritical fluid extraction(SFE)technique and by subsequent analysis using high-performance liquid chromatography(HPLC). Theexperimental parameters of temp., pressure and modifierswere varied to find the best extraction conditions. Theoptimum temp. and pressure for extraction of thesepolymer additives were found to be 120 and 384 bar, withmethanol as the modifier. The quantitative extractionswere significantly faster than those reported previouslyin the literature. The results showed that the SFE/HPLC



technique used in these experiments was a reliable andenvironmentally-friendly alternative to the commonly-used liquid extraction and analytical methods. 22 refs.EUROPEAN UNION; SCANDINAVIA; SWEDEN; WESTERNEUROPE

Accession no.770687

Item 172Macromolecular SymposiaVol.148, Dec.1999, p.463-81CHARACTERIZATION OF ACRYLIC DENTALPOLYMERSVera-Graziano R; Martinez-Richa A; Palacios-AlquisiraJ; Barcelo-Santana F; Castano-Meneses VMexico,Universidad Nacional Autonoma;Guanajuato,Universidad

The chemical composition, dimensions and the molecularparameters of four dental acrylic polymer materials andtwo polyacrylic acids of different molec.wt. used as modelcompounds were studied by NMR and IR spectroscopies,GPC, intrinsic viscosity and light scatteringmeasurements. Two of the dental polymers were shownto be mainly polyacrylic acid, while one showed the peakpattern for an acrylic acid/methyl acrylate copolymer ofabout 2:1 composition and one was an oligomer derivedfrom 2-hydroxyethyl methacrylate. The steric hindranceparameter, molecular stiffness and second virialcoefficient were calculated using different thermodynamicmodels. The Flory-Fox-Shafgagen and the Stockmayer-Fixman models fitted the experimental data reasonablywell and could be use to describe the molecular parametersof the acrylic polymers. 18 refs. (7th InternationalConference on Polymer Characterization (POLYCHAR-7), Denton, Texas, USA, Jan.1999)MEXICO

Accession no.770356

Item 173Flame Retardants 2000. Conference proceedings.London, 8th-9th Feb.2000, p.185-92PRACTICE OF FTIR ANALYSIS FOR FIREGASES (SAFIR)Mikkola EVTT Building Technology(BPF; Interscience Communications Ltd.; APME;European Flame Retardant Assn.; Fire RetardantChemicals Assn.)

The use of FTIR (Fourier transform infrared)spectrometers as a continuous monitoring techniqueovercomes many of the problems associated in analysesof hot fire gases. FTIR offers an opportunity to set up acalibration and prediction method for each gas showinga characteristic spectral band in the infrared region of thespectrum. A European project, SAFIR, aims to furtherdevelop the FTIR gas analysis of smoke gases to be anapplicable and reliable method for the determination oftoxic components in combustion gases related to fire test

conditions. Within this project, optimal workingconditions including sampling, calibration and analysisfor FTIR fire gas method are defined and verified undera variety of fire test scenarios. The FTIR method areshown to be a repeatable and reproducible method forthe determination of the most important toxic gascomponents of real fires. Moreover, the findings of thisproject concerning sampling techniques are most relevantfor other methods used for defining fire gases. 5 refs.EUROPEAN UNION; FINLAND; SCANDINAVIA; WESTERNEUROPE

Accession no.768669

Item 174Surface Coatings International83, No.3, March 2000, p.111-8DETERMINATION OF VOC EMISSIONS FROMLATEX PAINTS DURING AND AFTERAPPLICATION; METHODS, PERFORMANCEAND PRECISIONZeh HWacker Polymer Systems GmbH

VOC emissions from indoor latex paints during and afterapplication is determined by four different test methods:a chamber method in which an emission chamber iscombined with gas chromatography, two practicalmethods in which VOC emitted in a room is measuredeither by the determination of the total organic carbon orby infrared spectroscopy, and an ‘in-can-individual-VOCmethod’ which determines the VOC of a liquid paint bythe quantitative analysis of each volatile component. VOCemission data gathered by these methods are comparedwith calculations from a dynamic computer modeldescribing the time-dependence of the VOC emission inthe room atmosphere. This comparison indicates that the‘in-can-individual-VOC method’ with computercalculation allows variations in the size of the room, theapplication rate, VOC content of the paint and the rate ofair change, without the necessity of additionalexperiments, and therefor, offers an approach with areduction in costs. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.768107

Item 175Journal of Coatings Technology72, No.902, March 2000, p.53-61ACID ETCH OF AUTOMOTIVE CLEARCOATS.II. COMPARISON OF DEGRADATIONCHEMISTRY IN LABORATORY AND FIELDTESTINGSchmitz P J; Holubka J W; Xu L-FFord Motor Co.

X-ray photoelectron spectroscopy was used to determinewhether exposure conditions used in the laboratorygravimetric etch testing of acrylic melamine clearcoats



simulated field degradation pathways. The surfacechemistry of the field exposed panels was examined andthe results compared with those for laboratory treatedpowders having identical technologies. Consistency in theformation of a melamine salt and ammonium sulphateupon field exposure and laboratory acid treatmentindicated that the laboratory treatment conditionssimulated the field exposure conditions. 7 refs.USA

Accession no.767768

Item 176Journal of Adhesion Science and Technology14, No.5, 2000, p.745-64XPS ANALYSIS OF THE COVERAGE ANDCOMPOSITION OF COATINGS ON GLASSFIBRESThomason J L; Dwight D WOwens-Corning Science & Technology Center

The use of X-ray photoelectron spectroscopy as a methodfor characterising different sizings on glass fibres wasevaluated. A model, based on a patchy sizing overlayhypothesis, was developed to aid in the reduction of dataobtained from the X-ray photoelectron spectroscopicanalysis. It is shown that the spectroscopic results, whencombined with the weight fraction of the sizing, providea quantitative value for the coverage of the fibre surfaceby the sizing. 25 refs.USA

Accession no.767755

Item 177Polymer News25, No.2, Feb.2000, p.56-8POLYMER ANALYSIS ANDCHARACTERISATIONGarbassi FEniChem SpA

Analytical techniques, such as mass spectroscopy, atomicabsorption spectroscopy and atomic emissionspectroscopy, for the detection of trace elements, mainlymetal trace elements, in polymers, used particularly infood, are briefly considered. The disadvantages andsuitability of such techniques are summarised. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.766702

Item 178Adhesion ’99. Conference Proceedings.Cambridge, UK, 15th-17th Sept.1999, p.369-73INTERPHASE CHEMISTRY OF CARBON FIBRECOMPOSITE MATERIALSPrickett A C; Vickers P E; Smith P A; Watts J FSurrey,University(IOM Communications Ltd.)

The fibre-matrix interface in carbon fibre-reinforcedepoxy resin composites was studied by time of flightsecondary ion mass spectrometry (ToF-SIMS) using novelpreparation techniques. The initial adsorption betweenuncured resin or amine curing agent and the fibre wasinvestigated by the use of adsorption isotherms obtainedby the analysis of fibre surfaces following immersion inliquid solutions of the resin. The intact interphase of acomposite could be examined by ToF-SIMS followingmode I or mode II failure within the spectrometer by theuse of carefully designed in-situ fracture stages. 11 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.765326

Item 179Adhesion ’99. Conference Proceedings.Cambridge, UK, 15th-17th Sept.1999, p.347-50MICRO THERMAL ANALYSIS ATINTERPHASESHassler R; zur Muhlen EDresden,Institut fuer Polymerforschung; TAInstruments GmbH(IOM Communications Ltd.)

Details are given of a thermal analysis technique, referredto as micro thermal analysis, which combines the highresolution positioning of scanning probe microscopy withsome of the quantitative analysis capabilities of conventionalthermal analysis. The application of this technique incharacterising the thermal properties of interfaces inaluminium/epoxy resin adhesive joints and in glass fibre-reinforced epoxy resin composites is described. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;UK; WESTERN EUROPE

Accession no.765322

Item 180Macromolecules33, No.1, 11th Jan.2000, p.120-4BRANCHING AND CROSSLINKING INRADIATION-MODIFIED PTFE. A SOLID-STATENMR INVESTIGATIONFuchs B; Scheler UDresden,Institute of Polymer Research

High-resolution fluorine 19 NMR was used to investigatethe structural changes resulting from PTFE electronirradiation under vacuum. A quantitative analysis of thedata was used to establish the density of side groups andbranches. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.764731

Item 181Color and Appearance Retec 1999. Conferenceproceedings.



Nashville, Tn., 27th-29th Sept.1999, p. 178-87USING MICROSCOPY AS A PROBLEMSOLVING TOOL IN PLASTICSCompton CSun Chemical Corp.(SPE,Color & Appearance Div.)

Microscopy is a valuable tool for pigment evaluation andproblem solving in plastics and other applications. Theorganic pigments used in plastic applications are typicallysub-micron in size. Pigment performance is greatly affectedby how well the pigment particles are incorporated in thepolymer medium. Various microscopic evaluationtechniques that can be used to investigate dispersion quality,strength development and thermal stability are reviewed.In addition, various microscopic techniques for identifyingcontaminants are discussed. 7 refs.USA

Accession no.764247

Item 182Composites Part A: Applied Science andManufacturing31A, No.2, 2000, p.165-71FAILURE PHENOMENA IN TWO-DIMENSIONAL MULTI-FIBREMICROCOMPOSITES. PART IV: A RAMANSPECTRASCOPIC STUDY ON THE INFLUENCEOF THE MATRIX YIELD STRESS ON STRESSCONCENTRATIONSvan den Heuval P W J; Peijs T; Young R JEindhoven,University of Technology; UMIST; QueenMary & Westfield College

Raman spectroscopy is used to study the influence of shearyield stress of the matrix on stress situations in carbonfibre/epoxy resin composites containing a planar fibrearray. A mixture of two curing agents, with differentfunctionality and molecular weights, are used to cure theepoxy resin in order to obtain a matrix with varying cross-linked density. The carbon fibres are surface treated togive good fibre-matrix adhesion. Three matrix systemsare investigated in the study, each with a different yieldstress. The mechanical properties of each material aremeasured under tension and shear conditions. 35 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; UK; WESTERN EUROPE

Accession no.763633

Item 183Journal of Macromolecular Science AA36, No.11, 1999, p.1751-8POLYPROPYLENE PIPES FOR DRINKINGWATER SUPPLYHametner CAustrian Plastics Institute

The migration of phenolic antioxidants (which aretypically used for the stabilisation of PP pipes) into

drinking water in contact with PP pipes was studied.Austrian, German and International Standard methodswere used for water at 23C and 60C. The low moleculardegradation product 2,4-di-tert-butylphenol, rather thanthe high molecular antioxidants, was detected in theaqueous extracts. In warm water extracts, theconcentration of phenols, the total organic carbon contentand the effect on odour and flavour were considerablyhigher than in cold. Alkaline water extracted higheramounts of phenols but acidic drinking water showed noeffect. Thermal loading of PP during the extrusion processsignificantly increased the extractable phenols, totalorganic carbon content and flavour number/thresholdodour. 7 refs.AUSTRIA; EUROPEAN UNION; WESTERN EUROPE

Accession no.763574

Item 184West Conshohocken, PA, 1999, pp.6. NALOAN.ASTM D 2124-. METHOD FOR ANALYSIS OFCOMPONENTS IN POLY (VINYL CHLORIDE)COMPOUNDS USING AN INFRAREDSPECTROPHOTOMETRIC TECHNIQUEAmerican Society for Testing & MaterialsASTM D 2124-

Version 99. Photocopies and loans of this document arenot available from Rapra.USA

Accession no.760789

Item 185Journal of Coatings Technology72, No.900, Jan.2000, p.69-74ANALYSIS OF EXEMPT PAINT SOLVENTS BYGAS CHROMATOGRAPHY USING SOLID-PHASE MICROEXTRACTIONBodrian R RCalifornia,Polytechnic University

Acetone, methyl acetate and parachlorobenzotrifluoridehave been exempted as VOC solvents by the EPA. Inmeasuring coating VOC content, separate methods fordetermining exempt solvents are required. One suchmethod utilises solid-phase microextraction to sample theheadspace of solvent-based coatings to which thesurrogates acetone-d6, methyl acetate-d3 and/ormetachlorbenzotrifluoride have been added. The sampledexempt coating solvents are thermally desorbed andanalysed using gas chromatography with flame ionisationor mass spectral detection. This paper presents the resultsobtained for acetone and toluene in a large number ofaerosol paints. Additionally, the results from a round-robinstudy for acetone, methyl acetate andparachlorobenzotrifluoride in commercial solvent-basedcoatings are reported. 17 refs.USA

Accession no.760572



Item 186Journal of Thermal Analysis and Calorimetry57, No.3, 1999, p.847-51IDENTIFICATION OF POLYETHYLENE BYDIFFERENTIAL SCANNING CALORIMETRYTsukame T; Kutsuzawa M; Sekine H; Saitoh H;Shibasaki TSaitama,Criminal Investigation Laboratory;Saitama,University

A forensic sample consisting of melt-recrystallisedpolymers recovered from the scene of a fire in a factoryis identified by differential scanning calorimetry. Thefactory commonly used two kinds of film sheets, A andB, made by different manufacturers. It is necessary todecide whether the forensic sample related to material Aor B. The forensic sample and reference samples ofmaterials A and B are subjected to IR spectroscopy andpyrolysis gas chromatograph mass spectrometrymeasurements, which reveal their PE nature. The thermalbehaviour of the samples is examined by differentialscanning calorimetry (DSC) and they are found to beblends of two kinds of PEs, LDPE and LLDPE. Thesamples can be identified and distinguished from eachother via the DSC measurements. 6 refs.JAPAN

Accession no.760331

Item 187Journal of Thermal Analysis and Calorimetry58, No.1, 1999, p.13-8THERMAL CHARACTERISATION OFPOLYURETHANE ACRYLATE RESINSLedru J; Saiter J M; Grenet J; Yuossef B; Burel F;Bunel CRouen,University; Rouen,Institut National des SciencesAppliquees

Polyurethane acrylate resins cured by two differentmethods, thermally and photochemically, are investigatedby means of differential scanning calorimetry andthermally stimulated depolarisation currents. Even if bothcuring methods lead to the same material from a chemicalpoint of view, important differences exist between thethermocured resin and the photocured resin in terms ofmolecular relaxation behaviour. 8 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.760327

Item 188Applied Spectroscopy53, No.11, Nov.1999, p.1412-8IN-LINE NEAR-INFRARED MONITORING OFPOLYMER PROCESSING. I. PROCESS/MONITOR INTERFACE DEVELOPMENTReshadat R; Desa S; Joseph S; Mehra M; Stoev N;Balke S T

Toronto,University

Near-infrared inline monitoring of polymer processingmeans using an optical fibre-assisted spectrometer toobtain spectra of the polymer melt flowing throughcommonly used processing equipment (an extruder).Conditions in the extruder are typically 200 deg.C and20 MPa. The design of interfaces between thespectrometer and the molten polymer is shown. Threedesigns are shown, each permitting monitoring at adifferent location in the process: a melt-at-die interface,a melt-in-barrel interface and a strand interface. Thesedesigns are for monitoring just before the extruder exit,in the main barrel of the extruder and after the productexits from the extruder as a strand, respectively. All theseinterfaces protect the inserted optical fibre probe fromthe harsh environment within the extruder whilepermitting easy replacement or a probe withoutinterrupting the process. This latter characteristic is veryimportant because it permits easy probe repair as well asthe use of other types of probes (for monitoring colour orparticles, for example) to be used during a run. Examplesof near-infrared spectra obtained with each of theinterfaces used with an immiscible blend of PE and PPare shown. Large differences in the spectra demonstratethat the design of the interface will affect multivariateanalysis directed at composition prediction. Subsequentpapers are directed at using the melt-at-die interface forcomposition prediction and accounting for nonlinearrelationships between absorbance and concentration. 6refs.CANADA

Accession no.760231

Item 189Applied Spectroscopy53, No.11, Nov.1999, p.1403-11THERMAL VOLATILISATION ANALYSIS: AVERSATILE PLATFORM FORSPECTROSCOPIC INVESTIGATION OFPOLYMER DEGRADATION PROCESSESGuo X; Huang B; Dyakonov T; Chen Y; Padron L;Vickstrom T; Kuhn J; Hodkiewicz J; Stevenson W T KWichita,State University; Harrick Scientific Co.;Oklahoma State University; Koch Industries Inc.; ATIInstruments

Thermal volatilisation analysis (TVA) and sub-ambientthermal volatilisation analysis (SATVA) techniques aredescribed. In addition to rate profiling of the volatileproduct flux of thermal degradation under high-vacuumconditions through measurement of pressure in thevacuum line as a function of sample temperature, the TVAtechnique is shown to afford a convenient method for anon the basis of volatility under high-vacuum conditions,of product fractions of thermal degradation for subsequentspectroscopic analysis. The capacity and flexibility ofTVA as a platform for these analyses are illustrated in acase study format by degrading poly(bisphenol A, 2-



hydroxy propylether). The overall degradation process isquantified, and most significant pathways of thermolysisare identified through subsequent spectroscopic analysisof products of decomposition. The design and constructionof a modified vacuum-tight long-path gas IR cell, as aninterface allowing for the application of Fourier transforminfrared spectroscopy (FT-IR) for the online analysis ofvolatile products of polymer degradation, is described.Proof of concept and application of this new analyticaltechnique, subsequently referred to as TVA/FT-IR, isillustrated through the examination of appropriate aspectsof the thermal degradation of PMMA polymers. 49 refs.USA

Accession no.760230

Item 190Analytical Chemistry71, No.21, 1st Nov.1999, p.4793-9GEL PERMEATION CHROMATOGRAPHYCOUPLED TO FOURIER TRANSFORM MASSSPECTROMETRY FOR POLYMERCHARACTERIZATIONAaserud D J; Prokai L; Simonsick W JFlorida,University

On-line coupling of GPC to Fourier transform(FT) massspectrometry(MS) using a modified commercialelectrospray ionisation(ESI) interface was studied.Selected oligomer profiles for the sodiated oligomer ionsof a narrow molec.wt. PMMA were generated and usedfor obtaining a calibration curve. Using the MS-generatedcalibration curve and the refractive index response forquantification, an accurate MWD was calculated andshown to be in good agreement with the value specifiedby the supplier. GPC/ESI/FT-MS also allowed for anunequivocal end group determination and characterisationof a secondary distribution due to the formation of cyclicreaction products. A glycidyl methacrylate/butylmethacrylate copolymer with a broad MWD wasanalysed, fractionation and high resolving power beingrequired for adequate characterisation. MWD data showedthe advantages of coupling high-resolution MS and GPCto overcome the difficulty of analysing polydispersepolymers with MS alone. 34 refs.USA

Accession no.759794

Item 191Polymer40, No.26, 1999, p.7341-50SURFACE STRUCTURE OF KEVLAR FIBRESTUDIED BY ATOMIC FORCE MICROSCOPYAND INVERSE GAS CHROMATOGRAPHYRebouillat S; Peng J C M; Donnet J-BDu Pont de Nemours International SA; Haute-Alsace,Universite

Kevlar fibre surface structure is primarily and directlyobserved in the filament configuration by the tapping

mode atomic force microscopy (AFM). Themicrofibrils feature is observed with an average widthof 500 nm, composed of various types of periodicalunits of an average size 50 nm in a pleating appearance.At the less crystalline spot on the Kevlar fibre surface,the periodical organisations exhibit the skin core-likedifferentiation. In contrast, at the highly crystallinespot, the periodicity is more uniformly arranged by arectangular network manner. Inverse gaschromatography (IGC) is used as a tool to investigatethe surface structure heterogeneity by calculating thesurface energy of different types of probes adsorbedon the Kevlar fibre surface. The energy sitesdistribution plot of n-hexylamine adsorption at finitedilution exhibits a two-adsorbing-peaks curve. At thehigher energy site, a possible hydrogen bondinginteraction is proposed between n-hexylamine andoxygen-containing groups formed at the less crystallinesurface. According to the AFM and IGC results, aKevlar fibre surface organisations model at thenanometer scale is proposed. 19 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;SWITZERLAND; WESTERN EUROPE

Accession no.758987

Item 192Macromolecular Chemistry & Physics200, No.10, Oct.1999, p.2345-55THERMAL DEGRADATION MECHANISMS OFPOLYETHERIMIDE INVESTIGATED BYDIRECT PYROLYSIS MASS SPECTROMETRYCarroccio S; Puglisi C; Montaudo GIstituto per la Chimica e la Tecnol.dei Mat.Pol.;Catania,University

The thermal degradation of poly(2,2'-bis(3,4-dicarboxyphenoxy)phenylpropane-2-phenylenediimide)was investigated by TGA and direct pyrolysis massspectrometry and the pyrolysis of this polyimidecompared with that of an aromatic polyamide (NOMEX).The structure of preformed oligomers from the purifiedpolyetherimide and the structure of high temperaturepyrolysis products obtained at 620C were examined andthe thermal degradation pathways involved in thedegradation elucidated. 32 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.757742

Item 193Macromolecular Chemistry & Physics200, No.10, Oct.1999, p.2205-7COLLECTION OF SOLID-STATE CARBON-13CP/MAS NMR SPECTRA OF COMMONPOLYMERSWilhelm M; Neidhoefer M; Spiegel S; Spiess H WMax-Planck-Institut fuer Polymerforschung; Wiley-VCH Verlag GmbH



A collection of high resolution solid-state Carbon-13NMR spectra of a wide range of polymers is presented. Itis useful for reference purposes in case of unknown orpartly unknown samples, such as polymer blends, blockcopolymers or polymeric latices. 16 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.757725

Item 194Polymer Degradation and Stability66, No.1, 1999, p.107-25VACUUM PYROLYSIS OF PVC. II: PRODUCTANALYSISMiranda R; Pakdel H; Roy C; Darmstadt H; Vasile CQuebec,Universite Laval; Institut Pyrovac Inc.; PetruPoni,Institute of Macromolecular Chemistry

Vacuum pyrolysis of pure PVC was carried out at varioustemperatures between 220 and 520C and under a totalpressure of 2 kPa. The main gaseous and liquid pyrolysisproducts obtained during the different stages of thermaldegradation were identified and quantified bychromatographic methods. Global mass balance andchlorine mass balance were determined and differentmethods of capturing hydrogen chloride under vacuumconditions were tested. The elemental composition,surface properties and calorific value of the solid residuewere determined. 43 refs.CANADA; EASTERN EUROPE; RUMANIA

Accession no.757340

Item 195Polymer Recycling4, No.1, 1999, p.13-25COMPOSITIONAL ANALYSIS ANDFEASIBILITY STUDY OF RECYCLED HDPEFOR DIRECT FOOD CONTACT APPLICATIONSSalafranca J; Cacho J; Nerin CZaragoza,University

Five HDPE samples, consisting of a virgin HDPE forfood-contact applications, three samples of this polymertaken after each of the three sequential recycling cyclesand a real post-consumer sample were analysed. Twodifferent extraction methods were applied: a combinationof maceration and sonication; and the total dissolution ofthe polymer. In order to evaluate both the feasibility ofusing these polymers in food-contact applications and theevolution of HDPE composition through the recyclingprocess, samples were analysed by both qualitative andquantitative GC-MS. Furthermore, GC-FID was appliedto the determination of alpha-alkenes, the mostrepresentative compounds as indicators of polymer matrixdegradation. Finally, antioxidants were analysed byreversed phase HPLC. 34 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.756660

Item 196Polymer International48, No.10, Oct.1999, p.1042-5EFFECTS OF UV RADIATION ON SEVERALHIGH-PERFORMANCE POLYIMIDECOMPOSITESKiefer R L; Herring K; Wylie B J; Orwoll R A;Thibeault S AWilliamsburg,College of William & Mary; NASALangley Research Center

Three carbon fibre-reinforced polyimides were exposedto UV radiation at 177C, at three different intensities forthree different times, so that the product of intensity andtime was a constant. Intensities of 1, 2 and 3 suns, whereone sun is the power in space at one earth-sun distance,were used, for a time periods of 500, 250 and 167 h. Thesamples were characterised by X-ray photoelectronspectroscopy (XPS), thermogravimetric analysis,thermomechanical analysis and dynamic mechanicalanalysis. Measurement of bulk properties showed nodifference between samples exposed to heat and UVradiation, and control samples. Surface analysis by XPSshowed an apparent decrease in carbonyl concentrationon the surface of some exposed samples. This wascorrelated to surface contamination by a silicone-containing material. 3 refs.USA

Accession no.756185

Item 197Composites Part A: Applied Science andManufacturing30A, No.12, 1999, p.1401-13USE OF XPS FOR CHARACTERISATION OFGLASS FIBRE COATINGSThomason J L; Dwight D WOwens-Corning Science & Technology Center

X-ray photoelectron spectroscopy was applied to a studyof commercial and experimental glass fibres using threedifferent instruments. A protocol for plotting ratios ofappropriate atom concentrations was developed and theplots used to estimate the surface coverage of the coatingon the glass fibres and provide data on the chemicalcomposition of the coating. The relationships betweenthe spectroscopic data and coated glass fibre parametersare demonstrated using an overlay model and data fromthe three instruments are compared. 22 refs.USA

Accession no.755993

Item 198Analytical Chemistry71, No.20, 15th Oct.1999, p.4776-80COMPOSITION AND MICROSTRUCTUREDETERMINATION OF A LATEX SYSTEM BYPYROLYSIS GAS CHROMATOGRAPHY



Frank Cheng-Yu WangDow Chemical Co.

The composition and microstructure of polymers in alatex system were studied by pyrolysis gaschromatography. The composition and microstructureof a polymer in the emulsion phase were identified bydirect pyrolysis of the latex system, followed bycomparing the trimer peak pattern with appropriatemicrostructure standards. The polymer in the aqueousphase was pre-pyrolysis derivatised withtetrabutylammonium hydroxide to convert the acid toits butyl ester. Similar procedures were then used toexplore the composition and microstructure of thepolymer in the aqueous phase. Polymers analysedincluded SCX-2660 (probably a styrene-methylmethacrylate-butyl acrylate terpolymer), styrene-butylacrylate copolymer and styrene-alpha-methylstyrene-butyl acrylate terpolymer. 17 refs.

JOHNSON S.C.,& SON INC.USA

Accession no.755899

Item 199Oxford, Butterworth-Heinemann Ltd., 1999,pp.xxvii,920. 24cms. 12/1/00. 011PLASTICS MATERIALS. 7TH EDN.Brydson J A

The latest edition, now the seventh, of this reputable textbook, provides an overview of the scientific, technologicaland economic aspects of currently available plastics andrelated materials, and also focuses on new materials -many based on metallocene catalyst technology.Developments with condensation polymers, includingseveral new polyester-type materials of interest for bottleblowing and/or degradable plastics, are also covered. Thisedition also attempts to explain the basis of metallocenepolymerisation. The commercial importance of thematerials discussed is also noted.

Accession no.755818

Item 200Journal of Applied Polymer Science74, No.10, 5th Dec.1999, p.2432-8CHARACTERIZATION OF BISPHENOL A-BASED EPOXY RESINS BY HPLC, GPC, GPC-MALLS, VPO, VISCOMETRY, AND END GROUPANALYSIS: ON THE IDENTIFICATION OF 2,3-DIHYDROXYPROPYL-CONTAININGCOMPOUNDS, DETERMINATION OF MOLARMASS DISTRIBUTION, AND BRANCHINGPodzimek S; Kastanek ASYNPO

Results of the above characterisation are presented anddiscussed with particular reference to determination ofalpha-glycol-containing compounds, determination ofmolar mass and molar mass distribution, determination

of branching and determination of refractive indexincrement. 19 refs.CZECH REPUBLIC

Accession no.755647

Item 201Journal of Vinyl and Additive Technology5, No.3, Sept.1999, p.148-58NMR SPECTRA OF LEAD STABILISERSGrossman R FHalstab Corp.

High resolution proton and 13C NMR spectra of lead-based heat stabilisers and their reaction products, obtainedusing the magic angle spinning technique, supportstructural assignments inferred from IR spectra. Thesedemonstrate that lead stabilisers are unique compounds,rather than the double salts of lead oxide found intextbooks. 8 refs.USA

Accession no.755491

Item 202Polymers for Advanced Technologies10, No.4, April 1999, p.237-43CHARACTERISATION OF THE SURFACE OFBULK-MOULDED COMPOUNDSVallat M F; Schultz J; Mauzac C; Jacquin MInstitut de Chimie des Surfaces et Interfaces; PSAEtudes et Recherches Centre Technique de Belchamp

The surface characterisation of bulk moulding compound(BMC) automotive parts using complementary techniquesof surface analysis, i.e. SEM, X-ray photoelectronspectroscopy, time of flight secondary ion massspectroscopy, glow discharge spectroscopy and contactangle is described. Similarities and differences betweenBMC surfaces and sheet moulding compound (SMC)surfaces are pointed out. Particular emphasis is placed onmould release agents (polymeric and stearate) on the surfacewhich can influence future bonding behaviour. 14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.754736

Item 203Macromolecular Chemistry & Physics200, No.9, 1999, p.2074-9INVESTIGATION OF MOLECULARDIMENSIONS OF POLYSTYRENE AS AFUNCTION OF SOLVENT COMPOSITION:APPLICATION TO LIQUIDCHROMATOGRAPHY AT THE EXCLUSION-ADSORPTION TRANSITION POINTBaran K; Laugier S; Cramail HENSCPB

Liquid chromatography was used to study PS standards atthe exclusion-adsorption transition point using silica



adsorbents having differing porosities in various eluents. Thebehaviour of model PS chains in solvent mixturescorresponding to the critical adsorption conditions wasevaluated using viscometry and light scattering. It was foundthat critical adsorption conditions could be achieved if thepolymer chains entered the pores of the stationary phase andthat the characteristics of the elution mode could be definedwith the aid of the polarity index of the eluent. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.752269

Item 204Macromolecular SymposiaVol.141, 1999, p.95-101RECENT ADVANCES IN THE ANALYSIS OFPOLYMERS AND COPOLYMERS BY MASSSPECTROMETRYMontaudo M SIstituto per la Chimica e la Tecnol.dei Mat.Pol.

Progress which has been made in the use of MALDI massspectroscopy to provide reliable molec.wt. and MWDvalues is reported. Molec.wt. averages and MWD ofpolydisperse samples (PMMA, siloxanes, polyesters andcopolyesters) were obtained by off-line coupling of SECequipment with the MALDI mass spectrometer. SECtraces of the samples were recorded, selected fractionswere analysed by MALDI-TOF and the averagemolec.wts. of the fractions were determined from the massspectrum. A method for analysing unknown copolymers,which involves the use of Markoffian statistics, is alsopresented. 26 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.752091

Item 205Polimery44, No.4, 1999, p.246-54PolishUSE OF PHOTOELECTRON SPECTROSCOPYIN STUDIES OF THE DEPTH PROFILE OFPOLYPROPYLENE FILMZenkiewicz M; Golebiewski JMetalchem Plastics Processing Institute

The physical fundamentals of photoelectron spectroscopyare reviewed and the range of applications is given. ThreePP films were examined and the depth of oxidation wasfound to be in the nanometer range. The oxidation levelof the external layer increases as the specific energy ofcorona discharges is increased. 27 refs. Articles from thisjournal can be requested for translation by subscribers tothe Rapra produced International Polymer Science andTechnology.EASTERN EUROPE; POLAND

Accession no.747688

Item 206LCGC International12, No.9, Sept.1999, p.577/87LC-MS ANALYSIS OF POLYMER ADDITIVESBY EL AND API: IDENTIFICATION ANDQUANTIFICATIONYu K; Block E; Balogh MWaters Corp.

Mass spectrometry can be the ideal detector for liquidchromatography because it offers both universality and therequired selectivity for complex analytical problems. Thetwo most popular types of interface for the benchtop singlequadrupole LC-mass spectrometer are the particle beaminterface and the atmospheric pressure ionisation interface.The particle beam interface is used to generate electronionisation spectra and the API interface is used to generateeither electrospray or atmospheric pressure chemicalionisation. This comprehensive article supplies a detailedanalysis of a study in which organic extractable frompolypropylene was used as the model analyte todemonstrate how the information obtained separately fromEI and API can be complementary. Seven compounds wereseparated and detected by both MS detectors. 35 refs.USA

Accession no.747567

Item 207Macplas InternationalNo.10, Aug.1999, p.64-70DIFFERENTIAL SCANNING COLORIMETRYAND INFRARED SPECTROSCOPY INPOLYMER ANALYSISPanarotto A; Bertucci MCesap

Differential scanning calorimetry is one of the mostcommonly used methods for characterising the thermalproperties of polymers. This method, particularly ifcomplemented by IR spectroscopic analysis, also allowsthe nature of the materials under test to be determined.The principles involved in DSC and IR spectroscopy arediscussed.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.745360

Item 208Polimery Tworzywa Wielkoczasteczkowe44, No.3, 1999, p.218-21PolishDETERMINATION OF MIGRATION OFDIMETHYL TEREPHTHALATE ANDDIMETHYL ISOPHTHALATE FROM PLASTICSStareczek T; Kaminska G; Ermel J; KortylewskaEdited by: Gliwice,Institute of Plastics & Paint Industry

A gas chromatographic method is described fordetermining dimethyl terephthalate and dimethyl



isophthalate in food simulants. The method consists inextracting DMT and DMIP from the food simulants withchloroform and analysing of the compounds by GC withthe use of calibration curves and diethyl terephthalate asan internal standard. 3 refs. Articles from this journal canbe requested for translation by subscribers to the Rapraproduced International Polymer Science and Technology.EASTERN EUROPE; POLAND

Accession no.745025

Item 209Journal of Applied Polymer Science73, No.2, 11th July 1999, p.221-6EVALUATION OF EVA-PVAC BLENDBEHAVIOUR BY 1-D AND 2-D SOLID-STATENMRDe Souza C M G; Pacheco C R; Tavares M I BRio de Janeiro,Universidade Federal; PETROBRAS

Ethylene-co-vinyl acetate and poly(vinyl acetate) blendswere prepared in different proportions by melting in aHAAKE Rheomix mixer. The blends were prepared at afixed temperature, rotation rate, and processing time.High-resolution solid state NMR was used to characterisethe blends with respect to structure-mobility-compatibilityusing magic angle spinning with cross-polarisation andhigh power hydrogen decoupling and measurements ofthe proton spin-lattice relaxation time in the rotatingframe. Miscibility between polymer chains was alsostudied by two-dimensional hydrogen ion/carbon-13 shiftcorrelation (HETCOR). 21 refs.BRAZIL

Accession no.743489

Item 210Macromolecules32, No.11, 1st June 1999, p.3671-3LIQUID ADSORPTION CHROMATOGRAPHYOF COPOLYMERS: MOLAR MASS(IN)DEPENDENT RETENTIONBerek DSlovak Academy of Sciences

Liquid adsorption chromatography with a continuoussolvent gradient elution was shown by several previousauthors to be capable of separating random and graftcopolymers according to their chemical composition, withtheir molar masses not playing an important role. Atentative explanation of this finding is presented. It isassumed that the copolymer species travel along thecolumn with a velocity which exactly corresponds to thatof the eluent composition, exhibiting a displacing powerjust necessary to prevent a fast progress of themacromolecules due to their exclusion. Under specificconditions, retention of macromolecules at this adsorptionpromoting ‘barrier’ depends almost exclusively on thecopolymer composition and not on its molar mass. Thishypothesis is based on the mechanism of the recently-

proposed and tested liquid chromatographic elution ofhomopolymers under limiting conditions of desorptionand takes into account the simultaneous effect ofadsorption and exclusion of macromolecules onto/fromthe column packing. 17 refs.SLOVAK REPUBLIC; SLOVAKIA

Accession no.743327

Item 211Polymer Recycling3, No.4, 1997/1998, p.263-7PROCEDURES FOR THE COMPOSITIONALANALYSIS OF REINFORCED POLYESTERRECYCLATEBream C E; Hornsby P RBrunel University

In order to consider effective strategies for the recoveryand reuse of plastics recyclates, a quantitative method isdescribed for the characterisation of polyester-basedmoulding compounds. Analytical procedures aredescribed for the quantification of fibre, filler and fireretardant contents in polyester moulding compoundscontaining calcium carbonate filler, glass fibrereinforcement, and aluminium hydroxide flame retardant.3 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.742796

Item 212High Performance PlasticsAug.1999, p.10IDENTIFICATION OF PLASTICS IN WASTE

A review is presented of the methods used in theidentification of plastics waste prior to recyclingoperations, which was published in International PolymerScience and Technology, and translated from a Polishsource. Rapid spectroscopic methods are indicated, andtheir use in packaging and automotive recycling arediscussed.EASTERN EUROPE; POLAND

Accession no.742675

Item 213Journal of Polymer Science: Polymer Physics Edition37, No.13, 1st July 1999, p.1485-94GLASS TRANSITION AND MISCIBILITY INBLENDS OF TWO SEMI-CRYSTALLINEPOLYMERS: POLYARYL ETHER KETONE ANDPOLYETHER ETHER KETONEWoo E M; Tseng Y CTaiwan,National Cheng Kung University

A study was made of the miscibility in the amorphousregion of melt mixed blends composed of a novel polyarylether ketone (PK99) and PEEK using various methods,



including optical microscopy, DSC, SEM, FTIRspectroscopy and wide-angle X-ray diffraction. Sampleswere physically aged in order to resolve any possibleoverlapping Tg’s but only one single Tg was detected overthe entire composition range. No evidence forisomorphism was found and the crystal forms of therespective polymers remained distinct and unchanged bymiscibility in the amorphous region. 14 refs.TAIWAN

Accession no.742306

Item 214Applied Spectroscopy53, No.6, June 1999, p.672-81POST-CONSUMER PLASTIC IDENTIFICATIONUSING RAMAN SPECTROSCOPYAllen V; Kalivas J H; Rodriguez R GIdaho,State University

The suitability of Raman spectroscopy, when used withK-nearest neighbours, library searching or cyclic subspaceregression, for computerised classification of post-consumer plastics was evaluated. Plastics investigatedwere PETP, PP, PS, PVC, HDPE AND LDPE.Modifications were made to the original cyclic subspaceregression algorithm for modelling multiple sampleproperties and the adapted algorithm employed to directlycompare the mechanisms of principal componentregression and the PLS2 form of partial least-squares. Itwas found that Raman spectroscopy could be used toidentify both HDPE and LDPE. 33 refs.USA

Accession no.741260

Item 215Applied Spectroscopy53, No.5, May 1999, p.557-64COMPARISON OF NEAR-INFRARED ANDRAMAN SPECTROSCOPY FOR THEDETERMINATION OF CHEMICAL ANDPHYSICAL PROPERTIES OF NAPHTHAMin-Sik Ku; Hoeil ChungSK Corp.

Near-infrared and FTIR Raman spectroscopy werecompared and evaluated for the quantitative analysis ofnaphtha using partial least-squares regression. 19 refs.SOUTH KOREA

Accession no.740339

Item 216Applied Spectroscopy53, No.5, May 1999, p.551-6FOURIER TRANSFORM RAMAN SPECTRA OFLINEAR LOW-DENSITY POLYETHYLENE ANDPREDICTION OF THEIR DENSITY BYMULTIVARIATE DATA ANALYSIS

Sano K; Shimoyama M; Ohgane M; Higashiyama H;Watari M; Tomo M; Ninomiya T; Ozaki YKwansei-Gakuin,University; Hyogo,Prefectural PoliceHeadquarters; Yokogawa Electric Co.

FTIR spectra were measured for pellets of sixteen kindsof LLDPE with short branches and one kind of PE withoutany branch to explore the effects of the branches on thephysical properties and the Raman spectrum. Partial leastsquares analysis regression was applied to the Ramanspectra after multiplicative scatter correction to proposea calibration model that predicts the density of LLDPE.38 refs.JAPAN

Accession no.740338

Item 217Journal of Coatings Technology71, No.893, June 1999, p.53-60INVERSE GAS CHROMATOGRAPHY, SURFACEPROPERTIES, AND INTERACTIONS AMONGCOMPONENTS OF PAINT FORMULATIONSZiani A; Xu R; Schreiber H P; Kobayashi TEcole Polytechnique de Montreal; Nippon Paint Co.

Inverse gas chromatography analysis at very high dilutionand at finite concentrations of probe injection was carriedout on a series of polymers and pigments used in paintformulations. Values of dispersion surface energies, andof acid-base interaction parameters were obtained for thematerials, and pair interaction parameters were calculatedfrom the results. The dispersion stability of each pigment/polymer combination was measured and correlated withthe acid-base interaction parameters of the materials, andis shown to justify the availability of fundamentalthermodynamic interaction data to optimise performanceaspects of protective coatings. 23 refs.CANADA; JAPAN

Accession no.739845

Item 218Analytical Chemistry71, No.10. 15th May 1999, p.2037-45ANALYSIS OF POLYMERIC FLAMERETARDANTS IN ENGINEERINGTHERMOPLASTICS BY PYROLYSIS GASCHROMATOGRAPHY WITH AN ATOMICEMISSION DETECTORWang F C YDow Chemical Co.

Halogen-containing polymeric flame retardants inengineering thermoplastics were analysed by pyrolysisgas chromatography(Py-GC) with an atomic emissiondetector(AED) and a mass selective detector(MSD). TheAED was very effective in monitoring halogen-containingpyrolysates after Py-GC. The type of polymeric flameretardant used in thermoplastics could be identified bypeak pattern recognition through an AED halogen element



trace. A set of thermoplastic resins containing differentbrominated polymeric flame retardants was studied. Aftergeneration of the pyrogram by Py-GC/AED, thosepyrolysates produced from polymeric flame retardantswere identified by MSD analysis of a complex total ionchromatogram generated by the thermoplastic resins. Theresults demonstrated the effectiveness of the AED in thetasks of specific element monitoring and componentpattern recognition. The advantages and disadvantagesof using the AED are also discussed. 11 refs.USA

Accession no.738049

Item 219ACS, Polymeric Materials Science and Engineering.Vol.76. Conference proceedings.San Francisco, Ca., Spring 1997, p.128-9. 012ATOMIC FORCE MICROSCOPY STUDY OFINTRAOCULAR LENS IMPLANTS -TOPOGRAPHY AND SURFACE PROPERTIESKowalewski T; Ravi V NWashington,University; St.Louis,Veterans AffairsMedical Center(ACS,Div.of Polymeric Materials Science & Engng.)

Cataracts are one of the most common causes ofworldwide blindness. They are presently corrected bysurgery in which the natural cataractous lens is replacedby a synthetic intraocular lens. Successful visualrehabilitation is not only a function of patients’ healthand the surgical technique, but it also depends on theoptical, mechanical and bioperformance of the intraocularlens. Visual deterioration after surgery has been attributedto cellular debris deposited on the lens surface andcapsular opacification resulting from inflammation.Although the exact sequence of events that take placewhen an implant is exposed to the ocular environment invivo is not known, protein adsorption, complementactivation and cellular adhesion have been implicated andbelieved to be influenced by the surface properties of theimplants. The surface characteristics (surface topographyand viscoelasticity) of intraocular lenses are investigatedusing tapping-mode atomic force microscopy. 9 refs.USA

Accession no.737604

Item 220Polymer40, No.17, 1999, p.4763-7MODULATED DIFFERENTIAL SCANNINGCALORIMETRY: 14. EFFECT OF MOLECULARINTERACTIONS ON GLASS TRANSITIONBEHAVIOUR AND INCREMENT OF HEATCAPACITY IN MISCIBLE POLYMER BLENDSSong M; Hourston D J; Pollock H M; Hammiche ALoughborough,University; Lancaster,University

Modulated differential scanning calorimetry was usedto study miscible polymer blends. The blends studied

were poly(vinyl acetate)/poly(methyl acrylate),poly(phenylene oxide)/PS and two poly(styrene-co-acrylonitrile)/PMMA blends, the last two containingdifferent acrylonitrile contents. Specific molecularinteractions determined whether the glass transitiontemperature and the increment of heat capacity versuscomposition showed positive or negative deviationsfrom linearity for the blend systems. In the non-interacting system (poly(vinyl acetate)/poly(methylacrylate)), the glass transition temperature and incrementof heat capacity showed linear behaviour withcomposition. Thermodynamic theories for the observedresults were discussed. 17 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.737361

Item 221LCGC International12, No.7, July 1999, p.432/6QUANTITATIVE ANALYSIS OFPOLY(METHYLMETHACRYLATE) IN DRUGSBY CURIE-POINT PYROLYSIS GASCHROMATOGRAPHYMuguruma S; Uchino S; Oguri N; Kiji JJapan Analytical Industry Co.Ltd.; Tottori,University

Curie-point pyrolysis gas chromatography was used forthe quantitative analysis of residual synthetic adsorbentcrosslinked PMMA used in drug purification. Levels ofPMMA adsorbent below 0.15% in drug substances weresuccessfully measured quantitatively by Py-GC usingcharacteristic peaks that reflect the structure of theadsorbent, demonstrating that this analytical techniquecan be used to monitor compliance with the limit of 0.1%organic impurity in drug substances stipulated by ICHguidelines. 12 refs.JAPAN

Accession no.736647

Item 222Journal of Applied Polymer Science72, No.7, 16th May 1999, p.913-25HIGH-PERFORMANCE LIQUIDCHROMATOGRAPHY-MASS SPECTROMETRYOF EPOXY RESINSFuchslueger U; Rissler K; Stephan H; Grether H J;Grasserbauer MCiba Specialty Chemicals Inc.; Vienna,TechnicalUniversity

The application of liquid chromatography coupled tomass spectrometry for the analysis of epoxy resins wasshown in two examples. Electrospray (ESI) andatmospheric pressure chemical ionisation (APCI) werecompared with respect to the ionisation of diglycidylether of bisphenol A (DGEBA)-based epoxy resins. By-products in a typical modified solid DGEBA-based



epoxy resin and in a new weatherable crosslinker forpowder coating applications were characterised anddiscussed. 26 refs.AUSTRIA; SWITZERLAND; WESTERN EUROPE

Accession no.734831

Item 223Journal of Adhesion Science and Technology13, No.5, 1999, p.629-45ADHESION CHARACTERISATION OFPROTECTIVE ORGANIC COATINGS BYELECTROCHEMICAL IMPEDANCESPECTROSCOPYDeflorian F; Fedrizzi LTrento,University

This review describes in detail the influences on adhesionof different pretreatments or organic coatings, consideringaluminium, galvanised steel, and stainless steel substrates,and it was shown that the information obtained using anelectrochemical approach can be used for adhesionevaluation, with particular attention to monitoring ofadhesion in an aqueous environment, which is the mostdetrimental for protective organic coatings. 40 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.733531

Item 224Macromolecular Chemistry & Physics200, No.5, May 1999, p.1134-42POSSIBILITIES AND LIMITS OF PHOTONCORRELATION SPECTROSCOPY INDETERMINING POLYMER MOLECULARWEIGHT DISTRIBUTIONSFaraone A; Magazu S; Maisano G; Villari V; Maschio GMessina,University

The effect of concentration and polydispersity on thecollective diffusion coefficient(Dc) evaluated usingphoton correlation spectroscopy was investigated onPMMA in acetone solutions. The concentrationdependence of the Dc followed a linear regression law,the slope being fairly independent of polydispersity,molec.wt. and temp. The diffusion coefficient at infinitedilution obeyed a given scaling law. The inversion of thescattered intensity autocorrelation data by theregularisation method CONTIN permitted the evaluationof the MWD function of the polymeric samples. Althoughthis algorithm gave valuable information on averageamounts or on the widths of the distribution, it had limitedresolution power. A comparison with the results obtainedby size exclusion chromatography was therefore carriedout for a set of samples having monomodal and bimodaldistribution functions. 22 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.733222

Item 225Coloring Technology for Plastics.New York, N.Y., Plastics Design Library, 1999, p.197-207. 52MEASURING STABILISERS IN PIGMENTEDPLASTICS WITH NEAR-INFRAREDSPECTROSCOPYSolera P; Nirsberger M; Castillo NCiba Specialty Chemicals Corp.Edited by: Harris R M

Near-infrared (NIR) spectroscopy has become acommonplace analytical tool in the plastics industry. NIRtechniques have made quantification of many organiccomponents in polymer processing easy and quick. Thework presented outlines the methodology for using NIRto measure stabiliser levels in colour concentrates andnatural polymer formulations. Advantages and limitationsare considered as well as particle size and product form.4 refs.USA

Accession no.732217

Item 226Coloring Technology for Plastics.New York, N.Y., Plastics Design Library, 1999, p.191-5. 52PRACTICAL ANALYSIS TECHNIQUES OFPOLYMER FILLERS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY(FTIR)Coles B J; Hall C JHauser Inc.Edited by: Harris R M

The identification of polymers by FTIR is oftencomplicated by the presence of fillers. However, for kaolinclay, FTIR analysis should be able to identify the fillerand predict its concentration using a standard curve. Theresulting percentage is more reliable than a simple ash,which may change the chemical composition of the filler.2 refs.USA

Accession no.732216

Item 227Pitture e Vernici75, No.5, March 1999, p.7-8English; ItalianE.I.S. EVALUATION OF ATTACHED AND FREEPOLYMER FILMSCastela A S; Simoes A M P

Evaluation of the volume fraction of water in organiccoatings in immersion is often made by electrochemicalimpedance spectroscopy, EIS, and based upon theevolution of the coating capacitance. Among the severalmodels and equations proposed for this determination,the most frequently used is the Brasher equation. Most



frequently these determinations are made with appliedcoatings, although studies can be found in the literatureusing free films. The behaviour of a commercial coating- PVC plastisol - is studied, both applied on a metallicsubstrate and as a free film.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.731759

Item 228Journal of Thermal Analysis and Calorimetry55, No.2, 1999, p.559-63TG/FT-IR STUDIED OF POLY(VINYLCHLORIDE) BLENDSPielichowski KKrakow,Technical University

Thermogravimetry coupled with FTIR was used toinvestigate the stabilising action of 3-(2,4-dibromophenylazo)-9-(2,3-epoxypropane)carbazole onthe degradation of PVC. This secondary stabiliserincreased the initial temperature of hydrogen chlorideevolution (the main process responsible for PVCdecomposition), thereby allowing its application for novelPVC systems with enhanced thermal stability. 10 refs.EASTERN EUROPE; POLAND

Accession no.731454

Item 229Analytical Chemistry71, No.9, 1st May 1999, p.1809-14POLYMER ANALYSIS BY LIQUIDCHROMATOGRAPHY/ELECTROSPRAYIONISATION TIME-OF-FLIGHT MASSSPECTROMETRYNielen M W F; Buijtenhuijs F AAkzo Nobel Central Research

Different liquid chromatography modes in polymeranalysis were successfully interfaced with electrosprayionisation time-of-flight mass spectrometry in a singleexperimental set-up: the mass spectrometry data from sizeexclusion chromatography/mass spectrometry of PMMAwere used as absolute calibration points in the sizeexclusion chromatography/refractive indexchromatogram, and monomer mass and end groups wereinferred from the isotopically resolved mass spectra. 44refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.731446

Item 230Polymer Preprints. Volume 40. Number 1. March 1999.Conference proceedings.Boston, Ma., March 1999, p.226-7. 012SURFACE MODIFICATION OF POLYSTYRENESTUDIED BY IR-VISIBLE SUM FREQUENCY

GENERATION SPECTROSCOPYZhang D; Dougal S; Yeganeh M SExxon Research & Engineering Co.(ACS,Div.of Polymer Chemistry)

The effects of UV light and oxygen plasma on PS surfacesis investigated using SFG spectroscopy. The observedspectral changes provide strong support for thephotooxidation of the aromatic ring at the PS surface, asobserved by the dramatic decrease in the aromatic C-Hvibration during photo irradiation and plasma treatment.It is also found that the kinetics of the photooxidation ofthe PS surface, monitored by SFG, is much faster thansimilar process observed by other techniques, such asFTIR or SIMS. 13 refs.USA

Accession no.730043

Item 231Polymer Composites20, No.2, April 1999, p.314-20CHARACTERISATION OF MIXED FIBRENYLON COMPOSITES INCORPORATINGCOMPOSITE SCRAPLicea-Claverie A; Carrillo F J U; Alvarez-Castillo A;Castano V MTijuana,Instituto Tecnologico; Zacatepec,InstitutoTecnologico; UNAM

Recycling of engineering thermoplastics and theircomposites is discussed. A study on nylon-6,6 basedcomposites with mixed glass fibre and carbon fibrereinforcement, including nylon composite scrap in theirformulation, were reported. Several formulations wereprepared by injection moulding and were characterisedby stress-strain measurements, impact testing,simultaneous DTA and TGA, density measurements andSEM. Mechanical and thermal properties of the resultingcomposites are presented, discussed, and compared witha virgin standard composite. 26 refs.MEXICO

Accession no.729302

Item 232Analytical Chemistry71, No.7, 1st April 1999, p.1316-22CHARACTERIZATION OF NATURAL RESINSHELLAC BY REACTIVE PYROLYSIS-GASCHROMATOGRAPHY IN THE PRESENCE OFORGANIC ALKALIWang L; Ishida Y; Ohtami H; Tsuge S; Nakayama TNagoya,University; Gifu Shellac ManufacturingCo.Ltd.

A method for determining the chemical composition ofnatural resin shellac was developed based on reactivepyrolysis-gas chromatography(Py-GC) in the presence ofan organic alkali, tetramethylammoniumhydroxide(TMAH). Py-GC using 25% TMAH aqueous



solution permitted the highly sensitive determination ofterpenic acids, aleuritic acid, several minor fatty acids andthe wax components of shellac as their methyl derivativeson the resulting pyrograms with less than 2.0 % relativestandard deviations without using any cumbersomepretreatment. The observed average distributions of eachresin acid component determined by reactive Py-GC forshellac samples from India and Thailand showed that theaverage ratios among terpenic acids, aleuritic acid and theother fatty acids were about 53:24:14 for Indian shellacand 51:35:14 for Thailand shellac, respectively, suggestinga slightly significant difference. Clearer discrimination ofthe shellac samples from the two different countries was,however, achievable by applying principal componentanalysis for the mole percent distributions of all the acidiccomponents determined by reactive Py-GC. 24 refs.INDIA; JAPAN; THAILAND

Accession no.727139

Item 233ACS Polymeric Materials Science and Engineering.Fall Meeting 1997. Volume 77. Conferenceproceedings.Washington, D.C., 1997, p.594-5 .012EFFECT OF SECOND DIMENSION SAMPLINGRATE AND PARTICLE SIZE ON RESOLUTIONAND RUN TIME IN TWO DIMENSIONALLIQUID CHROMATOGRAPHY FOR THEANALYSIS OF POLYMERSMurphy R E; Schure M R; Foley J PRohm & Haas Co.; Villanova,University(ACS,Div.of Polymeric Materials Science & Engng.)

The optimisation of a two dimensional high performanceliquid chromatography (HPLC) (reverse phase liquidchromatography/gel permeation chromatography (GPC))system for the analysis of low molecular weight polymersis described. A test mixture of polyethylene glycols and acommercial surfactant was used. The analysis time of thesecond dimension, GPC, was varied by using differentcolumns. The columns had different particle sizes andlengths, and the two dimensional resolution was comparedby varying the run time in the second dimension.Following the optimisation, it was possible to complete atwo dimensional analysis in the time normally taken fora normal gradient HPLC run. It was established thatconventional columns could be run with higher flow rateswithout a significant loss of resolution. The combinationof shorter and smaller particle GPC columns resulted inlower sampling periods at lower flow rates thanconventional columns. The highest sampling rate into thesecond dimension gave the best resolution. 7 refs.USA

Accession no.726180

Item 234Shawbury, Rapra Technology Ltd., 1997, pp.315.220.00. 30cms. 9922

RAPRA COLLECTION OF INFRARED SPECTRAOF RUBBERS, PLASTICS ANDTHERMOPLASTIC ELASTOMERS. SECONDEDITIONSidwell J A

This book provides a set of transmission and pyrolysatespectra of a comprehensive range of technically importantrubber and plastics materials including copolymers andblends which are in current use. Materials are indexedunder both polymer and trade name.

Accession no.725345

Item 235Polymer40, No.12, 1999, p.3479-85INVERSE GAS CHROMATOGRAPHICCHARACTERIZATION OF POLY(ETHYLENEOXIDE)Al-Saigh Z YColumbus,State University

The inverse gas chromatography method was used toobtain the thermodynamic properties and the surfaceenergy of a semicrystalline polymer, PEO. PEO was usedas a stationary phase in the chromatographic column and16 solutes with a different chemical nature were used aseluents. Alkanes showed endothermic interactionparameters and the molar heat of mixing in a temp. rangeof 70-130C. Acetates and alcohols showed betterinteractions with the PEO layer and butanol was found tobe the best solvent for PEO among all solutes used. Thevariation in molec.wt. of PEO above 400 g/mol showedno apparent effect on the interaction coefficients. Thedispersive contribution of the surface energy of PEO wasmeasured as a function of temp., which ranged from 8.00and 13.00 mJ/sq m, indicating a poor surface energy ofPEO. 43 refs.USA

Accession no.721885

Item 236Journal of Adhesion68, Nos.1-2, 1998, p.117-42QUANTIFICATION OF COATING ADHESIONUSING LASER INDUCED DECOHESIONSPECTROSCOPYMeth J S; Sanderson D; Mutchler C; Bennison S JDuPont Co.

A new technique, laser induced decohesion spectroscopy,is presented, which is capable of measuring the practicalwork of adhesion between a transparent polymer coatingor substrate. A laser pulse directed onto the sample createsa blister at the transparent/opaque interface. The blister’sinternal pressure depends on the laser pulse energy, andat a critical pressure the sample fractures, creating anannular debond similar to that obtained in the standardblister test. By measuring physical variables such as the



curvature of the blister, and its radius and thickness, it ispossible to deduce the practical work of adhesion. 19 refs.USA

Accession no.721348

Item 237Journal of Adhesion Science and Technology13, No.3, 1999, p.379-91DETERMINATION OF THE ADHESIONPROPERTIES OF AN ALKYD PIGMENTEDCOATING BY ELECTROCHEMICALIMPEDANCE SPECTROSCOPYGonzalez J E G; Rosca J C MGran Canaria,University

Impedance measurements were performed in differentfrequency ranges at open circuit potential for an alkydcoating with titanium dioxide as a mineral pigment in3% sodium chloride. The most probable impedanceequivalent circuit method was considered for dataanalysis. The interpretation of the impedance spectrapermitted the determination of water permeation, theformation of blisters, swelling of the coating, and the lossof adhesion. 17 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.721335

Item 238ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.48-9 012QUANTITATION IN THE ANALYSIS OFOLIGOMERS BY HPLC WITH ELSDTrathnigg B; Kollroser M; Maier B; Berek D; Janco MGraz,Karl-Franzens-Universitat; Slovak Academy ofSciences(ACS,Div.of Polymeric Materials Science & Engng.)

The influence of the operating parameters used whenoperating evaporative light scattering detectors inconjunction with high performance liquidchromatography for the characterisation of oligomers wasinvestigated, using polyether samples. It was concludedthat the instrument was useful because it provided gradientelution, however, very careful calibration was requiredto obtain reliable quantitative data. 16 refs.AUSTRIA; WESTERN EUROPE

Accession no.720839

Item 239ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.46-7 012APPLICATION OF SEC AND HPLC TO THECHARACTERIZATION OF POLYMERS,OLIGOMERS, AND SMALL MOLECULES USEDIN COATINGS AND INKS

Kuo C; Grieser M D; Robinson DHenkel Corp.(ACS,Div.of Polymeric Materials Science & Engng.)

Applications are given of the use of size exclusionchromatography and high performance liquidchromatography for the characterisation of coatingssystems which either use water as the major solvent orutilise low molecular weight polymers, oligomers, andreactive additives which are then reacted to produce highmolecular weight and crosslinked films. 6 refs.USA

Accession no.720838

Item 240ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.35-6 012LIQUID CHROMATOGRAPHY OFMACROMOLECULES UNDER LIMITINGCONDITIONS OF SOLUBILITY: FIRSTEXPERIMENTAL OBSERVATIONSBartkowiak A; Hunkeler D; Murgasova R; Berek DSzczecin,Technical University; Swiss Federal Instituteof Technology; Slovak Academy of Sciences(ACS,Div.of Polymeric Materials Science & Engng.)

Liquid chromatography at the critical adsorption point(LC LCS) was investigated. The solubility ofmacromolecules, the sensitivity of LC LCS to suchvariables as the injection volume, concentration injected,mobile phase flow rate and mixing between the injectionzone, were investigated, using polymethyl methacrylate(PMMA) and polyacrylamide standards. It is proposedthat using tetrahydrofuran and n-hexane as eluents forPMMA, at the LC LCS, limited polymer insolubility oreven local precipitation is combined with the sizeexclusion of macromolecules. 12 refs.EASTERN EUROPE; POLAND; SLOVAK REPUBLIC;SLOVAKIA; SWITZERLAND; WESTERN EUROPE

Accession no.720833

Item 241ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.31-2 012LIQUID CHROMATOGRAPHY OFMACROMOLECULES AT THE CRITICALADSORPTION POINT: PROBLEMS ANDPITFALLSBerek D; Janco MSlovak Academy of Sciences(ACS,Div.of Polymeric Materials Science & Engng.)

The role of column packing pore size in liquidchromatography at the critical adsorption point wasinvestigating using three silica gels and a series ofpolymethyl methacrylates (PMMA), using toluene,tetrahydrofuran (THF) or their mixtures as eluents.



Toluene strongly promotes adsorption of PMMAs on thesilica surface, whereas THF suppresses adsorption. It wasestablished that the pore size of the column packingsplayed an important role in liquid chromatography at thecritical adsorption point. The column with the smallestpores largely determined the behaviour of the whole set.The feasibility of using silica gel as column packings forliquid chromatography at the critical adsorption point isquestioned. 14 refs.SLOVAK REPUBLIC; SLOVAKIA

Accession no.720831

Item 242ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.22-3 0122D-LC OF FUNCTIONAL POLYETHERSTrathnigg B; Kollroser M; Parth MGraz,Karl-Franzens-Universitat(ACS,Div.of Polymeric Materials Science & Engng.)

A combination of liquid chromatography under criticalconditions using coupled density and RI detection in onedimension, and gradient high performance liquidchromatography in the second dimension, was used inthe two-dimensional chromatographic analysis of theoligomers present in fatty alcohol ethoxylates. Fullresolution was achieved. 6 refs.AUSTRIA; WESTERN EUROPE

Accession no.720827

Item 243ACS Polymeric Materials Science and Engineering.FallMeeting 1997.Volume 77.Conference proceedings.Washington, D.C., 1997, p.20-1 012MOLECULAR CHARACTERIZATION OFCOMPLEX POLYMERS BY COUPLED LIQUIDCHROMATOGRAPHIC PROCEDURESBerek DSlovak Academy of Sciences(ACS,Div.of Polymeric Materials Science & Engng.)

Size exclusion chromatography alone cannot characterisethe constituents of complex polymer systems. Separationselectivity and characterisation of complex systems maybe enhanced with liquid chromatographic (LC) methodsutilising combinations of different separationmechanisms. These are termed coupled LC procedures.The applications of a variety of coupled LC proceduresare discussed. 16 refs.SLOVAK REPUBLIC; SLOVAKIA

Accession no.720826

Item 244ACS Polymeric Materials Science & Engineering,Spring Meeting 1998. Volume 78. Conferenceproceedings.

Dallas, Tx., Spring 1998, p.102-3. 012COUPLED PROGRAMMED PYROPROBE-MASSSPECTROMETRY ANDTHERMOGRAVIMETRIC-MASSSPECTROMETRYCarraher C E; Molloy H M; Louda J W; Baker EFlorida,Atlantic University; Florida,Center forEnvironmental Studies; Midwest Research Institute(ACS,Div.of Polymeric Materials Science & Engng.)

In 1977, a thermogravimetric analysis unit wassuccessfully coupled with a mass spectrophotometer, TG-MS. More recently, a coupled programmed pyroprobe-mass spectrophotometry system, also utilising IRspectroscopy, was employed as a means of describingdegradation sequences as a function of temperature. Theapplication of these tools as a means to define polymerstructure and degradation products is described. 9 refs.USA

Accession no.719193

Item 245ACS Polymeric Materials Science & Engineering,Spring Meeting 1998. Volume 78. Conferenceproceedings.Dallas, Tx., Spring 1998, p.219-20. 012SECONDARY TRANSITIONS IN POLYMERSPROBED BY DIFFERENTIAL SCANNINGCALORIMETRYBertolucci P R H; Harmon J PSouth Florida,University(ACS,Div.of Polymeric Materials Science & Engng.)

The use of differential scanning calorimetry to identifysecondary transitions in thermoplastics is studied. Thetemperature and breadth of the secondary transition arerelated to the those of the alpha transition in a variety ofmethacrylate, acrylate and styrene polymers, as well aspolycarbonate. The effect of thermal history and theposition and sharpness of these endothermic transitionsis discussed. Some comparisons are made between thistechnique and results obtained via dielectric analysis anddynamic mechanical analysis obtained in the laboratory.7 refs.USA

Accession no.718740

Item 246Macromolecular Chemistry & Physics200, No.2, Feb.1999, p.413-21THERMAL PROPERTIES ANDCRYSTALLISATION BEHAVIOUR OFPOLYHYDROXYBUTYRIC ACID IN BLENDSWITH CHITIN AND CHITOSANIkejima T; Yagi K; Inoue YTokyo,Institute of Technology

Films of blends of polyhydroxybutyric acid with chitinand chitosan were prepared as completely biodegradable



polyester-polysaccharide composites. Crystallisation wasexamined using DSC. Data are given from FTIR andcarbon 13 NMR. 31 refs.JAPAN

Accession no.716972

Item 247Journal of Biomedical Materials Research (AppliedBiomaterials)48, No.1, 1999, p.5-8EXTRACTABLE FREE MONOMERS FROMSELF-CURED DENTAL SEALANTS RESULTINGFROM DISPENSING ERRORSVaubert V M; Moon P C; Love B JVirginia,Polytechnic Institute

HPLC experiments were performed on a series of self-curing polybisglycidyl methacrylate dental sealants thatwere deliberately mismixed. The amount of extractablesealant under conditions of nonideal processing wasmeasured. 13 refs.USA

Accession no.716163

Item 248Macromolecular Rapid Communications20, No.2, Feb. 1999, p.95-7CURING OF MONOMER COMPOSITES. II. USEOF NMR TO MONITOR REAL TIME CURINGDYNAMICSMartin S J; McBrierty V J; Dowling J; Douglass D CDublin,Trinity College; Bausch & Lomb Inc.

Details are given of a method for monitoring the real-time curing dynamics of composite monomers, exploitingsite specific information provided by high resolutionNMR. Data using polyvinylpyrrolidone, polyhydroxy-ethyl methacrylate and polybutylhydroxycyclohexylmethacrylate are compared with results from a computersimulation based on a multicomponent kinetic model.7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;WESTERN EUROPE

Accession no.716161

Item 249Journal of Adhesion Science and Technology13, No.1, 1999, p.19-34RHEO-PHOTOACOUSTIC (RPA) FTIRSPECTROSCOPIC STUDIES OF THEADHESION OF THERMOSETS TOPOLYOLEFINSPennington B D; Urban M WNorth Dakota State University

Rheophotoacoustic FTIR analysis and previouslydeveloped theory were utilised in an attempt to correlatethe molecular level interactions in polymer bilayer

systems under elongational interactions in polymer bilayersystems under elongational deformations and changes inpotential energy, leading to determination of the work ofadhesion. This research expands the scope of previousfindings and provides a relationship between the C-Hstretching vibrational energy changes for acrylic/PE,epoxy/PE, acrylic/PP, and epoxy/PP bilayer systems andthe interfacial forces responsible for adhesion. 39 refs.USA

Accession no.715972

Item 250Analytical Chemistry71, No.2, 15th Jan.1999, p.468-75IDENTIFICATION AND DETERMINATION OFCROSSLINKERS IN CROSSLINKEDPOLYVINYLPYRROLIDONE(PVP) BYPYROLYSIS-GAS CHROMATOGRAPHY(GC)/MASS SPECTROMETRY(MS)Cheng T M H; Malawer E GInternational Specialty Products

Pyrolysis-GC and pyrolysis-GC/MS were used to identifyand quantify specific nitrogen-containing crosslinkercompounds incorporated into the structures of crosslinkedPVP polymers which appeared to be identical by FTIRspectroscopy. The pyrolyser regenerated and volatilisedspecific crosslinkers which could be distinguished fromother pyrolysate compounds by either peak retention timeor mass spectral release. Individual compounds studiedincluded 3-ethylidene-1-vinyl-2-pyrrolidone, 3,3'-ethylidenebis(1-vinyl-2-pyrrolidone) and N,N’-divinylimidazolidone. In general, the level of specificcrosslinkers in various commercial products ranged from1.8 to 2.5% w/w. The effect of pyrolysis temp. on thislevel varied with the crosslinkers studied. The crosslinkercontent obtained by this technique correlated with theswell volume data for a specific series of crosslinked PVPsamples made with a single crosslinker and having similarparticle size distributions. The pyrolysis methodologycould not distinguish the level of crosslinker which wasincorporated as a pendant functionality from that portionwhich was incorporated through both vinyl groups. 26refs.USA

Accession no.715578

Item 251Polymer Testing17, No.8, Dec.1998, p.533-41NMR STUDY OF COMMERCIALPOLYETHYLENE-CO-VINYL ACETATEde Souza C M G; Tavares M I BRio de Janeiro,Cidade Universitaria

Two EVA materials with distinct vinyl acetate ratios arestudied by nuclear magnetic resonance using solution andsolid techniques. These studies are made in order to obtain a



relation between the structure-properties-mobility and thisresponse can be utilised in order to have precise informationfor new applications as well as better understanding of thematerial behaviour. The results show that these polymerspresent characteristic mobilities as a function of vinyl acetatein the copolymer. Thus, as the quantity of vinyl acetateincreases the dyads and tryads distribution and the molecularmobility in the copolymer change, as a consequence of thedifferent commercial applications. 13 refs.BRAZIL

Accession no.714141

Item 252Journal of Thermal Analysis and Calorimetry54, No.2, 1998, p.565-76METHOD FOR ANALYSIS OF THE MEASUREDCURVES OF TEMPERATURE-MODULATEDDIFFERENTIAL SCANNINGCALORIMETRY(TMDSC) INVESTIGATION INTHE MELTING REGION OF POLYMERSSchawe J E K; Bergmann E; Winter WUlm,University; IFA GmbH

The measured signal of the TMDSC was examined for thecase of polymer melting. Fourier transform analysis wasused to evaluate the data, the resulting information beingthe amplitude and the phase shift of the first harmonic ofthe periodic heat flow component. It was shown that thisprocedure was not sufficient for quantitative discussions ifdeviations from the symmetric curve shape occurred in themeasured heat flow curves. For polymer melting, it wasshown that asymmetric curves would be measured if theexperimental temp. amplitude was too large. 15 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.713454

Item 253Journal of Thermal Analysis and Calorimetry54, No.2, 1998, p.477-99APPLICABILITY OF TEMPERATURE-MODULATED DIFFERENTIAL SCANNINGCALORIMETRY(TMDSC) TO POLYMERICSYSTEMS. GENERAL THEORETICALDESCRIPTION BASED ON THE FULL HEATCAPACITY FORMULATIONScherrenberg R; Mathot V; Steeman PDSM Research

An overview is presented of the different aspects ofTMDSC, using a general theoretical description basedon the full heat capacity formulation. It is demonstratedthat processes studied with the aid of TMDSC can besimply classified into three distinct regimes, dependingon the time scale and the susceptibility of the process tothe temp. modulation. 47 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.713453

Item 254Muanyag es Gumi34, No.12, 1997, p.A12-4HungarianASSESSMENT OF THE THERMAL HISTORY OFEXTRUDED UPVCMarossy KBorsodChem Rt.

The paper deals with the investigation by differentialscanning calorimetry of extruded rigid PVC formulations.The DSC traces of processed UPVC depend on thethermal history of the melt. The DSC tests can be used toestimate extrusion conditions e.g. of failed products. 16refs. Articles from this journal can be requested fortranslation by subscribers to the Rapra producedInternational Polymer Science and Technology.EASTERN EUROPE; HUNGARY

Accession no.713264

Item 255Surface Coatings International82, No.1, Jan.1999, p.26-30USE OF ELECTROCHEMICAL IMPEDANCESPECTROSCOPY FOR THE DETERMINATIONOF THE PROTECTIVE PROPERTIES OFSOLVENT- AND WATER-BASED PAINTSYSTEMSAl-Hashem A; Carew J A; Hasan AKuwait,Institute for Scientific Research

In this work, electrochemical impedance spectroscopywas used to evaluate the corrosion protection propertiesof the solvent-based coatings and water-based coatingsystems currently being proposed for use in the industrialinstallations in the Arabian Gulf region. Evaluation ofcorrosion damage levels for three coating systems after90 day immersion in 0.5M NaCl was performed usingthe EIS and visual observations. 22 refs.KUWAIT

Accession no.713236

Item 256Journal of Materials Science33, No.19, 1st Oct.1998, p.4721-5RAMAN SPECTRA OF HIGH MODULUSPOLYETHYLENE FIBRES BY RAMANMICROSCOPYLu S; Russell A E; Hendra P JSouthampton,University

Raman microscopy was used to analyse a series of highmodulus PE fibres, relating the Raman scatteringanisotropy to the mechanical performance of thefilaments. Measurements of the band intensity ratio ofthe fibres were made and related to their Young’s modulus.This relationship is useful in morphological studies ofPE fibres. 10 refs.



EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.711133

Item 257Applied Spectroscopy52, No.12, Dec.1998, p.1498-504MEASUREMENT OF ORIENTATION ANDCRYSTALLINITY IN UNIAXIALLY DRAWNPOLY(ETHYLENE TEREPHTHALATE) USINGPOLARISED CONFOCAL RAMANMICROSCOPYEverall N JICI Wilton Research Centre

Polarised confocal Raman microscopy was used tomeasure molecular orientation in uniaxially drawn PETPfilms, prepared with draw ratios from 1 to 3.5. Theorientation of both polarised Raman microscopy andpolarised attenuated total reflection IR spectroscopy.Crystallinity profiles were measured through the thicknessof the film samples and compared with the orientationgradients existing in the films. This procedure was todetermine whether the intuitive assumption thatorientation and crystallinity would be positively correlatedactually holds true on the microscopic scale for thesesamples. 18 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.711041

Item 258Plasticheskie Massy (USSR)No.3, 1997, p.30-3RussianBREAKDOWN OF AMMONIUM SALTS WITHREFERENCE TO THEIR INTRODUCTION INTOWOOD-BASED COMPOSITESVigdorovich A I; Efremov V N

The possibility was studied of using ammonium salts asplasticisers for wood-based composites, and thebreakdown of the ammonium salts during heating wasstudied by differential thermal gravimetry. 15 refs. Articlesfrom this journal can be requested for translation bysubscribers to the Rapra produced International PolymerScience and Technology.RUSSIA

Accession no.710456

Item 259Polymer Engineering and Science38, No.11, Nov.1998, p.1873-81PHYSICAL AND RELAXATION PROPERTIESOF FLAME-SPRAYED ETHYLENE-METHACRYLIC ACID COPOLYMERBrogan J A; Berndt C C; Simon G P; Hewitt DStony Brook,University; Monash,University

Details are given of the range of physical and chemicalproperties of flame-sprayed ethylene-methacrylic acidcopolymer following different processing conditions.Coatings were produced at a range of specifictemperatures by varying the propane flow rate and guntraverse rate. Coatings were scanned using dielectricrelaxation spectroscopy. 24 refs.AUSTRALIA; USA

Accession no.709520

Item 260Polymer Journal (Japan)30, No.10, 1998, p.771-4CRYSTALLITE SIZES AND LATTICEDISTORTIONS OF GEL-SPUN ULTRA-HIGHMOLECULAR WEIGHT POLYETHYLENEFIBRESXiao-Ping Hu; You-Lo HsiehCalifornia,University

A detailed method is reported for deriving the latticedistortions and crystallite sizes of UHMWPE fibres usinga full wide angle X-ray diffraction patterns. Theinstrumental broadening and the background scatteringis represented by a binomial. A discussion is includedabout the diffraction trace, peak assignments, and unitcell dimensions. 26 refs.USA

Accession no.709342

Item 261Chinese Journal of Polymer Science16, No.4, 1998, p.332-8DETECTION OF TG BY MODULATEDDIFFERENTIAL SCANNING CALORIMETRYRui Song; Jing Chen; Jingui Gao; Xin Lin; Qingrong FanChinese Academy of Sciences

The glass transition of PETP samples which weresubjected to solvent induced crystallisation (SINC) wasinvestigated by modulated differential scanningcalorimetry (MDSC) and density measurements. Thedifferential heat capacity signal from MDSC was used tomonitor the SINC process. 16 refs.CHINA

Accession no.709335

Item 262Journal of Applied Polymer Science71, No.1, 3rd Jan.1999, p.1-6MICROWAVE PLASMA REACTIONS OFIMIDAZOLE ON POLY(VINYL CHLORIDE)SURFACES: A SPECTROSCOPIC STUDYSchmitt B R; Heung Kim; Urban M WNorth Dakota State University

A closed-system microwave plasma reactor was used to reactimidazole molecules to PVC surfaces. Newly created



surfaces were analysed using ATR FTIR spectroscopy.Surface reactions on PVC were heavily dependent on a priorthermal history of the PVC substrate. A mechanism for thePVC-imidazole reactions was also presented. The PVC wasuseful as an implant for biomedical applications. 10 refs.USA

Accession no.709309

Item 263Applied Spectroscopy52, No.11, Nov.1998, p.1483-7SAMPLING CONSIDERATIONS FOR FT-RAMAN SPECTROSCOPY OF POLYMERS ANDSOLUTIONSBarrerra B A; Sommer A JMiami,University

Details are given of the determination of apparentabsorption coefficients and optimal sample thickness ofPE, PETP, cellulose, and cyclohexane by FT-Ramananalysis. A relationship was developed that permits theoptimal sample thickness for FT-Raman measurementsto be determined by measuring the absorbance spectrumof a sample whose thickness is known. Results arediscussed in the context of scattering theory, samplingconsiderations, and spectral artifacts. 9 refs.USA

Accession no.709038

Item 264Journal of Applied Polymer Science71, No.3, 18th Jan.1998, p.371-5PROPYLENE OLIGOMERS: EXTRACTIONMETHODS AND CHARACTERISATION BYFTIR, HPLC, AND SECEl Mansouri H; Yagoubi N; Scholler D; Feigenbaum A;Ferrier DINRA

Details are given of the isolation of propylene oligomersfrom polymer matrix by dissolution precipitation andSoxhlet methods. Characterisation was undertaken byFTIR, UV spectroscopy, HPLC, and GPC. Data were usedto explain their behaviour toward packaged food productsin PP packaging. 18 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.708984

Item 265European Polymer Journal34, No.12, Dec.1998, p.1817-28CURING OF POLYMER COMPOSITES. I. NMRCHARACTERIZATION OF COMPONENTMONOMERSMartin S J; O’Brien J E; Dowling J; McBrierty V JDublin,Trinity College; Bausch & Lomb Inc.

The use of NMR to probe the in-situ curing of monomermixtures commonly encountered in the manufacture ofcontact lenses was studied. Spectral lines were identifiedwhich monitored curing with time of individualcomponents in the monomer mix. This information canaid in gaining an understanding of the overall curingdynamics and provide important guidance in establishingsuitable protocols in the manufacturing process. As aprecursor to this goal, several commonly-used componentmaterials were characterised by high resolution protonand carbon-13 NMR spectroscopies. The efficacy of theoverall procedure is demonstrated. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; IRELAND;WESTERN EUROPE

Accession no.706520

Item 266Polimeros: Ciencia e Tecnologia8, No.1, Jan./March 1998, p.46-53PortugueseTHERMAL STABILITY OF POLYETHYLENETEREPHTHALATE PACKAGING:DETERMINATION OF OLIGOMERSFreire M T de A; Reyes F G R; Castle LCampinas,Universidade Estadual; UK,Min.ofAgriculture,Fisheries & Food

PETP food packaging materials were subjected todifferent heating conditions (50 minutes at 120-230C),and oligomers were identified by HPLC coupled withmass spectrometry and used as a parameter for evaluatingthe thermal stability of PETP. Small changes in oligomerdistribution were observed only for samples heated at230C, suggesting that PETP was thermally stable underthe heating conditions employed. The results alsosuggested the suitability of PETP as a food packagingmaterial for use in conventional and microwave ovens,and for secondary recycling under controlled conditions.28 refs.BRAZIL; EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.706082

Item 267Journal of Thermal Analysis and Calorimetry52, No.2, 1998, p.261-74THERMAL ANALYSIS OF SOMEENVIRONMENTALLY DEGRADABLEPOLYMERSDay M; Cooney J D; Shaw K; Watts JCanada,National Research Council

The thermal characteristics of a series of degradablepolymers for use in commercial composting facilities wasinvestigated using TGA and DSC. Phase changesassociated with some of the polymers investigated maycause problems in the interpretation of data fromcomposting degradation studies. Several biodegradable



polymers were observed to have melt transitions attemperatures similar to those found in a compostingenvironment. 19 refs.CANADA

Accession no.705674

Item 268Journal of Applied Polymer Science70, No.12, 19th Dec.1998, p.2457-61NUCLEAR MAGNETIC RESONANCE STUDYOF COMMERCIAL POLY(VINYL ACETATE)De Souza C M G; Tavares M I BRio de Janeiro,Universidade Federal

The commercial poly(vinyl acetate) bulk was studied byNMR at solution and solid state to understand thebehaviour of this polymer to obtain information onstructure, sample molecular mobility, and heterogeneity.To analyse the behaviour of this polymer, NMRtechniques were chosen, such as carbon-13 solution,magic angle spinning, cross-polarisation/magic anglespinning, proton spin-relaxation time in the rotating frameparameter and dipolar dephasing experiment. 13 refs.BRAZIL

Accession no.705529

Item 269Journal of Thermal Analysis and Calorimetry52, No.1, 1998, p.145-55GermanTHERMOANALYTICAL CHARACTERISINGUV-CURED POLYMER FILMSHosselbarth B; Friese K; Geyer WInstitut fuer Oberflaechenmodifizierung eV; Leipzig-Halle Ltd.; Umweltforschungzentrum

Thermooxidative and thermomechanical stabilities ofradiation-cured acrylates and epoxides were examined byTGA, DMA and DSC. The polymeric trifunctionalacrylates PETIA, TMPTA and THEIC displayed thehighest temperatures of onset of degradation. The highcrosslinking density of the films resulted in an almosttemperature-independent complex E-modulus, asmeasured by DMA. With increasing degree ofethoxylation or propoxylation of the monomers, decreasesin thermal stability and strength were found. Fordifunctional polymeric acrylates and epoxides, the TGtemperature was measured. The average degree of curingof UV-cured epoxy films could be determined from thetemperature of the maximum in the loss modulus. 13 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.705282

Item 270Journal of Thermal Analysis and Calorimetry52, No.1, 1998, p.131-43German

DETERMINATION OF VINYL ACETATECONTENT IN EVA COPOLYMERS. FACILITIESAND LIMITS OF APPLICATIONS OF MASSSPECTROMETRY ANALYSIS METHODSHaussler L; Pompe G; Albrecht V; Voigt DDresden,Institut fuer Polymerforschung

Ethylene-vinyl acetate copolymers were investigated bysimultaneous thermal analysis and pyrolysis gaschromatography. Both devices were coupled to a massspectrometer. Calibration with polyvinyl acetate led tosufficient accuracy in relation to the vinyl acetate content,because of the linear calibration plot. Quantitativedetermination of vinyl acetate was carried out at both 500and 700 C. The calibration plot was linear provided thatthe mass of vinyl acetate did not exceed a critical value.18 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.705281

Item 271Composites Science & Technology58, No.10, 1998, p.1641-7CHEMICAL ANALYSIS OF A FIELD-FAILEDCOMPOSITE SUSPENSION INSULATORChughtai A R; Smith D M; Kumosa M SDenver,University

The type of corrosive environment responsible for brittlefracture of suspension composite insulators wasestablished. A series of FTIR experiments was performedto identify chemical functionalities formed during thedegradation process of composite insulators affected bybrittle fracture. It was shown that the brittle fractureprocess was caused by the formation of nitric acid eitheroutside or inside an insulator leading to stress corrosioncracking of the glass/polymer composite rod material.Nitrate was detected on the composite fracture surfacesinside a 115 kV suspension composite insulator whichfailed in service by brittle fracture. 17 refs.USA

Accession no.705241

Item 272International Journal of Adhesion & Adhesives18, No.5, 1998, p.319-31LOW RESOLUTION PULSED NMR ANDULTRASOUND STUDY TO MONITOR THECURE OF AN EPOXY RESIN ADHESIVECocker R P; Chadwick D L; Dare D J; Challis R EKeele,University; Manchester,Metropolitan University

The cure of an epichlorohydrin-bisphenol A resin andcuring agent containing a primary diamine and an amido-polyamine was studied using two complementarytechniques, low resolution pulsed NMR spectroscopy andmeasurement of pulsed broad bandwidth ultrasoundpropagation velocity and absorption changes. The two



techniques independently gave a similar picture of thecure process, predicting cure events at the same times.The results obtained indicated that the cure followeddistinct phases, i.e. an initial liquid stage where shortpolymer chains were formed, followed by a second stagewhere longer molecules developed, a third stage wherecrosslinking between chains occurred and the adhesivebegan to solidify, and a final stage when solidificationwas completed. 19 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.704884

Item 273Polymer Degradation and Stability62, No. 1, Oct. 1998, p.41-8MECHANISMS OF THERMAL DEGRADATIONOF A POLYESTER FLAME-RETARDED WITHANTIMONY OXIDE/BROMINATEDPOLYCARBONATE STUDIED BYTEMPERATURE-PROGRAMMED ANALYTICALPYROLYSISSato H; Kondo K; Tsuge S; Ohtani H; Sato NNagoya,University; Toray Research Center Inc.

Thermal degradation of a flame-retarded PBTP consistingof PBTP and a synergistic flame-retardant system basedon brominated polycarbonate (copolycarbonatecontaining units from bisphenol A and tetrabrominatedbisphenol A plus tribromophenoxy end groups) andantimony trioxide was studied by means of varioustemperature-programmed analytical pyrolysis techniquessuch as temperature-programmed pyrolysis-massspectrometry, temperature-programmed pyrolysis-atomicemission detection and temperature-programmedpyrolysis-gas chromatography. During the degradation ofthe flame-retarded PBTP, brominated phenols were firstobserved to evolve at temperatures slightly lower thanthose for the flammable product evolution from thesubstrate polymer PBTP, followed by the evolution ofhydrogen bromide over the whole range of degradationtemperatures for the substrate polymer. These degradationprocesses were closely related to the synergistic effectsof antimony trioxide on the decomposition of brominatedpolycarbonate in the flame-retardant system to promotethe thermal degradation of brominated polycarbonate atlower temperatures than those for pure brominatedpolycarbonate. Furthermore, the evolution of the flamepoisoning antimony tribromide formed through thereaction between brominated polycarbonate and antimonytrioxide could also be monitored directly by temperature-programmed pyrolysis techniques. On the basis of thedata obtained by these temperature-programmed pyrolysistechniques, the thermal degradation of the flame-retardedPBTP and synergistic flame-retarding mechanisms arediscussed. 10 refs.JAPAN

Accession no.704607

Item 274Revista de Plasticos Modernos74, No.495, Sept.1997, p.255-61SpanishFTIR SPECTROPHOTOMETRY FOR THEDETECTION OF MICROSTRUCTURALCHANGES IN A POLYPROPYLENE/POLYETHYLENE COPOLYMER CAUSED BYARTIFICIAL AGEINGRomeu J; Pages P; Carrasco FCataluna,Universidad Politecnica; Girona,Universidad

A study was made of microstructural changes occurringin blue and red samples of an ethylene-propylenecopolymer exposed to artificial ageing in a Xenotestchamber for up to 5000 hours. The effects of ageingwere quantified by Fourier transform IRspectrophotometry. By calculating the reducedabsorption in selected spectral bands, it was possibleto detect oxidation and chain scission reactions andvariations in isotacticity which differed in thedifferently coloured specimens. 8 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.702522

Item 275Journal of Applied Polymer Science70, No.7, 14th Nov.1998, p.1307-10MULTIDIMENSIONAL SPECTROMETRY ANDMAPPINGFateley W G; Deverse R A; Hammaker R MKansas State University

A new inexpensive approach is described for mappingmolecular structure in polymeric materials which includesthe combination of interferometers and Hadamardtransform techniques to perform multidimensionalspectometry and mapping. 17 refs.USA

Accession no.702159

Item 276Journal of Materials Science.Materials in Medicine9, No.9, Sept.1998, p.529-33INVESTIGATION OF GLASS-IONOMERCEMENTS USING DIFFERENTIAL SCANNINGCALORIMETRYKhalil S K H; Atkins E D TBristol,University

Six commercial glass-ionomer cements commonly usedfor various dental applications were investigated usingDSC. Heat flow behaviour and heat capacity of thecements were measured during isothermal (at 37 C) settingreactions. All materials underwent an exothermic settingprocess, but with different enthalpies of reactions anddifferent heat capacities; there were no remaining endo-or exothermic reactions after the setting of the cement.



All materials examined were effective thermal insulators.18 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.702142

Item 277Journal of Materials Science33, No.14, 15th July 1998, p.3511-7MOLECULAR ORGANISATION INSTRUCTURAL PVDFGlennon D; Cox P A; Nevell R T; Nevell T G; Smith JR; Tsibouklis J; Ewen R JPortsmouth,University; West of England,University

Poly(vinylidene fluoride) containing 10% dibutyl sebacateplasticiser, as used in the construction of flexible oil andgas pipelines, was exposed to raised temperatures forprolonged periods of time, to acid etching and to varioustensile deformation regimes. The effects of thesetreatments on crystallinity and surface properties of thismaterial were examined in the light of analytical dataobtained by FTIR, DSC, X-ray diffraction, X-rayphotoelectron spectroscopy, goniometry and a variety ofmicroscopy techniques. 36 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.701984

Item 278Food Additives and Contaminants15, No.3, 1st April 1998, p.346-54PARTS-PER-TRILLION DETERMINATION OFSTYRENE IN YOGHURT BY PURGE-AND-TRAPGAS CHROMATOGRAPHY WITH MASSSPECTROMETRY DETECTIONNerin C; Rubio C; Cacho J; Salafranca JZaragoza,University

Headspace sampling methods prior to capillary gaschromatography are widely used for the determinationof volatile compounds present in very different types ofsamples. An automated and rapid system fordetermination of volatiles from yoghurt was developed.Thirty-five volatile organic compounds(VOCs) wereidentified in PS cups used for yoghurt packaging and 42VOCs from yoghurt samples. Quantitative analysis ofstyrene in several samples from the Spanish retail marketwas carried out. 16 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.700270

Item 279Journal of Applied Polymer Science70, No.6, 7th Nov.1998, p.1201-7PHOTODEGRADATION OF TEFLON AF1600DURING XPS ANALYSIS

Popovici D; Sacher E; Meunier MMontreal,Ecole Polytechnique

Teflon, type AF1600, which contains perfluorinateddioxole rings, was found to suffer significant degradationwhen exposed to X-rays whilst undergoing investigationby X-ray photoelectron spectroscopy. The degradationmechanism was significantly different to that offluoropolymers which contain only carbon and fluorine.It was established that oxygen was at least as twice assusceptible as fluorine, and that the amounts of oxygenloss were equal to those of fluorine. Oxygen could bedegraded by the breaking of only one bond, the oxygenthen forming a free radical. The free radicals producedby scission of carbon-carbon bonds participated inreactions leading to degradation and crosslinking. 9 refs.CANADA

Accession no.700200

Item 280Polymer International47, No.1, Sept.1998, p.72-5TEMPERATURE-MODULATED DIFFERENTIALSCANNING CALORIMETRY. II.DETERMINATION OF ACTIVATION ENERGIESZhong Jiang; Hutchinson J M; Imrie C TAberdeen,University

Alternating differential scanning calorimetry (ADSC), acommercial development of temperature-modulateddifferential scanning calorimetry, was used to determine theactivation energy associated with the relaxation processesin polycarbonate in the region of the glass transition. In thisprocedure the frequency of the temperature modulation isvaried over a range of approximately one decade, and themid-point of the step change in the complex heat capacity isevaluated. In these experiments, two different amplitudesof temperature modulation were employed. The results werein agreement with each other, and in good agreement withpublished values. Ripples seen on the Fourier-transformedsignals are attributed to the mode of the data analysis, andnot to noise on the data. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.700165

Item 281Materials World6, No.10, Oct.1998, p.617-9THROWING LIGHT ON FIBRES ANDCOMPOSITESYoung BManchester,University

The use is discussed of Raman spectroscopy to monitorthe stresses and strains on individual fibres in compositematerials. New instrumentation has caused rapid growthin the use of Raman spectroscopy for materialscharacterisation, including the introduction of charged-



coupled device cameras which offer significantimprovements in sensitivity and very low noise, and alsoholographic notch filters which are used to remove the laserline and allow single monochromators to be used. Boththese developments are incorporated in the Raman imagingmicroscope developed by Renishaw in collaboration withLeeds University Physics Department. Its use is describedwith reference to aramid fibre reinforced PP. 5 refs.

RENISHAW PLCEUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.699334

Item 282Farbe und Lack104, No.10, 1998, p.93/8GermanMODULATED DIFFERENTIAL SCANNINGCALORIMETRYHaessler RDresden,Institut fuer Polymerforschung

The use of modulated DSC for improved interpretationof product characteristics under thermal effects wasinvestigated. Tgs, for example, which are masked by post-curing or enthalpy relaxation, could be detected in a singlemeasurement and compared. The separation of complextransitions in multicomponent systems into individualparts such as melts, transition temps. and relaxations wasshown to be feasible. The potential for use of modulatedDSC in the field of epoxy resins was demonstrated usingexamples of the determination of Tg near the regions ofenthalpy relaxation, melt and post-curing. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.699054

Item 283Structure and properties of Oriented Polymers. SecondEdition.London, Chapman & Hall, 1997, p.234-68. 9NUCLEAR MAGNETIC RESONANCESpeiss H WMax-Planck-Institut fuer PolymerforschungEdited by: Ward I M(Leeds,University)

The basics of solid state NMR are outlined and the site-selective information available from multi-dimensionalNMR spectra about molecular order and dynamics inoriented polymers is illustrated with specific experimentalexamples. 55 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.697739

Item 284Structure and properties of Oriented Polymers. SecondEdition.

London, Chapman & Hall, 1997, p.181-233. 9INFRARED DICHROISM, POLARISEDFLUORESCENCE AND RAMANSPECTROSCOPYBower D ILeeds,UniversityEdited by: Ward I M(Leeds,University)

The three spectroscopic techniques for studyingmolecular orientation in polymers described in detailuse polarised electromagnetic radiation. The principlesof the techniques are outlined, relevant theory andexperimental details described, and a selection of resultspresented. 79 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.697738

Item 285Polymer39, No.20, 1998, p.4973-6EFFECTS OF SUBSTRATE INTERACTIONS INTHE LIQUID CHROMATOGRAPHY OFPOLYMERSKosmas M K; Bokaris E P; Georgaka E GIoannina,University

The elution behaviour of PMMA samples was studiedthrough two liquid chromatographic columns, onecontaining a substrate of silica covered with trimethylsilylgroups and the other a substrate of pure silica. Bothsubstrates had the same pore size and the solvent was thesame for both columns. The results were discussed andthey showed that the polymer-surface interactionschanged when the nature of the substrate was changed.14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;WESTERN EUROPE

Accession no.696588

Item 286Food Additives and Contaminants15, No.1, 1st Jan.1998, p.93-9SYSTEMATIC STUDY ON THE STABILITY OFSELECTED POLYMER ANTIOXIDANTS IN EUOFFICIAL AQUEOUS AND ALTERNATIVEFOOD SIMULANTS USING HPLCDemertzis P G; Franz RFraunhofer Institute for Food Technol. & Packag.

Details are given of the stability of five commercialantioxidants in food simulants and in an alternative fatsimulant. Analysis was performed using a rapid HPLCmethod with UV detection. 23 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.695963



Item 287Colloid & Polymer Science276, No.7, July 1998, p.565-9DESCRIPTION OF THE GLASS TRANSITIONMEASURED BY TEMPERATURE MODULATEDDIFFERENTIAL SCANNING CALORIMETRYSchawe J E KUlm,University

The temp. modulated DSC (TMDSC) technique could beused for heat capacity spectroscopy in the low frequencyrange. The measured property was the complex heatcapacity. The frequency-dependent relaxation transitionmeasured by TMDSC occurred in the temp. range of thethermal Tg. The non-equilibrium of the glassy state thusinfluenced the TMDSC curves. Experimental evidencewas the dependence of the shape of the heat capacity curveon the thermal history. A theoretical description of theinfluence of the non-equilibrium state on the spectroscopiccurves, based on the Tool-Narayanaswamy-Moynihanmodel, is presented. 23 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.695591

Item 288Composites Plastiques Renforces Fibres de VerreTextileNo.21, May/June 1997, p.48-54FrenchDURABILITY OF COMPOSITES: HOW TOACHIEVE RELIABLE ACCELERATED AGEINGSiampiringue N; Gaumet S; Lemaire JCentre National d’Evaluation de Photoprotection

The use of accelerated ageing tests andspectrophotometric techniques in studying thephotooxidative degradation of unsaturated polyester resinsand glass fibre-reinforced composites is examined.Results of accelerated and natural ageing tests arecompared, and criteria to be taken into account inachieving accelerated test results representative of realityare discussed. 5 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.695308

Item 289Polimeros: Ciencia e Tecnologia7, No.3, July/Sept.1997, p.19-23PortugueseFAILURE ANALYSIS OF MATERIALS BYADVANCED MICROSCOPIC TECHNIQUESChinaglia C R; Correa C ASao Carlos,Universidade Federal

Failure analysis techniques allowing the determinationof the chemical composition of a sample and its correlationwith the observed fracture mode are examined. Topics

discussed include the use of SEM in studying fracture inmineral filled thermoplastics, secondary electron imagingin obtaining information on sample topography,backscattered electron imaging in studying fillerdispersion in polymer matrices, and energy dispersive X-ray spectroscopy in determining the chemical compositionof the fillers or contaminants responsible for fractureinitiation. 5 refs.BRAZIL

Accession no.695299

Item 290Journal of Polymer Science : Polymer Physics Edition36, No.12, 15th Sept.1998, p.2165-75DESCRIPTION OF THERMAL RELAXATION OFPOLYSTYRENE CLOSE TO THE THERMALGLASS TRANSITIONSchawe J E KUlm,University

Using spectroscopic methods at relatively high frequency,the alpha-relaxation was measured in the thermodynamicequilibrium. In the caloric case this phenomenon is calledthermal relaxation transition. Using a conventionaldifferential scanning calorimeter, the transition of theequilibrium (the melt) into a nonequilibrium (the glassystate) was measured. This effect is called thermal glasstransition. Temperature-modulated DSC curves in theglass transition region were described using the Tool-Narayanaswamy-Moynihan model. 54 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.694872

Item 291Journal of Polymer Science : Polymer Physics Edition36, No.12, 15th Sept.1998, p.2103-9RAPID DETERMINATION OF COMONOMERCONTENT, CRYSTALLINITY, AND LONGSPACING BY MULTIPLE-PULSE PROTON NMRIN ETHYLENE-VINYL ALCOHOLCOPOLYMERSPerez E; Cerrada M L; Vanderhart D LInstituto de Ciencia y Tecnologia de Polimeros;US,National Institute of Standards & Technology

Capitalising on the superior sensitivity of proton NMR,relatively rapid estimates of three parameters, namely,comonomer content, crystallinity, and long spacing, weredetermined for three ethylene-vinyl alcohol copolymersusing solid state proton NMR measurements. Multiple-pulsetechniques were utilised (a) in conjunction with magic anglespinning for measuring comonomer content, (b) inconjunction with a relaxation time measurement fordetermining crystallinity, and (c) in conjunction with arelaxation time-based spin diffusion measurement fordetermining the long spacing. These three parameters,extracted from data collected in a total spectrometer time of



about 20 min., and were compared with similar parametersobtained using more conventional DSC, small angle X-rayscattering (including synchrotron), and solution-state NMRmeasurements, with good agreement. 23 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN; USA;WESTERN EUROPE

Accession no.694867

Item 292Smart Materials & Structures7, No.4, Aug. 1998, p.557-68IN SITU CURE MONITORING USING OPTICALFIBRE SENSORS. A COMPARATIVE STUDYPowell G R; Crosby P A; Waters D N; France C M;Spooncer R C; Fernando G FBrunel University; Cranfield,University

A comparative study is presented for different types ofoptical fibre sensor developed to monitor the cure of anepoxy resin system. The sensors were based ontransmission spectroscopy, evanescent wave spectroscopyand refractive index monitoring. 19 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.694840

Item 293Polymer Testing ’97. Day 3: Chemical Analysis.Conference proceedings.Shawbury, 7th-11th April 1997, Paper 4. 9TRAMAN SPECTROSCOPY OF POLYMERSWilliams K P J; Wilcock I CRenishaw plc(Rapra Technology Ltd.; Plastics & Rubber Weekly;European Plastics News)

Raman spectroscopy is now coming of age as a routineanalytical method. Advances in Raman technology havemeant that robust, user-friendly equipment can bemanufactured at a reasonable cost. These advances aredescribed, together with applications of Raman imagingmicroscope systems to polymer analysis. 11 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.694712

Item 294International Polymer Processing13, No.2, July 1998, p.142-8PEROXIDE INDUCED CROSSLINKING ANDDEGRADATION OF POLYAMIDEYu Q; Zhu SMcMaster University

Peroxide-induced crosslinking and degradation of nylon12 were investigated using ESR. Various reactionmechanisms are proposed. 20 refs.CANADA

Accession no.694268

Item 295Macromolecular Chemistry & Physics199, No.8, 1998, p.1623-9THERMAL STABILITY ANDCRYSTALLISATION KINETICS OF PEEKChen J-Y; Chen M; Chao S-CTaiwan,National Sun Yat-Sen University

TGA, dynamic rheological analysis and polarised lightmicroscopy were used to assess thermal stability of PEEK.Emphasis is given to the effect of melting temperature onthermal stability. 23 refs.CHINA

Accession no.694246

Item 296Injection Molding6, No.8, Aug. 1998, p.56/9MATERIALS ANALYST: PART 13.PERFORMANCE PROBLEMS: WHEN THEPELLETS DON’T MATCH THE PARTSSepe MDickten & Masch Mfg.

The use of differential scanning calorimetry andthermogravimetric analysis as analytical tools in partfailure determination is applied. Problems are examinedin part performance of moulded 30% glass-reinforced,low-viscosity PEI and a second part moulded from PPSwith proprietary additives to improve wear resistance. Theimportance of checking the composition of the basicmaterial is stressed.USA

Accession no.693205

Item 297Journal of Applied Polymer Science69, No.11, 12th Sept.1998, p.2175-85IR SPECTROSCOPY AS A QUANTITATIVE ANDPREDICTIVE ANALYSIS METHOD OFPHENOL-FORMALDEHYDE RESOL RESINSHolopainen T; Alvila L; Rainio J; Pakkanen T TJoensuu,University; Dynoresin Oy

A set of resin samples was characterised by IR and carbon-13 NMR spectroscopy. The suitability of IR spectroscopyfor the quantitative analysis of resins was evaluated bystatistical methods using the NMR reference data ascalibration. The values of interesting properties, e.g. theamount of free phenol and the formaldehyde-to-phenolmolar ratio, of the resins being similar to the calibrationresins were predicted from the IR spectra. The predictedresults were compared with those observed by carbon-13NMR spectroscopy. 15 refs.FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.692990

Item 298Journal of Materials Science33, No.13, 1st July 1998, p.3245-9



XPS MONITORING OF THE REMOVAL OF ANAGED POLYMER COATING FROM A METALSUBSTRATE BY TEA-CARBON DIOXIDELASER ABLATIONCottam C A; Emmony D C; Cuesta A; Bradley R HLoughborough,University; Aberdeen,Robert GordonUniversity

X-ray photoelectron spectrometry was used to observethe changes in surface chemistry during the removal ofpaint from a zinc coated steel substrate using TEA-carbondioxide laser ablation. Laser ablation at both plasma andsub-plasma fluences were investigated and their relativemerits discussed. The laser was shown to be effective inpaint removal and was not impaired by ageing in the paint.32 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.692055

Item 299Analytical Chemistry70, No.15, 1st Aug.1998, p.3298-303IMPROVEMENTS IN POLYMERCHARACTERIZATION BY SIZE-EXCLUSIONCHROMATOGRAPHY AND LIQUIDCHROMATOGRAPHY AT THE CRITICALCONDITION BY USING ENHANCED-FLUIDITYLIQUID MOBILE PHASES WITH PACKEDCAPILLARY COLUMNSHao Yun; Olesik S V; Marti E HOhio,State University; Ashland Chemical Co.

The use of the above combination of techniques isdescribed and results obtained for samples of PS, PMMA,styrene-methyl acrylate copolymers and functionalisedPS are presented and discussed. 32 refs.USA

Accession no.691471

Item 300Polymer39, No.22, 1998, p.5293-300QUANTITATIVE CARBON-13 SOLID-STATENMR AND FT-RAMAN SPECTROSCOPY INNOVOLAC RESINSOttenbourgs B; Adriaensens P; Carleer R; VanderzandeD; Gelan JLimburg,University

A qualitative and quantitative study of the curing behaviourof a high-ortho novolac resin with paraformaldehyde underdifferent conditions was conducted. The degree of cure asa function of the formaldehyde/phenol ratio, the degree ofconversion and the final structure after curing weredetermined on the basis of a quantitative carbon-13 solidstate NMR with cross-polarisation and magic anglespinning. The spin-lattice relaxation time was measuredas a probe to follow the evolution of cure. Fourier

transform-Raman spectroscopy was proposed as aqualitative tool to follow the degree of crosslinking in thishigh-ortho novolac. 54 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;WESTERN EUROPE

Accession no.689414

Item 301Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.1415-7. 012IN SITU SPECTROSCOPY OF CO2-INDUCEDPLASTICISATION OF GLASSY POLYMERSKazarian S G; Brantley N H; Eckert C AGeorgia,Institute of Technology(SPE)

In situ spectroscopy is used to study the plasticisation ofglassy polymers by high-pressure and supercritical CO2.The methodology for in situ spectroscopic analysis of theinteractions between CO2 and polymers is described. Thechanges in IR spectra of CO2 incorporated into variouspolymers indicate a specific interaction between CO2 andpolymer functional groups. Increased polymer segmentalmobility is also observed, indicative of the plasticisationphenomenon. Implications of these discovered molecularinteractions are discussed. 25 refs.USA

Accession no.687565

Item 302Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.1860-4. 012QUANTITATIVE ANALYSIS OF CHEMICALBLOWING AGENTS BY DSCPrasad A; Shanker MMillennium Petrochemicals Inc.(SPE)

It is shown that differential scanning calorimetery (DSC)can be used to determine quantitatively the level andcomposition of chemical blowing agents such asazodicarbonamide (azo) in commercial formulations.DSC can also be used to obtain the onset of decompositiontemperature and the rate of decomposition of azo in thepresence of group II and group IV metal salt activators.DSC has the potential to detect the level of undecomposedblowing agents present in processed foam products andto qualitatively determine the degree of dispersion of theblowing agent and the activators in commercialformulations. Advantages of DSC over the currently usedEGA technique are ease of operation, shorter analysis timeand detection of azo concentrations as low as 1%. 12 refs.USA

Accession no.687551

Item 303Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.2114-8. 012



APPLICATION OF GC/MS INTHERMOPLASTICS PROBLEM SOLVINGShaker D C; Kim H CLNP Engineering Plastics(SPE)

The use of GC/MS (gas chromatography/mass spectrometry)in the thermoplastics problem solving area is outlined. GC/MS is a hyphenated technique; i.e. it combines the twotechniques, chromatography and spectroscopy. In thisprocedure, a material is introduced into the GC, componentsare separated and sent to the MS where they are ionised, andthe resulting particles are separated by mass. The applicationsof GC/MS to solving complex problems are discussedthrough positive identification of base resins, contamination,odours and solvents.USA

Accession no.687499

Item 304Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.2101-5. 012TEMPERATURE GRADIENT INTERACTIONCHROMATOGRAPHY OF POLYMERSChang T; Lee W; Lee H C; Mays J W; Harville S;Frater D JPohang,University of Science & Technology;Alabama,University at Birmingham(SPE)

Temperature gradient interaction chromatography (TGIC)is a conventional reversed phase BPLC technique, but thecolumn temperature is varied during elution. A very fineand reproducible control of interaction between polymerchains and the stationary phase can be achieved by changingthe column temperature. Under a suitable temperatureprogramming, this method provides a far superior resolutionto conventional size exclusion chromatography. In addition,elution in TGIC is more sensitive to molecular weight alone.Thus it provides an excellent route to separating branchedpolymer molecules of similar hydrodynamic volume butdiffering molecular weight. 8 refs.KOREA; USA

Accession no.687496

Item 305Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.2037-41. 012MODULATED DIFFERENTIAL SCANNINGCALORIMETRY TO STUDY REACTINGPOLYMER SYSTEMSVan Mele B; Van Assche G; Van Hemelrijck ABrussels,Free University(SPE)

Modulated (temperature) differential scanning calorimetry(MTDSC or MDSC) is used to simultaneously study theevolution of heat flow and heat capacity for the isothermaland non-isothermal reactions of polymer systems. An

epoxy-anhydride thermosetting system is used as anexample. Vitrification and devitrification steps areobserved. The heat flow phase during isothermal andnonisothermal cure is always small, but its evolutioncontains information on relaxation phenomena, vitrificationand devitrification, in the course of the chemical reaction.Modelling of the (heat flow related) chemical kinetics andthe (heat capacity related) mobility restrictions contributesto a better understanding of the reaction mechanism andreaction kinetics up to a high degree of chemicalconversion. The use of MTDSC as a tool for a quantitativeconstruction of the vitrification curve in Temperature-Time-Transformation and Continuous-Heating-Transformationdiagrams is illustrated. 20 refs.BELGIUM; EUROPEAN COMMUNITY; EUROPEAN UNION;WESTERN EUROPE

Accession no.687483

Item 306Antec ’98. Volume II. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.2215-8. 012PRACTICAL ANALYSIS TECHNIQUES OFPOLYMER FILLERS BY FOURIERTRANSFORM INFRARED SPECTROSCOPY(FTIR)Coles B J; Hall C JHauser Inc.(SPE)

The identification of polymers by FTIR is oftencomplicated by the presence of fillers. However for kaolinclay, an FTIR analysis should be able to identify the fillerand predict its concentration using a standard curve. Theresulting percentage is more reliable than a simple ash,which may change the chemical composition of the filler.2 refs.USA

Accession no.687418

Item 307Polymer Engineering and Science38, No.6, June 1998, p.922-5IDENTIFICATION OF OFF-FLAVOURCOMPOUNDS IN HDPE WITH DIFFERENTAMOUNTS OF ABSCENTSVillberg K; Veijanen A; Gustafsson IJyvaskyla,University; Borealis AB

Details are given of the addition of zeolite to HDPEdrinking water pipes in an attempt to eliminate odoursand to remove odour-causing compounds. The systemused for analysis of volatile organic compounds was agas chromatographic/mass spectrometric sniffing system.Purge and trap techniques were used to introduce thevolatile, off-flavour components into the gaschromatograph. 16 refs.FINLAND; SCANDINAVIA; SWEDEN; WESTERN EUROPE

Accession no.686400



Item 308Polymer39, No.19, 1998, p.4665-73SURFACE GLASS TRANSITION BEHAVIOUROF AMORPHOUS POLYMER FILM BYSCANNING FORCE MICROSCOPY ANDSURFACE SPECTROSCOPYKakiyama T; Tanaka K; Takahara AKyushu,University

The surface molecular motion of amorphous polymericsolids was measured by lateral force microscopy, scanningviscoelasticity microscopy, and differential X-rayphotoelectron spectroscopy. Data are given for PS andstyrene-methyl methacrylate copolymers. 35 refs.JAPAN

Accession no.686392

Item 309Revista de Plasticos Modernos73, No.487, Jan.1997, p.26-31SpanishTEMPERATURE MODULATED DIFFERENTIALSCANNING CALORIMETRY: A STEP FORWARDIN STUDYING THE THERMAL PROPERTIESOF POLYMERSPerena J MInstituto de Ciencia y Tecnologia de Polimeros

The principles of temperature modulated DSC aredescribed, and a number of examples are presented of itsapplication to studies of the thermal properties of plastics.Some limitations of the technique are also examined. 6refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.686251

Item 310Analytical Chemistry70, No.13, 1st July 1998, p.456A-61ACHARACTERISING SYNTHETIC POLYMERSBY MALDI MSKuang Jen Wu; Odom R WEvans C.,& Associates

An review is given of the use of matrix-assisted laserdesorption/ionisation time-of flight (MALDI TOF) massspectroscopy to determine MWDs and structures ofsynthetic organic polymers, including the ion desorptionmechanism, synthetic polymer analysis, molecular weightanalysis, and its use in calibration of GPC profiles. 30refs.USA

Accession no.686157

Item 311Food Additives and Contaminants

15, No.2, 1998, p.217-28EFFECTS OF PACKAGING AND STORAGECONDITIONS ON VOLATILE COMPOUNDS INGAS-PACKED POULTRY MEATEilamo M; Kinnunen A; Latva-Kala K; Ahvenainen RVTT Biotechnology & Food Research;Finland,Technical Research Centre

Volatile compounds released by raw chicken legs packedin modified atmosphere packages were determined todevelop a spoilage indicator for monitoring the shelf lifeof raw chicken. The effects of four packaging factors(headspace volume, oxygen transmission rate of thepackage, residual oxygen and carbon dioxideconcentration) and three storage factors (temperature,illumination and storage time) on the amounts of volatilecompounds in the headspace of gas packages containingtwo chicken legs were studied. Statistical experimentaldesign was applied and a linear screening designcomprising 18 experiments (fractional factorial) wasutilised. Volatile compounds in package headspace weredetermined by gas chromatography/mass spectrometry.The results were compared with the results of sensoryevaluation and microbial determinations. 8 refs.FINLAND; SCANDINAVIA; WESTERN EUROPE

Accession no.686119

Item 312International Journal of Adhesion & Adhesives18, No.3, 1998, p.193-8USE OF XPS AND TOF-SIMS TO INVESTIGATEADHESION FAILURE OF A CATIONICRADIATION CURED COATING ONGALVANISED STEELLeadley S R; Watts J F; Rodriguez A; Lowe CSurrey,University; Becker Industrial Coatings

Details are given of coating delamination in a hot, humidenvironment for a cationic radiation cured coating ofcycloaliphatic epoxy resin. X-ray photoelectronspectroscopy and time-of-flight mass spectroscopy of thedelaminated surface showed that the phosphorushexafluoride anion of the photoinitiator segregates to theinterface. The durability of the coating was improved byreformulation with a reduced concentration ofphotoinitiator. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.684932

Item 313Antec ’98. Volume I. Conference proceedings.Atlanta, Ga., 26th-30th April 1998, p.816-20. 012METHODS FOR THE MEASUREMENT OFCRYSTALLINITY OF PREFORMS ANDBOTTLES MADE FROM PETPBashir Z; Al-Alouish I; Al-Raqibah I; Ibrahim MSABIC Corp.



(SPE)

PETP has established itself as a material for makinglightweight, clear and tough bottles. Ideally, a preformwith zero or very low crystallinity (for purposes of clarity)is sought, while the final bottle should have highcrystallinity (for enhancing gas barrier and mechanicalproperties). Monitoring crystallinity is thus important. Anattempt is made to evaluate methods of crystallinitymeasurement using density, differential scanningcalorimetry and modulated differential scanningcalorimetry to study the crystallinity of preforms andbottles. The applicability and appropriateness of eachtechnique for different PETP sample types, andinterpretation problems are also discussed. 20 refs.SAUDI ARABIA

Accession no.684627

Item 314Polymer Journal (Japan)30, No.5, 1998, p.439-43DIRECT DETERMINATION OF MOLECULARWEIGHT DISTRIBUTION BY SIZE EXCLUSIONCHROMATOGRAPHY(SEC) WITH 750 MHZPROTON NMR DETECTION (ON-LINE SEC-NMR)Ute K; Niimi R; Hongo S; Hatada KOsaka,University

The above on-line SEC-NMR technique was used toanalyse MWDs of isotactic PMMAs with Mn rangingfrom 3270 to 22,200. The molec.wt. of the polymer inflowing eluate was determined directly (without aconventional calibration procedure) from he relativeintensity of NMR signals due to the end group andrepeating units. The MWD determined in this manner wasproved to be accurate by SEC-NMR experiments onuniform isotactic PMMAs consisting of exactly 23, 40and 80 repeating units. Investigation was also undertakento optimise flow rate and NMR parameters for quantitativeSEC-NMR measurements. The signal-to-noise ratio of750 MHz SEC-NMR spectra was 9.2 times that obtainedpreviously with 500 MHz SEC-NMR operated undersimilar conditions. 17 refs.JAPAN

Accession no.684613

Item 315Shawbury, Rapra Technology Ltd., 1996, pp.150.95.00. 30cms. 9511ENVIRONMENTAL STRESS CRACKING OFPLASTICSWright D CRapra Technology Ltd.

This book reviews the factors which influenceenvironmental stress cracking, and examines the currentstate of knowledge regarding specific categories ofplastics. The book is divided into three main sections

focusing on the prediction of ESC and assessment bytesting, factors that influence ESC and data on specificplastics. Methods for the experimental evaluation ofenvironmental stress are described. This book isavailable for purchase from Publication Sales, RapraTechnology Ltd.

Accession no.683806

Item 316Journal of Adhesion Science and Technology12, No.5, 1998, p.507-21EFFECT OF CURING TEMPERATURE ON THEADHESION STRENGTH OF POLYAMIDEIMIDE/COPPER JOINTSCho J H; Kong D I; Park C E; Jin M YPohang,University of Science & Technology;Korea,Research Institute of Chemical Technology

The adhesion strength of polyamideimide/copper jointswas investigated as a function of the curing temperatureand time. The effects of copper oxide formed by thermaltreatment and alkaline treatment on the adhesive strengthof the joints were examined. The locus of failure of thejoints was also studied by SEM and X-ray photoelectronspectroscopy. 21 refs.KOREA

Accession no.682955

Item 317Polymer Engineering and Science38, No.4, April 1998, p.566-72DYNAMIC AND ISOTHERMALTHERMOGRAVIMETRIC ANALYSIS OF APOLYCYANURATE THERMOSETTING SYSTEMZacharia R E; Simon S LPittsburgh,University

Isothermal and dynamic thermogravimetric analysis(TGA) were performed on a polycyanurate thermosettingmaterial. The effects on thermal stability of the coppernaphthenate catalyst were studied by comparing twosystems with different amounts of catalyst. Tests wereperformed isothermally at temperatures ranging from 200-240C for times up to one week. Dynamic tests were alsoperformed at rates of 0.1 C/min to 40 C/min attemperatures ranging from 180 to 600C. Resultsdemonstrate the difficulties of extrapolating dynamic TGAdata to use conditions to predict long-term thermalstability. 14 refs.USA

Accession no.681689

Item 318European Polymer Journal34, No.2, Feb.1998, p.163-70STUDY OF TALC-ADDITIVE INTERACTIONSBY COMBINED TGA-FTIR SYSTEMBertin D; Boutevin B; Rigal G; Fourty G



Montpellier,Ecole Nationale Superieure de Chimie;Talcs de Luzenac SA

By using combined TGA/FTIR thermogravimetricanalysis, accurate real time qualitative and quantitativedata can be obtained for thermal decomposition ofpolymers. It was used to study interactions between anadditive and a filler (talc), highlighting a degradationphenomenon of additive by talc, and this phenomenondepended on the structure and chemical composition oftalc. This procedure also applied to analysis of degradationof other additives by talc. Thus, polymer formulationswill rapidly be optimised in various areas of filledpolymers. 12 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.681630

Item 319Journal of Polymer Science : Polymer ChemistryEdition36, No.9, 15th July 1998, p.1363-71LIQUID CHROMATOGRAPHY OFMACROMOLECULES AT THE CRITICALADSORPTION POINT. II. ROLE OF COLUMNPACKING: BARE SILICA GELBerek D; Janco M; Meira G RSlovak,Academy of Sciences; INTEC CONICET

Data are presented manifesting the role of columnpackings from the point of view of both their pore sizeand surface chemistry. Bare silica gels that are the mostcommonly used LC CAP column packings and modelmacromolecules, viz. narrow PMMA, were investigated.20 refs.ARGENTINA; SLOVAK REPUBLIC; SLOVAKIA

Accession no.681599

Item 32020th Annual Anniversary Meeting of the AdhesionSociety. Conference proceedings.Hilton Head Island, S.C., 23rd-26th Feb.1997, p.519-21. 8(10)USING XPS TO INVESTIGATE FIBRE/MATRIXCHEMICAL INTERACTIONS AT THEINTERFACE IN CARBON FIBRE REINFORCEDCOMPOSITESWeitzsacker C L; Xie M; Drzal L TMichigan,State UniversityEdited by: Drzal L T; Schreiber H P(US,Adhesion Society)

With composites expanding into areas from aerospace torecreation, different matrices are being investigated totailor composites to specific uses. The degree of adhesionbetween the fibre and matrix, influenced by chemicalreactions, mechanical interactions and topography at thefibre/matrix interface, has been recognised as a criticalfactor in determining the performance of fibre-reinforced

composites. The interaction and chemical reaction offunctional groups in the matrix with functional groups atthe fibrer surface contribute to the adhesion. Directanalysis of the fibre/matrix interface by surface analyticalmethods such as X-ray photoelectron spectroscopy is nottrivial due to the thickness of a matrix layer over fibresand the complexity of the matrix system. Indirect analysisof the matrix/fibre interface is possible using modelcompounds which represent functional groups wheredifferences in results are indicative of reaction betweenfibre and matrix. The matrix functional groups that maychemically react with the fibre surface can be separatedand investigated individually. Mixtures of modelcompounds can be used to investigate functional groupsreactions between the components, and with the fibresurface. Model compounds based on epoxy, polyimide,polyphenylene sulphide and vinyl ester matrices areinvestigated to characterise the chemical reactions at thefibre/matrix interface. XPS is used to characterise boththe carbon fibre surfaces and the reacted carbon fibresurfaces. The model compounds representative of eachof these matrices demonstrate the range of possiblereactions and interactions possible between the fibre andmatrix, ranging from no reaction to distinct chemicalreactions. 4 refs.USA

Accession no.681439

Item 321Cleanrooms12, No.5, Suppl. May 1998, p.S13/20APPLICATION OF FTIR FOR MONITORINGCLEANROOM AIR AND PROCESS EMISSIONSZazzera L; Reagen W3M Co.

The use of FTIR monitoring methods for HAP, VOC, PFCand HFC emissions for identification and quantificationin process exhaust and in clean room air, is discussed. Asummary is included of the various protocols, test methodsand references for the use of FTIR spectroscopy togenerate verifiable data. Results of field trials andlaboratory study trials are presented, which demonstrateits value as a monitoring method in the semiconductorindustryUSA

Accession no.679498

Item 322Analytical Chemistry70, No.8, 15th April 1998, p.1563-8POLYMER ANALYSIS BY MICRO-SCALE SIZE-EXCLUSION CHROMATOGRAPHY(SEC)/MALDI TIME-OF-FLIGHT MASSSPECTROMETRY WITH A ROBOTICINTERFACENielen M W FAkzo Nobel Central Research



A report is presented on the development of a micro-scaleSEC system in which the MALDI matrix solution iscoaxially added to the column effluent and directly spottedonto the MALDI targets in a robotic interface. Each spotcorresponds to the 10-s elution window from the micro-SEC column, thus yielding a narrow polymer distributionwhich is amenable to characterisation by MALDI massspectroscopy. The performance of the system isdemonstrated by the characterisation of a polybisphenolA carbonate and a complex dipropoxylated bisphenol A/adipic acid/isophthalic acid copolyester resin. 29 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.679150

Item 323Polymer Engineering and Science38, No.2, Feb.1998, p.265-73DSC STUDIES ON THE CRYSTALLISATIONCHARACTERISTICS OF POLY(ETHYLENETEREPHTHALATE) FOR BLOW MOULDINGAPPLICATIONSDaw-Ming Fann; Huang S K; Jiunn-Yih LeeTaiwan,National University of Science & Technology

The crystallisation behaviour of blow moulded PETPbottles, which helps determine the product’s transparency,was investigated by DSC dynamic cooling experimentsthat simulated the cooling that occurs in the injection blowmoulding manufacturing process. DSC measurementswere used to obtain information on related aspects, suchas the ease of crystallisation from glassy and molten statesand crystallinity in the products. An Avrami equation wasused for calculation of the crystallisation kineticparameters. 40 refs.TAIWAN

Accession no.678858

Item 324TAPPI 1997 Polymers, Laminations and CoatingsConference. Conference Proceedings. Book 1.Toronto, Ontario, 24th-28th Aug.1997, p.173-82. 012INFLUENCE OF MINERAL FILLERS ON THEPROCESSING OF LLDPE FILMSAnsari D M; Higgs R PECC International Ltd.(TAPPI)

A study was made of the thermal properties and meltrheology of linear LDPE masterbatches filled withcalcium carbonate, talc and calcined clay. Films wereprepared by extrusion blowing and temperature changeswere monitored along the bubble. Filler distribution withinthe films was assessed by optical and electron microscopy.Rheological properties of the diluted masterbatches wereevaluated over four decades of shear rate. The mineralfillers increased cooling rates and improved bubblestability. Coarser calcium carbonate grades gave the

greatest improvement, while fine grades and talc had littleeffect. Micrographs revealed the level of interparticlecontact and alignment of anisotropic particles which gaverise to the observed differences. Filler type and contentdid not significantly influence shear rheology at the shearrates associated with film extrusion. 17 refs.CANADA; EUROPEAN COMMUNITY; EUROPEAN UNION;UK; USA; WESTERN EUROPE

Accession no.677503

Item 325TAPPI 1997 Polymers, Laminations and CoatingsConference. Conference Proceedings. Book 1.Toronto, Ontario, 24th-28th Aug.1997, p.35-44. 012EFFECT OF TITANIUM DIOXIDE ONEXTRUSION STABILITYMerkley J HEastman Chemical Co.(TAPPI)

Rheological techniques for following the degradation andchanges in molecular weight and MWD of titaniumdioxide-filled polyolefins during extrusion coating areexamined. These include measurements of the crossoverpoint between loss modulus and storage modulus and thevariation in complex viscosity versus frequency curvesseen in the rotational mechanical spectrometer curves,variations in viscosity versus shear rate seen in thecapillary extrusion rheometer curves, and shifts in theDMTA curves.CANADA; USA

Accession no.677489

Item 326Journal of Polymer Science : Polymer ChemistryEdition36, No.5, 15th April 1998, p.851-60PEROXIDE INDUCED CROSSLINKING ANDDEGRADATION OF PVCYu Q; Zhu S; Zhou WMcMaster University

Peroxide induced crosslinking and degradation of PVCwere investigated using an on-line ESR technique. Thereaction variables included temperature, peroxide type andconcentration. The mechanism involved in the reactionwas determined base on the radical information. The gelcontent and swelling ratio were also measured. 38 refs.CANADA

Accession no.674965

Item 327Journal of Materials Science Letters17, No.6, 15th March 1998, p.511-3EVIDENCE OF MOLECULAR ORIENTATION INPOLY(3-BUTYLTHIOPHENE) FILMS BYELECTRON SPIN RESONANCEMEASUREMENTS



Pawlicka A; Walmsley L; Faria R M; Nascimento O RSao Paulo,University; Paulista,Universidade Estadual

It was demonstrated that ESR could show evidence ofmolecular orientation in films of poly(3-butyl thiophene),making ESR useful to study orientation in conjugatedpolymers when it is wished to avoid radiation damage orfor a non-destructive investigation before X-raymeasurements. 11 refs.BRAZIL

Accession no.674766

Item 328Macromolecules30, No.25, 15th Dec.1997, p.7970-6DSC, FT-IR, AND ENERGY DISPERSIVE X-RAYDIFFRACTION APPLIED TO THE STUDY OFTHE GLASS TRANSITION OF POLY(P-PHENYLENE SULPHIDE)Caminiti R; D’Ilario L; Martinelli A; Piozzi A; Sadun CRoma,Universita La Sapienza; Roma,Istituto Nazionaleper la Fisica della Materia

The glass transition of PPS was studied by means of DSC,FTIR spectroscopy and energy dispersive X-ray diffraction.All of the techniques showed the alpha-transition of thepolymer. The results of the different techniques wereconsistent if the onset temperature for the DSC experimentswas taken as representative of the glass transition. The glasstransition temperature was found to vary as a function ofthe heating rate. The activation energy of the glass transitionprocess was calculated by means of a theoretical model.The results were discussed. 47 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.672088

Item 329Kunststoffe Plast Europe88, No.2, Feb.1998, p.34-5WHAT HAS GONE WRONG?Sass ANRW GmbH

Practical case studies are used to demonstrate how usefuldifferential scanning microscopy analysis can be formaterial testing and damage analysis on plastics and plasticparts. It measures the physical and chemical properties ofthe plastic as a function of temperature. Information gainedby use of the analytical tool is examined, and case studiesrelating to fluctuating material quality through the use ofrecyclate, and the oxidation of PP water pipes are discussed.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.671875

Item 330Industrial & Engineering Chemistry Research37, No.3, March 1998, p.1140-53

SHEATH-CORE DIFFERENCES CAUSED BYRAPID THERMOOXIDATION DURING MELTBLOWING OF FIBRESKelley S L; Shambaugh R LOklahoma,University

A technique based on intrinsic viscosity measurementswas developed for measuring sheath and core molecularweights during melt blowing of fibres. A mathematicalmodel is described which accounts for rapid diffusion andthermooxidation. Experimental molecular weightmeasurements for PP fibres were compared withtheoretical predictions. 29 refs.USA

Accession no.670584

Item 331Polymer Bulletin40, No.2-3, Feb./March 1998, p.227-34COMPATIBILISATION OF POLYSULPHONE/POLYAMIDE BLENDS BY REACTIVEPOLYSULPHONES. EVIDENCE FORCOPOLYMER FORMATIONWeber M; Heckmann WBASF AG

Melt blending studies using polysulphone with differentfunctional groups and polyamide were performed in a batchtype mixer. Blends were investigated by solvent extractionand TEM. Model experiments revealed the possibility tocompatibilise these blends by reactive blending techniquesusing functionalised polysulphones. 14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.670478

Item 332Journal of Polymer Science : Polymer Physics Edition36, No.1, 15th Jan.1998, p.133-41NEW APPROACH FOR ESTIMATING THERECRYSTALLISATION RATE ANDEQUILIBRIUM MELTING TEMPERATUREHong Gyun Kim; Robertson R EMichigan,University

A method was described for measuring the heat and rateof crystallisation following partial melting. The methoduses a specific sequence of temperatures with a differentialscanning calorimeter, and the melting and recrystallisationprocesses were confirmed by optical observations. Themethod was applied to poly(butylene terephthalate). Themelting temperatures obtained from recrystallisation wereused in the Hoffman-Weeks equation to deduce 236 C asthe equilibrium melting temperature for PBTP. 22 refs.USA

Accession no.669994

Item 333Composites Science & Technology57, No.8, Aug.1997, p.975-83



EFFECTS OF SILANE COUPLING AGENTS ONTHE INTERPHASE AND PERFORMANCE OFGLASS-FIBRE REINFORCED POLYMERCOMPOSITESWu H F; Dwight D W; Huff N TOwens-Corning Science & Technology Center

A single filament model of a commercial glass fibre-reinforcement manufacturing process was used to applymethacryloxy and amino silanes with one, two and threesilanols to two different glass fibres in a molecular model.Surface analyses by angular-dependent X-rayphotoelectron spectroscopy, electric-kinetic analysis, andcontact-angle measurements were used to characterise thesurface coatings. The micro-indentation technique wasused to evaluate fibre-matrix interfacial adhesion.Changes observed in surface chemistry, micromechanics,and composite properties as functions of silanol type arecorrelated. Data includes molecular models of couplingagent on E-glass surface, chemisorption of coupling agentinto glass surface, isoelectric point values for eachtreatment, composite flexural strength, composite TS, andcomposite interfacial shear strength before and after 3-days in boiling water. Matrix was polyester resin (E-701from Owens Corning). 22 refs. (Presented at 6th Int. Conf.on Composite Interfaces, Microphenomena in AdvancedInterfaces, Zichron Yaacov, Israel, 5th-8th May 1996).USA

Accession no.669950

Item 334Polymer Bulletin39, No.6, Dec.1997, p.721-7COMPARISON OF CALIBRATION WITH PPGAND PS STANDARDS IN SIZE EXCLUSIONCHROMATOGRAPHY MEASUREMENTS FORCHARACTERISATION OF OLIGOLACTONEMACROMONOMERSSchoch M; Gopp U; Steurich S; Sandner BHalle,Martin-Luther-Universitat

The calibration of size exclusion chromatographymeasurements for the determination of the molecularweights of oligolactone macromonomers was carried outusing PPG and PS as standards. Results are comparedwith those obtained by end-group analysis with protonNMR14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.669429

Item 335Analytical Chemistry70, No.1, 1st Jan.1998, p.131-5USE OF MALDI-TOF TO MEASUREMOLECULAR WEIGHT DISTRIBUTIONS OFPOLYDISPERSE POLYMETHYLMETHACRYLATE

Rashidzadeh H; Baochuan GuoCleveland,State University

Using PMMA samples, some of the causes of massdiscrimination encountered in the MALDI-TOF analysisof polydisperse polymers were investigated. It was foundthat detector saturation could be a major instrumentalfactor causing mass discrimination. This was due to thestrong signals of matrix-related ions and low-massoligomer ions. The matrix effect as another source of massdiscrimination was analysed quantitatively. 34 refs.USA

Accession no.666829

Item 336Polymer39, Nos.6-7, 1998, p.1439-43TEMPERATURE MODULATED DSC STUDY OFPOLYETHYLENE TEREPHTHALATECRYSTALLIZATION. II. APPLICABILITY TONON-ISOTHERMAL PROCESSToda A; Tomita C; Hikosaka M; Saruyama YHiroshima,University; Kyoto,Institute of Technology

The non-isothermal crystallisation of PETP was examinedby temp. modulated DSC(TMDSC). A new analyticalmodel of TMDSC was applied to the process, takingaccount of the response of exothermic heat flow to temp.modulation in an apparent heat capacity of complexquantity. By examining the frequency dependence of theapparent heat capacity, the applicability was successfullyexamined for the non-isothermal process. The method wascapable of determining the temp. dependence of crystalgrowth rate from TMDSC data analysis. The results werein good agreement with the dependence determined fromliterature values of spherulite growth rate measured byoptical microscopy. 12 refs.JAPAN

Accession no.666765

Item 337Polymer Journal (Japan)29, No.11, 1997, p.910-3FRACTIONATION OF PEO STAR SAMPLES BYSUPERCRITICAL FLUIDSCansell F; Botella P; Six J-L; Garrabos Y; Tufeu R;Gnanou YCNRS

Details are given of the use of supercritical fluids for thefractionation of PEO. The fractionation of a binary mixtureof star and linear chains of PEO was studied. 25 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.666545

Item 338Polymer39, No.2, 1998, p.255-66



INVESTIGATION OF PHYSICAL AGEING INPOLYMETHYLMETHACRYLATE USINGPOSITRON ANNIHILATION, DIELECTRICRELAXATION AND DYNAMIC MECHANICALTHERMAL ANALYSISDavis W J; Pethrick R AStrathclyde,University

Physical ageing of PMMA was studied using positronannihilation lifetime spectroscopy (PALS), dielectricrelaxation spectroscopy (DRS) and dynamic mechanicalthermal analysis (DMTA) and the results obtained fromthese techniques were compared. A correlation existedbetween the free volume as measured by PALS and thechanges which occurred in the DRS and DMTA data. Itwas concluded that “thermorheologically simplicity” wasprobably an oversimplification for this system and thatphysical ageing was associated with a redistribution, notjust a shift, of molecular relaxation processes. Therelaxation distribution changed as the glass transitiontemperature was approached. The free volume distributionprobably changed during ageing, but it was not possibleto quantify these changes from the PALS study. 43 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.665913

Item 339Journal of Applied Polymer Science67, No.3, 18th Jan.1998, p.487-500SURFACE ENERGY MAPPING OF KEVLARFIBRES BY INVERSE GASCHROMATOGRAPHYRebouillat S; Donnet J B; Guo H; Wang T KDu Pont (UK) Ltd.; Ecole Nationale Superieure deChimie de Mulhouse

The surface energy characteristics of three Kevlar fibreswere systematically studied using two inverse gaschromatography (IGC) techniques, i.e. at an infinite probedilution and at a finite probe concentration, with the latterallowing a unique mapping of the surface energy levels,which complements greatly the more traditionalcharacterisation of the highest energy sites. The standardthermodynamic parameters, such as the free energy andthe adsorption enthalpy and entropy, as well as thedispersive and the specific component of the fibre surfaceenergy, were determined from the retention behaviour atzero coverage of selected molecules of various polarity.Using the second IGC approach, i.e. at finiteconcentration, the isotherms for the adsorption of n-octaneand n-hexylamine on the three selected Kevlar fibres wereconstructed by the one peak method. 29 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.665736

Item 340Journal of Applied Polymer Science

67, No.3, 18th Jan.1998, p.449-53COMPATIBILITY STUDY OFPOLYCARBONATE-POLYVINYLPYRROLIDONE BLEND USING HIGHRESOLUTION SOLID STATE NUCLEARMAGNETIC RESONANCEda Silva E P; Tavares M I BRio de Janeiro,Universidade Estadual do NorteFluminense; Rio de Janeiro,Universidade Federal

The combining NMR techniques in the solid state permitthe evaluation of the polymeric systems homogeneity. Inpolycarbonate-polyvinyl pyrrolidone blends, the responseof proton spin-lattice relaxation time in the rotating framewas the determinant to obtain information on the transitionwhen the quantity of polyvinyl pyrrolidone is close to 40wt% and a better organisation of amorphous phase wasdetected. 13 refs.BRAZIL

Accession no.665732

Item 341Applied Spectroscopy51, No.12, Dec.1997, p.1823-5INVESTIGATION OF CHEMICALINTERACTIONS AT THE STEEL/POLYMERINTERFACE BY FT-IR DIFFUSEREFLECTANCE SPECTROSCOPYBistac S; Vallat M F; Schultz JInstitut de Chimie des Surfaces et Interfaces

Interactions between a steel surface and an ethylene-vinylacetate copolymer grafted with maleic anhydride wereinvestigated by FTIR diffuse reflectance spectroscopy.The failed surfaces obtained after a mechanical separationof the polymer/steel assemblies were analysed. A two-step mechanism was proposed: the opening of theanhydride cycle by a hydrolysis reaction, leading to theformation of a carboxylic diacid, followed by the reactionof the acid with some oxidised metallic elements presentat the metal surface. This study underlines the contributionof FTIR reflectance techniques to the understanding ofadhesion mechanisms. 7 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.665698

Item 342Applied Spectroscopy51, No.12, Dec.1997, p.1784-90DEPTH PROFILING STUDY OF EFFECT OFANNEALING TEMPERATURE ON POLYMER/POLYMER INTERFACES IN LAMINATESUSING CONFOCAL RAMANMICROSPECTROSCOPYHajatdoost S; Olsthoorn M; Yarwood JSheffield,Hallam University; Utrecht,University

The effect of annealing temperature on molecularinteractions at the interface of polymer laminates was



reported. Depth profiling was carried out using confocalRaman microspectroscopy to study polyacrylonitrile/polyvinyl alcohol and polyacrylonitrile/polyacrylic acidlaminates. The laminates were annealed at 65, 75 and 90C.It was demonstrated that the degree of hydrogen bondinginteraction between the nitrile and alcohol groups nearthe interfacial region changes between laminates annealedat different temperatures. For comparison, Ramanmapping of a polyacrylonitrile-polyvinyl alcohol blendwas used to study the interactions between the polymersin this (disordered) system. 29 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; UK; WESTERN EUROPE

Accession no.665697

Item 343Applied Spectroscopy51, No.11, Nov.1997, p.1741-4CHARACTERISATION OF DENTURE ACRYLICRESIN SURFACES MODIFIED BY GLOWDISCHARGESSuzer S; Ozden N; Akaltan F; Akovali GBilkent,University; Ankara,University; MiddleEast,Technical University

Resin samples prepared by compression moulding usinga PMMA denture base material were exposed to radiofrequency glow discharges to improve the wettability ofthe material. FTIR reflectance, X-ray photoelectronspectroscopy and contact angle measurements were usedto characterise the changes introduced by the glowdischarge plasma. 18 refs.TURKEY

Accession no.665695

Item 344Applied Spectroscopy51, No.11, Nov.1997, p.1736-40GENERALISED TWO-DIMENSIONAL FOURIERTRANSFORM INFRARED PHOTOACOUSTICSPECTRAL DEPTH-PROFILING ANALYSISJiang E Y; McCarthy W J; Drapcho D L; Crocombe RABio-Rad Laboratories Inc.

A new application of generalised two-dimensionalcorrelation spectroscopy in photoacoustic depth-profilinganalysis. Both rapid-scan and step-scan photoacousticspectroscopy (obtained by using the software-baseddigital signal processing technique) of multilayer sampleswere used to calculate generalised two-dimensionalcorrelation maps. Advantages of this unambiguousanalysis method in enhancing spectral as well as depthresolutions, over conventional two-dimensionalcorrelation and other spectral depth-profiling methods,were discussed. 31 refs.USA

Accession no.665694

Item 345Applied Spectroscopy51, No.11, Nov.1997, p.1668-77RAPID-SCAN TWO-DIMENSIONAL FT-IR: ANEFFICIENT APPROACH TO DYNAMICINFRARED SPECTROSCOPYSteeman P A MDSM Research

A new and efficient mode of operation is presented thatinvolves a continuous rapid-scan FTIR spectrometer, themeasurement technique relying completely on theutilisation of the digital signal processor for dataacquisition and manipulation. Experimental andmathematical details were discussed. Application of therapid-scan technique was illustrated with some results fora styrene-acrylonitrile/butadiene copolymer. 17 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.665692

Item 346Applied Spectroscopy51, No.11, Nov.1997, p.1593-6RAMAN IMAGING OF DENTAL ADHESIVEDIFFUSIONWieliczka D M; Kruger M B; Spencer PMissouri,University

Using micro-Raman spectroscopy, chemical andmorphological information on the dentin/adhesiveinterface was collected with minimal sample preparation.Results provided direct evidence of an adhesivepreparation and demineralisation depth for two adhesivesystems. 17 refs.USA

Accession no.665691

Item 347Injection Molding5, No.12, Dec. 1997, p.44-5MATERIALS ANALYST: PART 3. LOT-TO-LOTVARIATIONSepe MDickten & Masch Mfg.Co.

The use is examined of thermogravimetric analysis as ananalytical tool for the diagnosis of part failure in injectionmoulding. The consistent performance of an ethylenevinyl acetate copolymer was evaluated and the need toseparate the component parts of the material to test forthe amount of vinyl acetate in the compound is discussedin order to develop a thermal history. Once this history isestablished, a customer can institute an incoming QC teston the material’s composition rather than by adjustingthe process for each new lot and performing producttesting after the parts have been produced.USA

Accession no.664180



Item 348Polymer Degradation and Stability57, No.3, 1997, p.313-24THERMOANALYTICAL STUDY OF THEEFFECT OF EAA AND STARCH ON THETHERMOOXIDATIVE DEGRADATION OFLDPEBikiaris D; Prinos J; Perrier C; Panayiotou CThessaloniki,University

The effect of ethylene-acrylic acid copolymer (EAA) andplasticised starch (PLST) on the thermooxidativedegradation of LDPE was examined. The course ofoxidation was followed using TGA to monitor the weightchanges during heating and DSC to study the heat changestaking place during oxidation. Three types of blend wereexamined: LDPE-plasticised starch, LDPE-EAA andLDPE-starch-EAA blends. All blends contained cobaltstearate as prooxidant. 36 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GREECE;WESTERN EUROPE

Accession no.664073

Item 349Pitture e Vernici73, No.17, 1997, p.38-43English; ItalianRELEASE OF VOLATILE DERIVATIVES FROMINITIATORS IN RADIATION CURINGVisconti M; Cattaneo M; Li Bassi GLamberti SpA

Details are given of the development of a technique forthe direct evaluation of volatile organic compounds duringthe radiation curing process. This method was used toevaluate the release of benzaldehyde from commerciallyavailable alpha-hydroxyketones during curing. 8 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.663242

Item 350Iranian Journal of Polymer Science & Technology10, No.2, Summer 1997, p.35-46PersianAPPLICATIONS OF HIGH-RESOLUTIONSOLID-STATE CARBON 13 NMRSPECTROSCOPY TO POLYMERSFarahmand F G; Morshedian JIran,Polymer Research Centre

A brief review is given of the theory and applications ofcarbon 13 NMR to polymer analysis. Mention is made ofconformational analysis, polymer reactions in solid state,analysis of crosslinked systems, homogeneity of polymericblends, analysis of surface species, and variable temperaturecarbon 13 NMR solid state spectroscopy. 37 refs.IRAN

Accession no.663219

Item 351Analytical Chemistry69, No.23, 1st Dec.1997. p.4872-7SAMPLE PRECONCENTRATION USING ION-EXCHANGE POLYMER FILM FOR LASERABLATION SAMPLING INDUCTIVELYCOUPLED PLASMA ATOMIC EMISSIONSPECTROMETRYWing Tat Chan; Yip H H GHong Kong,University

An efficient sample pretreatment/introduction techniquefor the inductively coupled plasma atomic emissionspectrometry (ICP-AES) using ion exchange for analytepreconcentration and matrix separation and laser ablationsampling for sample introduction was developed.Ammonium pyrrolidone dithiocarbamate-PS films werecoated on glass plates for analyte preconcentration. 32 refs.HONG KONG

Accession no.662915

Item 352Pigment & Resin Technology26, No.6, 1997, p.370-7FTIR SPECTROSCOPY OF LAC RESIN AND ITSDERIVATIVESSarkar P C; Shrivastava A KIndian Council of Agricultural Research; RanchiCollege

Fourier transform infrared spectroscopy was applied tothe study of lac resin, a complex natural resin of insectorigin, and some of its derivatives. The results obtainedby this method are compared with those from earlierstudies that used classical methods of chemical analysis.Experiments include the preparation of hard and softresins, dewaxed lac, ammoniated lac, lac acetal,halogenated lac, hydrolysed lac, rebuilt lac (rebulac), andthe preparation of lac metal salts. It is found that FTIRhas several advantages over classical methods, but thatFTIR data requires supplementing by other instrumentaltechniques such as FT-Raman spectroscopy and solid statenuclear magnetic resonance. 21 refs.INDIA

Accession no.662758

Item 353Journal of Vinyl and Additive Technology3, No.3, Sept.1997, p.249-55PRACTICAL GUIDE TO THE IDENTIFICATIONOF MONOMERIC PLASTICIZERS INFLEXIBLE PVC COMPOUNDSKozlowski R R; Gallagher T KAristech Chemical

The performance of a flexible PVC compound is oftendefined by its plasticiser content and composition and asimple, accurate and fast method of plasticiseridentification could, therefore, be an effective quality



control and benchmark performance test in new productdevelopment studies. Gas chromatography was shown toprovide the most effective identification method and itwas demonstrated that it could be complemented by IRspectroscopy, liquid chromatography and physicalobservations to confirm identity. 4 refs.USA

Accession no.661993

Item 354Macromolecules30, No.21, 20th Oct.1997, p.6674-6HIGH-RESOLUTION CALORIMETRY STUDYOF THE ORDER-DISORDER TRANSITION IN ADIBLOCK COPOLYMER MELTVoronov V P; Buleiko V M; Podneks V E; Hamley I W;Fairclough J P A; Ryan A J; Mai S M; Liao B X; Booth CRussian Academy of Sciences; Leeds,University;UMIST; Manchester,University

A new method is reported for locating the order-disordertransition in a diblock copolymer, namely high-resolutioncalorimetry, and the result compared with determinationsby small-angle X-ray spectroscopy and rheology. 13 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; RUSSIA; UK;WESTERN EUROPE

Accession no.658801

Item 355Polymer Science Series A39, No.8, Aug.1997, p.953-7STUDY OF SOLUBLE POLYAMIC ACIDS ANDPOLYESTER IMIDES BY METHODS OFEXCLUSION LIQUID CHROMATOGRAPHYNesterov V V; Kudrysvtsev V V; Svetlichnyi V M;Gazdina N V; Bel’nikevich N G; Kurenbin O I;Zhukova T ISt.Petersburg,Institute of Macromol.Compounds

The molecular and conformation characteristics of a seriesof polyamic acids and polyester imides, obtained by high-temp. imidisation of polyamic acids in N-methylpyrrolidinone or m-cresol, were studied byviscometry and exclusion liquid chromatography. Thedifferences in the molec.wts. of the products of polyamicacid imidisation in N-methylpyrrolidinone and m-cresolwere explained by the different characters of inactivationof the anhydride groups. 20 refs. (Full translation ofVys.Soed.A, 39, No.8, 1997, p.1387-91)RUSSIA

Accession no.658622

Item 356Macromolecules30, No.18, 8th Sept.1997, p.5285-9FURTHER APPLICATION OF A PROCEDUREFOR MOLECULAR WEIGHT ANDMOLECULAR WEIGHT DISTRIBUTION

MEASUREMENT OF POLYDISPERSEPOLYMERS FROM THEIR MATRIX-ASSISTEDLASER DESORPTION/IONISATION TIME-OF-FLIGHT MASS SPECTRAVitalini D; Mineo P; Scamporrino EIstituto per la Chimica e la Tecnol.dei Mat.Pol.;Catania,Universita

A recently reported off-line procedure to estimatemolecular weight averages and MWD index, also forpolydisperse polymers, directly from their matrix-assistedlaser desorption/ionisation time-of-flight mass spectra(MALDI-TOF) was applied to poly(bisphenol A-carbonate), a poly(ether-sulphone resin) andpoly(dimethylphenylene oxide), all having a widepolydispersity index. The molecular weight and MWDobtained values were compared with those determinedby GPC or supplied by makers. A structuralcharacterisation of these polymers was also performedby examining their MALDI-TOF mass spectra. 29 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.657168

Item 357Injection Molding5, No.10, Oct. 1997, p.60/2MATERIALS ANALYST: PART 2. BRITTLE PPOSepe MDickten & Masch Mfg.

The use is described of differential scanning spectroscopy(DSC) as an analytical tool in the diagnosis of part failure.Degradation of the polymer during processing isexamined, and the example is investigated of a 30% glassreinforced PPO which showed brittleness and for whichthe causes of failure were revealed by means of DSCanalysis.USA

Accession no.655661

Item 358Macromolecular SymposiaVol.119, July 1997, p.317-24CHEMICAL ANALYSIS OF POLYMERS USINGTRANSMISSION ELECTRON MICROSCOPY/ELECTRON ENERGY-LOSS SPECTROSCOPY:THE EXAMPLE OF POLY(ETHYLENETEREPHTHALATE)Varlot K; Martin J M; Quet C; Kihn YLyon,Ecole Centrale; CEMES-LOE

Electron energy-loss spectroscopy analysis of PETP wasperformed in the analytical TEM to evaluate thepossibility of chemical analysis of the polymer at sub-micrometre scale. Due to irradiation damage, it wasnecessary to work at the lowest possible electron dose,and with the specimen cooled to liquid nitrogentemperature. In the acquired spectra, an identification of



the different chemical bondings in agreement with X-rayabsorption near-edge spectroscopy experiments isproposed. 14 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.653745

Item 359Macromolecular SymposiaVol.119, July 1997, p.309-15CARBON-13, MAGNESIUM-25 AND BORON-11SOLID STATE NMR STUDY OF A FIRERETARDED ETHYLENE-VINYL ACETATECOPOLYMERPecoul N; Bourbigot S; Revel BEcole Nationale Superieure de Chimie de Lille; CentreCommun de Mesures RMN

Flame retardance of ethylene-vinyl acetate copolymer canbe achieved using magnesium hydroxide incorporated inthe polymeric matrix. The adduct of a small amount ofzinc borate as synergistic agent in the formulationincreases the fire-proofing properties. Multinuclei solid-state NMR appears as a means to characterise materialsbefore and after combustion. It was shown thatendothermic dehydration, water vapour evolved andformation of a glassy coating provided the flameretardancy of interest to the polymer matrix. 12 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.653744

Item 360Macromolecular SymposiaVol.119, July 1997, p.269-76QUANTITATIVE ATR-FTIR SPECTROSCOPY ATPOLYMER SURFACES: SORPTION ANDMOLECULAR CONFORMATIONMueller M; Schmitt F JDresden,Institute of Polymer Research

Adsorption and diffusion phenomena at or within polymersystems were investigated by surface sensitive ATR-FTIRspectroscopy. For a systematic description, a study wasmade of (1) the competitive adsorption and desorptionbehaviour of proteins on polymer surfaces, (2) swellingof hydrophilic polymers by water molecules, which canbe accompanied by conformational changes, and (3)induced orientational changes of hydrophobicallymodified polypeptides by apolar solvents. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;WESTERN EUROPE

Accession no.653740

Item 361Macromolecular SymposiaVol.119, July 1997, p.227-34INELASTIC NEUTRON SCATTERING STUDIES

OF POLYETHYLENE AND N-ALKANESParker S FRutherford Appleton Laboratory

High quality inelastic neutron scattering (INS) spectra ofrandomly oriented polycrystalline PE, polydeutero-polyethylene and highly oriented polyethylene arepresented and a number of new features described. 9 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.653736

Item 362Macromolecular SymposiaVol.119, July 1997, p.157-64INFRARED ABSORPTION SPECTRA OFPOLYMERS FROM CLASSICAL MOLECULARSIMULATIONSoldera A; Dognon J PCEA/Le Ripault

A method is proposed to predict the IR spectra ofamorphous polymers. Based on classical molecularsimulation and Kramers-Kronig relations, it allows thecomputations of absorption and transmittance spectra ofpolymer films in near and middle infra-red domains withgood agreement with experimental data. 22 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; FRANCE;WESTERN EUROPE

Accession no.653730

Item 363Macromolecular SymposiaVol.119, July 1997, p.79-87CREEP RATE SPECTROSCOPY USING A LASERINTERFEROMETER AS ULTRA-HIGHRESOLUTION TECHNIQUE FOR STUDY OFRELAXATIONSPeschanskaya N N; Yakushev P N; Sinani A B;Bershtein V ARussian Academy of Sciences

An original laser interferometry creep rate spectroscopy(CRS) method was developed and used as the low-frequency and high-resolution technique for studyingmicroplasticity and relaxations in different materialsincluding brittle ones. New possibilities for CRS forpolymers are demonstrated. 13 refs.RUSSIA

Accession no.653722

Item 364Macromolecular SymposiaVol.119, July 1997, p.49-63POTENTIAL OF TWO-DIMENSIONAL NEAR-INFRARED CORRELATION SPECTROSCOPYIN STUDIES OF PRE-MELTING BEHAVIOUR OFNYLON 12



Ozaki Y; Yongliang Liu; Noda IKwansei-Gakuin,University; Procter & Gamble Co.

This review paper discusses the potential of generalisedtwo-dimensional near-infrared correlation spectroscopyin studies of pre-melting behaviour and hydrogen bondsof nylon 12. A study on dissociation and hydrogen bondsof N-methylacetamide is also reviewed as a modelcompound study of nylon 12. FTIR spectra were measuredover a temperature range of 30-150C where gradualweakening of inter- or intramolecular associativeinteractions and decrease of local order leading to theeventual fusion of nylon 12 crystals are observed. 24 refs.JAPAN; USA

Accession no.653720

Item 365Macromolecular SymposiaVol.119, July 1997, p.25-48UNDERSTANDING POLYMERS BYVIBRATIONAL SPECTROSCOPY: SOMERECENT ADVANCES IN THEORY ANDEXPERIMENTMeier R JDSM Research

A rapid scan version of two-dimensional spectroscopy isintroduced and applied to study the phases of anacrylonitrile-butadiene-styrene polymer system. Somerecent advances in the application of computationalchemistry to the evaluation of vibrational spectra arepresented. Some specific applications are discussed. 31 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;NETHERLANDS; WESTERN EUROPE

Accession no.653719

Item 366International Journal of Polymer Analysis andCharacterization3, No.4, 1997, p.369-79HPLC QUANTIFICATION OF THIOETHERANTIOXIDANTS IN POLYETHYLENE AFTERDISSOLUTION OF POLYMER UNDERPRESSURE IN ALIPHATIC SOLVENTMacko T; Furtner B; Lederer KLeoben,Montan-Universitat

A new method is described for the quantitativedetermination of some sulphur-containing antioxidants inPE. The polymer matrix is dissolved in hot n-heptane/isopropyl alcohol, 97/3 v/v at 160 deg.C under elevatedpressure (0.33 MPa) and precipitated by cooling. Thesolution is injected directly into a normal-phase silica gelcolumn flushed with the same solvent as used for thedissolution of the polymer. This method gives high recoveryof the antioxidants, good repeatability of the analysis anda low detection limit of 0.011 mg 4,4'-thiobis(3-methyl-6-tert-butylphenol) (Santonox R) /1 g PE; 0.074 mgditetradecyl-beta,beta’-thiodipropionate (Chimox 14) / 1

g PE; and 0.125 mg dioctadecyl-beta,beta’-thiodipropionate(Irganox PS 802) /1 g PE. 23 refs.AUSTRIA; WESTERN EUROPE

Accession no.653220

Item 367Macromolecular SymposiaVol.118, June 1997, p.383-8FREE VOLUME STUDIES IN MISCIBLEPOLYMER BLEND SYSTEMSCampbell J A; Goodwin A A; Ardi M S; Simon G P;Landry-Coltrain C J TMonash,University; Eastman Kodak Co.

A brief review is presented of the published literaturerelating to the use of positron annihilation lifetimespectroscopy in studying the effects of miscibility on thefree volume of miscible, amorphous polymer blends.Studies of a fully miscible polyvinyl phenol/PVAC blend,a partially miscible polyphenyl methacrylate/polycarbonate blend and a largely immiscible PS/PVACblend are reported. The results indicate that miscibleblends tend to show a negative deviation of free volumesize, and to a lesser degree free volume fraction, on mixingdue to the intimacy of packing of the blend componentmacromolecules. The largely immiscible blend showspositive deviation of free volume size which is ascribedto additional free volume at the interface. 13 refs.AUSTRALIA; USA

Accession no.652994

Item 368Journal of Polymer Science : Polymer ChemistryEdition35, No.12, 15th Sept.1997, p.2431-9ESR STUDY ON CHEMICAL CROSSLINKINGREACTION MECHANISMS OF PE USING ACHEMICAL AGENT. II. EFFECT OF PHENOLICANTIOXIDANTSYamazaki T; Seguchi THitachi Cable Ltd.; Japan,Atomic Energy ResearchInstitute

The effect of antioxidant on the reaction mechanism ofchemical crosslinking of PE with dicumyl peroxide at hightemperatures was investigated by ESR. The antioxidantreacted with the alkyl radicals in PE formed by the thermaldecomposition of dicumyl peroxide above 120C anddisturbed the crosslinking. 10 refs.JAPAN

Accession no.652659

Item 369Applied Spectroscopy51, No.8, Aug.1997, p.1176-8QUANTITATION OF POLYETHYLENE GLYCOLCONCENTRATION USING RAMAN



SPECTROSCOPYMelendez Y; Schrum K F; Ben-Amotz DPurdue,University; Maryville College

Raman spectroscopy is used to quantitate the amount ofpolymer in solution, in particular polyethylene glycoldissolved in chloroform. For various chain lengths andpolymer weight fraction ranges, it is shown that the ratiosof peak intensifies in the C-H stretching region may beused to quantitate polymer weight fraction with about 1%uncertainty. For low polymer weight fraction ranges (0-10%), the relationship between Raman intensity andpolymer weight fraction is essentially linear, while athigher ranges (0-50%) the intensity follows a nonlinearfunction derived from basic concentration relationshipsand indicates a universal scaling with polymer chainlength. 10 refs.USA

Accession no.652414

Item 370Polymer38, No.17, 1997, p.4381-5SEPARATION AND IDENTIFICATION OFETHYLENE-PROPYLENE BLOCKCOPOLYMERJunting Xu; Linxian Feng; Shilin Yang; Yinan Wu;Yiqing Yang; Xiangming KongZhejiang,University; Shanghai,Research Institute ofPetrochemical Technology

A commercial impact resistant PP alloy was fractionatedusing the temperature rising elution fractionationtechnique and several ethylene-propylene blockcopolymers with different ethylene contents wereobtained. The block structure of the fractions wasidentified by combining the fractionation results withcarbon-13 NMR spectroscopy and DSC results. Sometransition segments were found between PE and PPsegments in the block copolymers. With increasing elutiontemperature, the number and kind of transition segmentsdecreased, together with the length and meltingtemperature of the PE segment in the block copolymerfractions. 18 refs.CHINA

Accession no.651909

Item 371Analyst122, No.8, Aug.1997, p.777-81DETERMINATION OF FINISHING OILS INACRYLIC FIBRES BY NEAR-INFRAREDREFLECTANCE SPECTROMETRYBlanco M; Coello J; Fraga J M G; Iturriaga H;Maspoch S; Pages JBarcelona,Universidad Autonoma

The potential of near-infrared diffuse reflectancespectrometry for quality control analyses in the textile

industry is explored with a view to the quantification offinishing oils in acrylic fibres by partial least-squaresregression, using a rotary cuvette system for recordingspectra. Calibration is performed with a set of samplesthat encompasses every source of variability, and thewavelength region where absorption is mostly due to theoil is used to construct several models from which thatleading to the minimum relative standard error for asample test set is selected. The results provided by variousmathematical treatments used to minimise scatteringresulting from the differential linear density of the samplesreveal no significant differences between predictionerrors. The model is used to quantify levels of finishingoil in routinely manufactured samples for a period of sixmonths, during which time two batches show poorpredictions due to a new component appearing in theproduct. Modification of the calibration model to accountfor this component substantially increases robustness andallows the accurate quantification of all batchesmanufactured after the model is developed. 28 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.651451

Item 372Analyst122, No.9, Sept.1997, p.101R-15RANALYTICAL EXTRACTION OF ADDITIVESFROM POLYMERSVandenberg H J; Clifford A A; Bartle K D; Carroll J;Newton I; Garden L M; Dean J R; Costley C TLeeds,University; ICI; Newcastle,University ofNorthumbria

Plastics contain many other small molecules as well asthe polymer itself. These include additives to alter thepolymer properties or prolong the life of the polymer,such as plasticisers, antioxidants and UV light absorbers.There may also be processing aids, residual monomers,low molecular weight oligomers and inadvertentcontaminants present. It is important for the manufacturerand regulators to know the level of these materials in thepolymer to ensure the product is fit for its intendedpurpose. Food contact plastics are regulated by maximumconcentrations allowable in the plastic, which applies toresidual monomers and processing aids as well asadditives. There are some methods for determiningconcentrations of additives without extraction from thepolymer, such as nuclear magnetic resonancespectrometry, UV spectrometry and UV desorption-massspectrometry. However, in order to determine the levelsin the polymer, it is usually necessary to extract thecompounds quantitatively from the plastic before analysis.A review is presented of the available extractiontechniques. 102 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.651430



Item 373Analytical Chemistry69, No.16, 15th Aug.1997, p.3304-13QUANTITATIVE ANALYSIS OF PESTICIDES INPOST-CONSUMER RECYCLED PLASTICSUSING OFF-LINE SUPERCRITICAL FLUIDEXTRACTION(SFE)/GASCHROMATOGRAPHY-ECDNerin C; Batlle R; Cacho JZaragoza,University

The SFE of several organochlorine and organophosphoruspesticides and two metabolites from recycled plastics wasstudied. The recycled plastics, used as agricultural soil covers,were a mixture of LDPE and EVA. The SFE was optimisedand compared with the classical sonication and totaldissolution extraction methods. The plastic was extractedwith supercritical carbon dioxide under different extractionconditions, depending on the physical matrix characteristics.Average recoveries of the eleven chemicals studied rangedfrom values greater than 90% with an overall relativestandard deviation of 4.3% for plastics films to values lowerthan 40% with an overall standard deviation of 7.2% forplastics pellets. The variables affecting the whole extractionprocess and the results obtained in the comparison betweenthe three extraction methods are discussed. 45 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.650545

Item 374European Polymer Journal33, No.7, July 1997, p.1135-42FOURIER TRANSFORM INFRAREDSPECTROSCOPY APPLIED TO THE STUDY OFPVC DECOMPOSITIONBeltran M; Marcilla AAlicante,Universidad

The process of PVC decomposition was studied by FTIRunder dynamic conditions. The IR spectra were directlyobtained from PVC films pyrolysed in-situ in a speciallydesigned infra red cell. A qualitative description of thechanges observed in the spectra was presented. 35 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; SPAIN;WESTERN EUROPE

Accession no.650382

Item 375Macromolecular SymposiaVol.118, June 1997, p.261-5HIGH PERFORMANCE LIQUIDCHROMATOGRAPHY CHARACTERIZATIONOF MACROMOLECULESChang T; Lee H C; Lee WPohang,University of Science & Technology

A new chromatographic method for polymer molecularweight characterisation, temperature gradient interaction

chromatography, is described. Fine and reproduciblecontrol of interaction between polymer chains and thealkyl chain bonded silica packing material can be achievedby varying the column temperature. The method can beused to characterise binary polymer mixtures, where onecomponent is separated by the size exclusion mechanismand the other is simultaneously separated by theinteraction mechanism in a single isocratic elution. Theapplication of this technique to the characterisation of PSand PS/PMMA mixtures is examined. 12 refs.KOREA

Accession no.649987

Item 376Macromolecules30, No.13, 30th June 1997, p.3781-7CHARACTERISATION OF POLYESTERS BYMATRIX-ASSISTED LASER DESORPTIONIONISATION MASS SPECTROMETRYWilliams J B; Gusev A I; Hercules D MPittsburgh,University

A series of aliphatic polyesters, characterised byasymmetric oligomer distributions, heteroterminated linearchains, and cyclic oligomers, were studied using MALDI.Structural characterisation results were compared withthose from fast atom bombardment mass spectrometry,electrospray ionisation mass spectrometry, NMR and end-group titration. MALDI molecular weight determinationwas contrasted with those from GPC and NMR. 23 refs.USA

Accession no.649761

Item 377Shawbury, Rapra Technology Ltd., 1997, pp.120. 12ins. 15/4/97. Rapra Review Rept. No.95, vol.8, No. 111997,THERMAL ANALYSIS OF POLYMERSSepe M PDickten & Masch Mfg.Co.Edited by: Dolbey R(Rapra Technology Ltd.)Rapra Review Report No.95

A review is presented of the techniques involved in thethermal analysis of polymers. Techniques discussedinclude differential scanning calorimetry, differentialphotocalorimetry, thermogravimetric analysis,thermomechanical analysis, dynamic mechanical analysis,dielectric, thermally stimulated current/relaxation mapanalysis analysis, and thermal conductivity analysis. 381refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.647258

Item 378Journal of Applied Polymer Science65, No.3, 18th July 1997, p.595-600



MOLECULAR WEIGHT OF POLYETHYLENEGLYCOLS BY VAPOR PRESSUREOSMOMETRY: AN ALTERNATIVE DATATREATMENTSabadini E; Assano E M; Atvars T D ZCampinas,Universidade Estadual

The number-average molec.wt. of some polyethyleneglycols was analysed using vapour pressure osmometry.This technique generally worked with a plot of thedifference in electrical resistance/concentration versusconcentration and the molec.wt. was determined by thecalibration constant obtained from the curve intercept. Itwas demonstrated that this method induced a highdispersion of the data, which could be minimised using aplot of difference in electrical resistance versusconcentration.. More precise values of molec.wt. couldthus be obtained and the number-average molec.wt. ofseveral polyethylene glycols could be directly obtainedfrom the ratio between the curve slopes obtained for astandard and the polymer sample. 10 refs.BRAZIL

Accession no.645677

Item 379Speciality Chemicals17, No.5, June/July 1997, p.165/70MAKING LIQUID CHROMATOGRAPHY MOREACCESSIBLEKuehler T C; Sellen M; Lavold T; Batt J; Langridge J;Raso R; Rontree J AAstra Hassle AB; Micromass AB; Micromass UK Ltd.

Until recently, mass spectrometry was regarded as a highlysophisticated technique requiring careful use of theinstrument by a sole operator, and demanding meticuloussample preparation by the chemist. However, movestowards open-access, chemist-operated systems have beenreported on mass spectrometers equipped with a varietyof ionisation modes. The reliability and robustness ofatmospheric pressure ionisation, the ease and speed ofsource tuning, the fact that it is unnecessary to optimisethe source conditions for each sample individually andthe reproducibility of results have made API techniquesthe ionisation methods of choice. Details are given. 5 refs.EUROPEAN COMMUNITY; EUROPEAN UNION;SCANDINAVIA; SWEDEN; UK; WESTERN EUROPE

Accession no.645281

Item 380Polymer Degradation and Stability57, No.2, 1997, p.135-49THERMAL DEGRADATION KINETICS OFPOLYPROPYLENE. III.THERMOGRAVIMETRIC ANALYSISChan J H; Balke S TToronto,University

Thermogravimetric data were obtained for the pyrolysisof polypropylene, and several previously published

interpretation methods were applied to the data. The widetemperature range used in this work (45-580C)encompassed a change in the decomposition mechanismand this greatly limited the utility of the methods. Toaccommodate this mechanism change, the data weretreated as a pseudo-first order reaction. The loweractivation energy occurring at lower degradationtemperatures was attributed to scission of the ‘weak links’in the polymer. The higher activation energy was similarto the carbon-carbon dissociation energy and wasassociated with random scission throughout the polymer.47 refs.CANADA

Accession no.645116

Item 381Polymer Degradation and Stability57, No.2, 1997, p.113-25THERMAL DEGRADATION KINETICS OFPOLYPROPYLENE. I. MOLECULAR WEIGHTDISTRIBUTIONChan J H; Balke S TToronto,University

A kinetic model for the thermal degradation of PP wasdeveloped and fitted to MWD data obtained by hightemperature size exclusion chromatography. In a seriesof ampoule experiments, reaction temperatures of 275-315C were examined with reaction times of up to 48 h. Asingle-parameter version of the model, containing anapparent rate constant, was found to provide excellentfits of all MWDs. Values of the parameter varied withboth temperature and reaction time. 35 refs.CANADA

Accession no.645114

Item 382Analytical Chemistry69, No.13, 1st July 1997, p.2485-95MASS SPECTROMETRIC INVERSE GASCHROMATOGRAPHY: INVESTIGATION OFPOLYMERIC PHASE TRANSITIONSPanda S; Bu Q; Huang B; Edwards R R; Liao Q; Yun KS; Parcher J FMississippi,University

An improved inverse gas chromatographic methodinvolving the use of a mass-specific detector fordetermination of the Tg of polymeric materials isdescribed. This new method allows the use of severalprobe solutes simultaneously with an automated, closed-loop injector and stepped temperature programming. Theresult is a single continuous chromatogram for each probesolute over a range of temperatures encompassing the Tg.Several different methods for the exact determination ofTg from the chromatogram were investigated. Two newmethods were also proposed for the evaluation of Tg fromeither the temperature dependence of the second moments



of the elution peaks for probe solutes or simple inspectionof the variation of elution peak height (width) withtemperature. 51 refs.USA

Accession no.645093

Item 383Analytical Chemistry69, No.12, 15th June 1997, p.15R-28RCOATINGSAnderson D GWitco Corp.

A review is presented of analytical techniques applicableto the examination of coatings, raw materials andsubstrates since 1995. The most highly referenced areaswere found to be IR spectroscopy, NMR, HPLC, thermalanalysis and gas chromatography. 704 refs.USA

Accession no.640310

Item 384Polymer Bulletin38, No.6, June 1997, p.681-8SEPARATION OF BLOCK COPOLYMERS FROMPARENT HOMOPOLYMERS BY MEANS OFLIQUID CHROMATOGRAPHY AT THECRITICAL ADSORPTION POINTJanco M; Berek D; Onen A; Fischer C H; Yagci Y;Schnabel WSlovak Academy of Sciences; Istanbul,TechnicalUniversity; Hahn-Meitner-Institut Berlin GmbH

The principle underlying the above method is describedand results of its application to block copolymersconsisting of methyl methacrylate and tetrahydrofuranblocks are presented and discussed. The technique isshown to be suitable for characterisation of blockcopolymers with regard to the presence of homopolymerand multiblock (triblock) fractions. 5 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; GERMANY;SLOVAK REPUBLIC; SLOVAKIA; TURKEY; WESTERNEUROPE

Accession no.640169

Item 385Antec 97. Volume III. Conference proceedings.Toronto,27th April-2nd May 1997,p.3588-92. 012FOURIER TRANSFORM INFRARED MICROSPECTROSCOPY MAPPING. APPLICATIONSTO VINYL SIDING INDUSTRYGarcia D; Black JElf Atochem North America Inc.(SPE)

Fourier transform IR (FTIR) spectroscopy is a powerfulanalytical technique capable of yielding high qualityinformation with a spacial resolution as low as 10 microns.

When coupled with an automated mapping stage, it canoffer unique evaluation capabilities. A number ofapplications of FTIR spectroscopy mapping to the vinylsiding industry are described. Examples focus ondetermining, in single sample mapping experiments, thecompositional changes associated with capstock tosubstrate transition and evaluating the degradation speciesand level observed during weathering exposurethroughout the thickness of the siding panel. 4 refs.USA

Accession no.639927

Item 386Antec 97. Volume II. Conference proceedings.Toronto, 27th April-2nd May 1997, p.2310-4. 012QUANTITATIVE ANALYSIS OF LDPE/LLDPEBLEND USING DSC AND FTIR METHODSPrasad A; Mowery DQuantum Chemical Co.(SPE)

A blend of LDPE and LLDPE is widely used for blownfilm applications. For quality control an accurate and rapidmethod is required to identify the type and compositionof alpha-olefin in an LDPE/LLDPE blend. A rapid,accurate and new test method is developed which utilisesDSC and FTIR techniques. The melting point of LDPEvaries with density and usually is in the range of 106 deg.Cto 112 deg.C for film grade resins. The DSC thermogramof LLDPE is characterised by a broad range of meltingwith a lower melting peak around 106 deg.C to 110 deg.Cand a higher one in the range of 120 deg.C to 124 deg.C.In the blend with LDPE, the ratio of the two endothermicpeak heights changes. At a given weight percent of LDPE,this ratio depends on the type of LLDPE. The separatecalibrations for butene-1, hexene-1, and octene-1 LLDPEsare developed to quantify the blend composition fromDSC thermograms provided the alpha-olefin type isidentified by a rapid method such as FTIR. 17 refs.USA

Accession no.638387

Item 387Shawbury, Rapra Technology Ltd., 1992, pp.112. 12ins.30/6/97. Rapra Review Rept. No.61, Vol.6, No.1, 1992.FOOD CONTACT POLYMERIC MATERIALSSidwell JRapra Technology Ltd.Edited by: Dolbey R(Rapra Technology Ltd.)Rapra Review Report No.61

A review is presented of the current and proposedEuropean legislation on materials in contact with food,as well as the latest technological advances. Withreference to legislation, details are given of EC directivesissued, their implementation, FDA regulations, recyclingand waste management legislation. Technical



developments in food contact materials cover barrierpolymers in multilayer packaging films, migration ofspecies from food contact materials, and methods ofanalysis of multilayer food contact materials. 485 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.637749

Item 388Polymer38, No.12, 1997, p.3035-43CHARACTERIZATION OF POLYETHYLENETEREPHTHALATE AND POLYETHYLENETEREPHTHALATE BLENDSFox B; Moad G; van Diepen G; Willing I; Cook W DCSIRO,Div.of Chemicals & Polymers;Monash,University

A method was developed for direct determination of themolec.wt. of the PETP component in PETP/ABS blendsby GPC. The technique was used to demonstrate that anobserved deterioration in the mechanical properties, e.g.Izod impact strength, of PETP/ABS blends on processingcould be correlated with a decrease in the molec.wt. ofthe PETP component. Various methods for evaluating themolec.wt. and the chemical microstructure of PETP wereexamined. The use of NMR spectroscopy as a means ofquantitatively identifying end groups and comonomersthat were present at the 1-4% level in commercial PETPwas critically evaluated with reference to the stability ofPETP and PETP end groups in various NMR solvents.New proton NMR chemical shift assignments forcyclohexanedimethanol units are presented and thereactivity of hydroxy end groups in trifluoroacetic acidmixtures is examined. 34 refs.AUSTRALIA

Accession no.636573

Item 389Polymer Testing16, No.2, 1997, p.193-8NMR CARBON-13 HIGH RESOLUTION STUDYOF POLY(ETHYLENE-CO-VINYL ACETATE)Stael G C; Tavares M I BCCT/UENF

EVA was analysed by carbon-13 high-resolution usingNMR employing solution and solid state techniques. Theanalyses of this copolymer by solution NMR permittedthe copolymer composition to be obtained, and usingsolid-state NMR, a study of molecular mobility wascarried out. Both studies were made to correlate thestructure and properties. 9 refs.BRAZIL

Accession no.634101

Item 390Trends in Polymer Science

5, No.3, March 1997, p.97-102CHARACTERISATION OF POLYMER BLENDSBY INVERSE GAS CHROMATOGRAPHYAl-Saigh Z YOhio,State University

A brief review is presented of the use of inverse gaschromatography to characterise polymer blends.Comparisons between data from inverse gaschromatography and DSC are discussed. 23 refs.USA

Accession no.632110

Item 391Polymer News22, No.1, Jan.1997, p.15POLYMER ANALYSIS ANDCHARACTERISATION. SOLID STATE NMR: ISIT BECOME TRULY POPULAR?Garbassi FEniChem SpA

A very brief review is presented of specific areas wheresolid state NMR can contribute to polymer analysis.Mention is made of polymer morphology, interactions,dynamics and polymer reactions. 10 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; ITALY;WESTERN EUROPE

Accession no.632071

Item 392Analytical Chemistry69, No.4, 15th Feb.1997, p.618-22COMPOSITION AND MICROSTRUCTUREANALYSIS OF CHLORINATEDPOLYETHYLENE BY PYROLYSIS GASCHROMATOGRAPHY AND PYROLYSIS GASCHROMATOGRAPHY/MASS SPECTROMETRYCheng-Yu Wang F; Smith P BDow Chemical Co.

A pyrolysis gas chromatography method was developedto determine the composition and microstructure ofchlorinated PE (CPE). The method used specific aromaticcompounds which were formed throughdehydrochlorination of trimers after pyrolysis of CPEpolymers at elevated temperatures. The composition andmicrostructure calculation was based on the differencebetween the levels of ethylene and vinyl chloride trimersformed. The composition of CPE polymers used in thisstudy was corroborated with carbon-13 NMR results andthe manufacturers product specification. 23 refs.USA

Accession no.629089

Item 393Biomaterials18, No.5, March 1997, p.415-9



DETECTION OF PEROXY SPECIES IN ULTRA-HIGH MOLECULAR WEIGHTPOLYETHYLENE BY RAMAN SPECTROSCOPYChenery D HSmith & Nephew Group Research Centre

Samples of gamma-sterilised UHMWPE were examinedusing infra-red and Raman spectroscopies. The purposeof this study was to detect the peroxy intermediates bythe novel use of Raman spectroscopy to confirm thatoxidation proceeded by this mechanism. 16 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.625483

Item 394Polymer38, No.1, 1997, p.1-7MODULATED DIFFERENTIAL SCANNINGCALORIMETRY: 6. THERMALCHARACTERISATION OF MULTICOMPONENTPOLYMERS AND INTERFACESHourston D J; Song M; Hammiche A; Pollock H M;Reading MLoughborough,University of Technology;Lancaster,University; ICI Paints

A quantitative thermal method, based on the differentialof heat capacity signal from modulated temperaturedifferential scanning calorimetry, was described fordetermining the weight fraction of interface and the extentof phase separation in polymer materials. The interfacewas modelled as discrete fractions, each with its owncharacteristic increment of heat capacity. The materialsused to demonstrate the range of the method were PSblended with poly(phenylene oxide) (PPO), pure PS, purePPO, a styrene-isoprene-styrene triblock copolymer (SIS),SIS blended with PPO, PMMA/poly(vinyl acetate) blendsand PVC sandwiched with poly(n-butyl acrylate). Two-phase and four-phase systems were used. The calculatedresults agreed well with experimental results for two- andfour-phase systems. 20 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.621625

Item 395Analytical Chemistry69, No.1, 1st Jan.1997, p.66-71LIQUID CHROMATOGRAPHY AT THECRITICAL CONDITION USING ENHANCED-FLUIDITY LIQUID MOBILE PHASESSouvignet I; Olesik S VOhio,State University

The use of enhanced-fluidity liquid mixtures of THF andcarbon dioxide for liquid chromatography at the criticalcondition was examined. For PS polymers, the molec.wt.range that could be analysed at the critical condition was

compared for THF/carbon dioxide and other common liquidmixtures. As enhanced-fluid liquids were highlycompressible, it was possible to reach the critical conditionby changing the pressure of the THF/carbon dioxidemixture. Approaching the critical condition by pressurevariation was compared with that possible with temp.changes. Pressure variation was a more accurate andreproducible means of reaching the critical condition thantemp. variation. Finally, THF/carbon dioxide mixtures wereused as mobile phases at the critical condition for PS tocharacterise styrene-methyl acrylate copolymers. 25 refs.USA

Accession no.620015

Item 396Shawbury, Rapra Technology Ltd., 1995, pp.108. 12ins.18/7/95. Rapra Review Rept. Vol.7, No.11, 1995,MOLECULAR WEIGHT CHARACTERISATIONOF SYNTHETIC POLYMERSHolding S R; Meeham ERapra Technology Ltd.; Polymer Laboratories Ltd.Edited by: Dolbey R(Rapra Technology Ltd.)Rapra Review Report No. 83

Techniques are examined for the determination of themolecular weight distribution and molecular weight averagesof synthetic polymers. The use is discussed of gel permeationchromatography in combination with other techniques suchas light scattering and viscometry to provide informationabout the molec.wt. of a polymer and potentially significantinformation on the composition of copolymers and blends.The use of solution viscosity is also examined as a valuablequality control technique. 411 refs.EUROPEAN COMMUNITY; EUROPEAN UNION; UK;WESTERN EUROPE

Accession no.556661

Item 397Analytical Chemistry60,No.9,1st May 1988,p.932-7IDENTIFICATION OF DYES IN SOLIDPOLYMETHYL METHACRYLATE BY MEANSOF LASER DESORPTION FOURIERTRANSFORM ION CYCLOTRON RESONANCEMASS SPECTROMETRYHsu A T;Marshall A GOHIO STATE,UNIVERSITY

It is demonstrated that the above technique can detect andidentify (by chemical formulae) dyes in solid PMMAcommercial plastics at concentrations at least on order ofmagnitude lower (0.1% vs 1-2wt%) than those obtainedby the best currently-available alternative method (ATRFourier transform IR spectrometry). Both untreated andredissolved PMMA can be characterised, in the presenceand absence of up to three dyes in a single sample. 44 refs.USA

Accession no.357996



Item 398Oxford, Pergamon Press Ltd., 1984, pp.ix,445.LS.24.50. 9ins. 2copies. 12/7/85. Analytical ChemistryVol.8. 91TANALYSIS OF PLASTICSCrompton T R

This book covers all aspects of the analysis of plastics bychemical and physical methods. It is divided into eightchapters which each deal with a particular polymer orgroup of polymers:- polyolefins, polypropylene, higheralkene polymers, styrene polymers, chlorine-containingpolymers, methacrylates, polybutadienes, polyesters andpolyethers. The techniques discussed includespectroscopy, chromatography, fractionation,, X-raydiffraction, autoradiography, DTA, TGA and DSC.UK

Accession no.280400

Item 399Weinheim, Verlag Chemie GmbH, 1981, pp.XV,687.12ins. 22/3/82. R.ROOM. 91TATLAS OF POLYMER AND PLASTICSANALYSIS. VOL.3....ADDITIVES ANDPROCESSING AIDS: SPECTRA AND METHODSOF IDENTIFICATION. 2ND REV.EDN.Scholl F

The spectroscopic and chromatographic data that arerequired for the identification of plastics additives and

processing aids are presented. Over 1300 IR spectra and60 UV spectra are included. The functions andcompositions as well as the physical and chemicalmethods of identification of the following materials arediscussed: plasticisers, fillers, pigments, antioxidants, UVstabilisers, optical brighteners, antistatic agents,biostabilisers, flame retardants, lubricants, accelerators,hardeners and blowing agents. 608 refs.

Accession no.211056

Item 400Members Rept.49 Shawbury, 1980, pp.12. 12ins.2copies. 26/6/80. 91THIGH PERFORMANCE LIQUIDCHROMATOGRAPHY - ANALYTICALAPPLICATIONS IN THE RUBBER ANDPLASTICS INDUSTRIESSidwell J ARubber & Plastics Research Assn.of Gt.BritainRUBBER & PLASTICS RA.MEMBERS REPT.049

This report details some of the high-performance liquidchromatography work carried out at RAPRA and reviewsreported in the literature. 11 refs.

RUBBER & PLASTICS RESEARCH ASSN.OFGT.BRITAINAccession no.154074

Subject Index


Subject Index

AABS, 160 164 207 225 345 365 388

398ABSORPTION, 56 226 297 306 374

382ABSORPTION SPECTRA, 274ABSORPTION SPECTROSCOPY,

358 362ACCELERATOR, 399ACCURACY, 131ACETIC ACID, 76 266ACETONE, 185 224 266 311ACETONITRILE, 21 266ACID, 277 288ACOUSTIC MICROSCOPY, 126ACRYLATE, 269ACRYLIC, 199ACRYLIC ACID COPOLYMER,

172 217 348ACRYLIC POLYMER, 33 172 255

299 314 335 371 384 397ACRYLIC-MELAMINE RESIN, 44

175ACRYLONITRILE, 119ACRYLONITRILE COPOLYMER,

57ACRYLONITRILE-STYRENE

COPOLYMER, 72 110 220 345ACTIVATION ENERGIES, 49 75

146 169 280 288 317 328 380381

ADDITIVE, 29 36 71 89 99 107 108112 124 128 132 151 161 171178 181 199 201 206 225 226250 272 288 289 302 306 318324 325 353 366 372 377 387391 397 399

ADHESION, 32 61 62 145 157 167176 202 223 231 236 237 247249 312 316 341 346

ADHESIVE, 9 20 62 167 168 179272 346

ADSORPTION, 46 56 65 93 103178 203 210 221 241 285 319339 360 384

ADSORPTIONCHROMATOGRAPHY, 105 210

AEROPLANE, 36 62 121AFFINITY CHROMATOGRAPHY,

50 97AGEING, 66 80 86 88 112 148 152

274 288 298 309 338 377ALCOHOL, 56 235 288ALCOHOLYSIS, 39

ALKYD RESIN, 237ALPHA TRANSITION, 245 290

328ALUMINIUM, 126 168 179 223 266ALUMINIUM HYDROXIDE, 211ALUMINIUM OXIDE, 6AMINE, 36 48 130 151 161 178 272AMMONIUM PYRROLIDONE

DITHIOCARBAMATE, 351AMMONIUM SALT, 258AMORPHOUS, 14 54 74 78 99 117

141 170 207 213 274 283 340362 367

ANISOTROPY, 13 256 324ANNEALING, 24 54 74 101 135

136 277 308 338 342ANTI-STICK AGENT, 6ANTIMONY, 95ANTIOXIDANT, 65 86 93 107 132

171 183 195 286 288 366 368372 387 399

ANTISTATIC AGENT, 399AQUEOUS, 46 198 223 232ARAMID FIBRE, 281AROMA, 56 57AROMATIC, 48 125 192 278 288

299 392ATMOSPHERIC PRESSURE, 50

206 222ATOMIC ABSORPTION

SPECTROSCOPY, 177ATOMIC EMISSION

SPECTROSCOPY, 95 177 218273 351

ATOMIC FORCE MICROSCOPY,30 38 44 58 59 62 108 115 118142 145 154 167 179 191 219277

ATTENUATED TOTALREFLECTANCESPECTROSCOPY, 43 61 69 126257 262 301 360

AUGER ELECTRONSPECTROSCOPY, 13

AUTOMATION, 46 50 212 278 382AUTOMOTIVE APPLICATION, 44

56 62 67 175 202 212 236 329AUTOOXIDATION, 169

BBACKSCATTERED ELECTRON

IMAGING, 289BAG, 266BAGASSE, 100

BAND STRUCTURE, 262BARIUM SULPHATE, 40BARRIER PROPERTIES, 56 57 86

94 168 387BENZENE, 382BETA RELAXATION, 325BIAXIALLY ORIENTED, 104BIOCOMPATIBLE, 42BIODEGRADABLE, 37 112 267

387BIODETERIORATION, 5 37 112

246 267 387BIOMATERIAL, 42 46 246 262BIOMEDICAL APPLICATION,

262BIREFRINGENCE, 257 284BISPENTAMETHYLPIPERIDYL

SEBACATE, 66BISPHENOL A, 200 222 272 356BISPHENOL A COPOLYMER,

189BISPHENOL A DIGLYCIDYL

ETHER, 178BISPHENOL A EPOXY RESIN,

11BISPHENOL A

POLYCARBONATE, 4 29 78135 159 322 367

BISPHENOL DIGLYCIDYLETHER, 178

BLEND, 11 12 15 25 47 58 60 6364 69 72 77 91 98 107 110 112125 137 139 146 147 151 156186 188 193 209 213 220 228234 246 309 331 340 347 348363 367 375 377 386 388 390391 394

BLOCK COPOLYMER, 127 193274 354 370 384 394

BLOW MOULDING, 313 323BLOWING AGENT, 302 399BLOWN FILM, 324 386BODY ARMOUR, 281BOILING POINT, 120 185 266BONDING, 32 168 202BONDING AGENT, 168 179BONNET, 329BOTTLE, 57 131 212 266 313 323BOUND WATER, 51BOUNDARY LAYER, 81BRANCHING, 18 35 60 102 200

216BRITTLE, 41 62 271 289 357 363BROMINE CONTAINING

COPOLYMER, 273

Subject Index


BUCKET, 67BUILDING APPLICATION, 7 385BULK MOULDING

COMPOUND, 202BUMPER, 67BUTYL ACRYLATE

COPOLYMER, 28 198BUTYL METHACRYLATE

COPOLYMER, 166 190BUTYLENE COPOLYMER, 102

113

CCALCINED CLAY, 324CALCIUM CARBONATE, 65 211

289 324CALCULATION, 8 14 77 98 114

149 162 172 190 227 276 277285 290 310 323 328 330 337344 362 382 390 392 394

CALIBRATION, 6 47 173 190 208216 229 238 270 297 309 310319 334 378 392

CALORIMETRY, 9 61 64 65 74 88133 150 154 186 290 302 305313 354 359

CAPILLARYELECTROPHORESIS, 46 5097

CAPILLARY GASCHROMATOGRAPHY, 76

CAPILLARY RHEOMETRY, 324325

CAR, 56 67CARBON 13, 130 193 209 265

268 297 359 370 389 392CARBON BLACK, 40 93CARBON DIOXIDE, 57 298 301

311 373 395CARBON DISULPHIDE, 311CARBON FIBRE-REINFORCED

PLASTIC, 36 178 182 196 231320

CARBONYL GROUP, 274 288CARBOXYLIC ACID, 288 341CASTING, 94 262 367CELLULAR MATERIAL, 80 84

85 97 302CELLULOSE, 43 82 263CELLULOSE ACETATE, 79CELLULOSE NITRATE, 46 79

185CEMENT, 276CHAIN LENGTH, 272 274CHAIN SCISSION, 274 380CHAR, 194CHEMICAL BONDING, 358

CHEMICAL COMPOSITION, 2572 80 89 103 107 146 159 172197 198 211 213 229 232 289318

CHEMICAL FORCEMICROSCOPY, 58

CHEMICAL IONISATION MASSSPECTROSCOPY, 222

CHEMICAL REAGENT, 53 334CHEMICAL RECYCLING, 39CHEMICAL RESISTANCE, 57

175CHEMICAL STRUCTURE, 1 8 12

16 25 31 47 49 51 53 56 66 6873 77 83 89 93 98 102 103 114130 133 140 152 158 159 164166 168 180 200 222 228 229243 264 268 269 274 275 277283 284 286 291 300 301 308310 317 318 328 331 334 337355 356 364 365 368 370 376382 391

CHEMILUMINESCENCE, 88CHEMOMETRIC ANALYSIS, 140

216CHINA CLAY, 226 306CHITIN, 246CHLORINATED

POLYETHYLENE, 146 392CHLORINE, 17 194 373CHLORODIFLUOROETHANE,

337CHLOROFORM, 3 208 369 382CHROMATOGRAPHIC

ANALYSIS, 66 81 86 89 96 97105 112 119 137 141 152 171191 194 229 235 303 304 366375 382 384

CHROMATOGRAPHY, 3 21 25 2829 30 34 35 39 40 46 50 52 5355 56 60 66 71 72 75 80 81 8486 87 89 96 97 102 103 105107 108 112 113 114 116 119120 124 128 137 141 152 158159 160 166 169 171 172 174183 185 186 190 191 194 195200 203 204 206 208 210 218222 229 233 235 239 240 241242 243 259 264 273 278 285295 299 303 304 307 310 311314 319 322 325 334 349 353355 356 366 372 373 375 376379 381 382 383 384 388 395398 399

CHROMIC ACID, 61CHROMOGEN, 16 288CLAY, 324CLEARCOAT, 27 44 175

CLOUD POINT, 12 98 125COATED FIBRE, 179COATED METAL, 157 227COATING, 19 27 44 62 66 121 126

138 163 168 174 175 185 217222 223 227 236 237 239 255259 266 298 312 325 359 383

COBALT STEARATE, 348COHESION, 94 145 167COLOUR, 274 288COLOURANT, 181COLUMN CHROMATOGRAPHY,

233 375COLUMN PACKING, 50 203 235

241 319 375COMBUSTION, 359COMPATIBILITY, 63 90 209 331

340COMPLEX VISCOSITY, 325COMPOSITE, 10 13 17 36 62 79

81 82 90 100 134 141 176 178179 182 196 197 199 202 211231 234 258 265 271 281 288289 296 318 320 333 339 357377

COMPOSITION, 72 73 100 122123 130 220 241 243 389 392394

COMPUTER AIDED ANALYSIS,46 67 108 173 174 214 309

COMPUTER MODEL, 144 152174 338

COMPUTER SIMULATION, 248367

CONCENTRATION, 55 102 105129 130 183 197 215 224 250262 283 300 311 317 339 353378

CONE CALORIMETER, 150 359CONFOCAL RAMAN

MICROSPECTROSCOPY, 168342

CONFORMATIONALANALYSIS, 360

CONTACT ANGLE, 37 61 202217 277 333 343

CONTACT LENS, 265CONTAINER, 57 266 278CONTAMINATION, 17 128 160

181 289 357COOLING, 57 67 139 309 323 324

358COOLING RATE, 57 126 207 309

323 324COPOLYESTER, 204 322COPOLYETHERSULPHONE, 47COPOLYMER COMPOSITION,

28 57 70 94 198 210 220 370

Subject Index


COPPER, 61 316 317CORONA TREATMENT, 205CORRELATION

SPECTROSCOPY, 344 364CORROSION, 255 271CREEP RATE SPECTROSCOPY,

363CRESOL, 355CRITICAL CONCENTRATION,

241CRITICAL POINT, 103 395CRITICAL SOLUTION

TEMPERATURE, 125CROSS-POLARISATION, 193 209

268 300CROSSLINK, 83 279CROSSLINK DENSITY, 179 269CROSSLINKED, 110 179 221 250CROSSLINKING, 9 10 20 24 27

36 46 48 49 73 85 115 134 161180 187 265 272 279 288 294300 309 326 368 377

CROSSLINKING AGENT, 222288

CRYSTALLINE, 2 59 143 147 283313

CRYSTALLINITY, 2 13 24 42 5457 62 63 64 69 94 102 113 114117 122 126 131 139 143 147168 257 260 274 277 281 291309 313 323 357 364 367 377391

CRYSTALLISATION, 2 9 12 1322 24 26 52 54 57 59 74 78 107117 122 131 136 139 147 148155 170 246 261 295 309 323329 332 336 386

CRYSTALLISATIONTEMPERATURE, 136 309

CRYSTALLITE, 57 139 260CURE TEMPERATURE, 2 48 161CURE TIME, 36 265 309CUREMETER, 134CURING, 8 20 27 36 68 73 83 89

138 144 149 161 163 178 182187 247 248 265 269 272 300305 309 312 316 349 377

CURING AGENT, 36 151 161 178182 222 250 272 288 317

CYCLOHEXANE, 21 263 285

DDATA ANALYSIS, 13 216 237 267

291 319DATA COLLECTION, 291 345DEBONDING, 236DECANE, 382

DEFECT, 67 88 126 289 329DEFORMATION, 41 59 67 249

277 283DEGRADABLE, 37 112 267 387DEGRADATION, 4 16 39 44 58

65 66 80 85 86 87 88 92 94 101112 119 135 148 152 164 175183 189 194 195 213 228 244258 266 267 274 279 288 294298 302 309 311 318 325 326330 338 347 357 374 377 380385

DEGRADATION PRODUCT, 4 1734 75 87 112 128 152 175 183194 274 279 288

DEGRADATIONTEMPERATURE, 194 269 380

DEGREE OF BRANCHING, 18 35DEGREE OF CROSSLINKING, 9

27 300 377DEGREE OF CRYSTALLINITY,

143 313DEGREE OF CURE, 10 36 269DEHYDROCHLORINATION, 146

392DELAMINATION, 255 312DENSITY, 18 52 56 106 131 168

179 216 231 261 289 313 367DENTAL APPLICATION, 172 247

276 343 346DEPOLYMERISATION, 39 165

266DEPTH PROFILING, 205 333 342

344DERIVATIVE

THERMOGRAVIMETRY, 380DESORPTION, 71 93 104 210 310

360DETECTION LIMIT, 56 174 289DIACID, 288 341DIBUTYL PHTHALATE, 76DIBUTYL SEBACATE, 277DICHLOROXYLENE, 48DICHROISM, 284DICUMYL PEROXIDE, 368DICYANATE POLYMER, 11DIELECTRIC ANALYSIS, 9 377DIELECTRIC CONSTANT, 46

237 338DIELECTRIC PROPERTIES, 46

245 338DIELECTRIC RELAXATION

SPECTROSCOPY, 49 110 259338

DIELECTROMETRY, 9DIETHYLENE GLYCOL, 26 121

266DIFFERENTIAL

INTERFERENCEMICROSCOPY, 324

DIFFERENTIALPHOTOCALORIMETRY, 377

DIFFERENTIAL SCANNINGCALORIMETRY, 2 6 7 8 10 1112 15 17 18 20 22 24 29 36 4151 54 56 63 64 65 74 77 78 8385 88 94 95 98 101 110 113 114122 125 126 131 133 134 135136 139 144 146 147 149 154155 161 163 164 170 186 187207 211 213 220 245 246 252253 254 258 261 267 269 276277 280 282 287 290 291 296302 305 309 313 323 324 328329 332 336 348 357 367 370377 382 386 387 390 394 398

DIFFERENTIAL THERMALANALYSIS, 2 6 7 8 10 12 1517 18 20 22 24 29 36 41 54 5663 64 65 74 77 78 83 88 94 9598 101 110 113 114 122 125126 131 133 134 136 139 144146 147 149 154 155 161 163164 170 186 187 207 211 213231 245 246 252 253 254 258267 269 276 277 280 287 290291 296 302 309 313 323 324328 329 332 336 348 357 367370 377 382 386 387 390 398

DIFFUSE REFLECTANCESPECTROSCOPY, 341

DIFFUSION, 9 56 80 99 124 125264 274 346 351 360 372 387394

DIFFUSION COEFFICIENT, 5699 111 224

DIGITAL ANALYSIS, 10DIGLYCIDYL ETHER

BISPHENOL A, 200DIMETHYL FORMAMIDE, 21 77DIMETHYL ISOPHTHALATE,

208DIMETHYL SULPHOXIDE, 342DIMETHYL TEREPHTHALATE,

39 208DIPHENYLMETHANE

DIISOCYANATE, 9DISCOLOURATION, 288DISPERSION, 181 217 289 361DISTILLED WATER, 56DISTORTION, 20 260DISTRIBUTION, 60 102 338DOMESTIC APPLIANCE, 80DOUGH MOULDING

COMPOUND, 211DRAW RATIO, 117 257 283 284

Subject Index


DRINKING WATER, 183 307DUCTILE FAILURE, 289DYE, 16 397DYNAMIC, 71 144 317 323 374DYNAMIC DIFFERENTIAL

SCANNING CALORIMETRY,11

DYNAMIC INFRAREDSPECTROSCOPY, 345

DYNAMIC LIGHTSCATTERING, 111

DYNAMIC MECHANICALANALYSIS, 36 56 73 83 92114 134 161 196 245 269 309377

DYNAMIC MECHANICALTHERMAL ANALYSIS, 325338 367

DYNAMIC PROPERTIES, 179317 325

DYNAMIC SPECTROSCOPY,345

DYNAMIC VISCOELASTICPROPERTIES, 101

EELECTRICAL CONDUCTIVITY,

38ELECTRICAL INSULATOR, 271ELECTRICAL PROPERTIES, 38

46 338 378ELECTROCHEMICAL

IMPEDANCESPECTROSCOPY, 5 223 227237 255

ELECTRODIALYSIS, 97ELECTROKINETIC

CHROMATOGRAPHY, 46ELECTROKINETIC

POTENTIAL, 333ELECTRON DISPERSIVE X-RAY

ANALYSIS, 6ELECTRON ENERGY LOSS

SPECTROSCOPY, 13 358ELECTRON IONISATION MASS

SPECTROMETRY, 206ELECTRON MICROSCOPY, 2 5

13 63 82 108 129 181 289 324ELECTRON SCANNING

MICROSCOPY, 2 5 13 63 82108 129 181

ELECTRON SPECTROSCOPYFOR CHEMICAL ANALYSIS,61

ELECTRON SPIN RESONANCESPECTROSCOPY, 45 66 294326 327 368

ELECTRONIC APPLICATION, 5ELECTROPHORESIS, 46 50 97ELECTROSPRAY IONISATION,

190 222 229 376ELEMENTAL ANALYSIS, 15 115

160 194 351ELUENT, 203 235 375ELUTION, 35 46 203 210 266 285

370 375 382ELUTION CHROMATOGRAPHY,

50ELUTION FRACTIONATION, 52ELUTION VOLUME, 35 285 310

356EMISSION, 56 87 174 321END GROUP, 36 102 130 151 229

274 314END-GROUP ANALYSIS, 190

200 334 376 388ENDOTHERM, 54 56 74 78 94

125 136 139ENDOTHERMIC, 235 245 276

309 329 359ENERGY ABSORPTION, 207ENERGY CONTENT, 357ENERGY DISPERSIVE X-RAY

ANALYSIS, 108 129 289 328ENGINEERING APPLICATION,

309 367ENTHALPY, 36 64 74 125 179 187

276 282 309 339 354 375ENTROPY, 339 375ENVIRONMENTAL SCANNING

ELECTRON MICROSCOPY,324

ENVIRONMENTAL STRESSCRACKING, 315

EPICHLOROHYDRIN, 272EPOXY NOVOLAC RESIN, 11EPOXY RESIN, 10 11 20 32 36 47

62 68 144 145 149 151 157 161178 179 182 199 200 222 249255 269 272 282 292 305 309312 320

EQUIPMENT, 6 46 138 194 197218 309 335 379

ERROR ANALYSIS, 13ETHANOL, 56 311ETHERSULPHONE

COPOLYMER, 47ETHYLENE ACRYLIC ACID

COPOLYMER, 51 348ETHYLENE-BUTYLENE

COPOLYMER, 52ETHYLENE CONTENT, 370 392ETHYLENE COPOLYMER, 22 60

63 102 113 154 209 259 348359 389

ETHYLENE GLYCOL, 39 266ETHYLENE-HEXENE

COPOLYMER, 52ETHYLENE-PROPYLENE

COPOLYMER, 69 274 370ETHYLENE TEREPHTHALATE

COPOLYMER, 131ETHYLENE-VINYL ACETATE

COPOLYMER, 57 70 100 209226 251 270 306 341 347 359373 389

ETHYLENE-VINYL ALCOHOLCOPOLYMER, 56 57 94 291387

ETHYLIDENE VINYLPYRROLIDONE, 250

EVANESCENT WAVESPECTROSCOPY, 111 292

EXCLUSIONCHROMATOGRAPHY, 28 2934 35 40 41 50 52 55 60 97 102103 108 112 114 116 158 166204 210 229 239 240 243 299314 322 334 355 375 381

EXOTHERM, 85 323EXOTHERMIC, 54 276 309 329

336EXTENDER, 121EXTRACTION, 71 97 128 171 185

195 266 331 372 373EXTRACTION

CHROMATOGRAPHY, 97EXTRUSION, 6 7 40 70 72 183

188 195 225 254 266 324 325

FFADING, 288FAILURE, 17 30 36 167 178 182

254 271 289 296 341 347 357FAILURE ANALYSIS, 36 108 145

167 254 289 329FAST ATOM BOMBARDMENT

MASS SPECTROSCOPY, 376FATTY ACID, 232FIBRE, 31 33 43 82 100 178 179

182 231 256 260 330 339 371FIBRE GLASS, 76 176 197FIBRE OPTIC, 36FIBRE-REINFORCED PLASTIC,

36 100 141 178 231 258 281320

FIELD EMISSION SCANNINGTRANSMISSION ELECTRONMICROSCOPY, 289

FIELD-FLOWFRACTIONATION, 35 97

FILLED, 179 318 325

Subject Index


FILLER, 17 43 45 65 81 90 93 184207 211 226 289 306 307 318324 325 399

FILLER CONTENT, 81 90 324FILLER DISTRIBUTION, 289 324FILM, 1 3 16 27 37 38 40 41 49 56

57 61 62 65 86 92 102 104 106115 117 118 135 142 148 156167 168 186 205 246 257 262266 269 288 289 308 324 327349 351 362 373 374 386 387

FINITE ELEMENT ANALYSIS,108

FIRE RETARDANT, 359FLAME IONISATION, 185FLAME RETARDANT, 95 152

211 218 273FLAMMABILITY, 150 173 273

359FLASH CHROMATOGRAPHY,

97FLASH PYROLYSIS, 4FLAVOUR, 183FLEXIBLE, 84 277 283 353FLOATATION, 97FLOW INJECTION ANALYSIS,

50FLOW MICROCALORIMETRY,

93FLOW RATE, 50 143 233 324 372FLUORESCENCE, 17 293FLUORESCENCE

SPECTROSCOPY, 108 116 157FLUOROPOLYMER, 279 387FOAM, 80 84 97 302FOOD-CONTACT

APPLICATION, 124 177 195208 264 286 387

FOOD PACKAGING, 57 124 168195 266 278 311

FORMULATION, 30 108 164 174217 312

FOURIER TRANSFORMINFRARED SPECTROSCOPY,1 3 6 8 11 24 25 26 29 30 34 3640 41 60 63 64 72 77 83 88 9293 94 98 102 107 108 113 117126 135 136 150 153 156 160161 163 165 169 170 173 181189 190 213 215 216 226 228246 249 250 252 259 262 264271 274 275 277 288 300 306309 316 318 321 328 341 343344 345 352 360 364 374 381385 386 397

FRACTION, 35 170 204 394FRACTIONATION, 28 52 97 107

113 337 370 398

FRACTURE, 67 82 98 178 236271 289

FRACTURE MORPHOLOGY, 213 54 61 98 115 191 319 346391 394

FREE ENERGY, 339FREE RADICAL, 45 266FREE VOLUME, 18 56 99 338

367 382FREEZING POINT, 324FREQUENCY, 78 118 179 255 256

287 309 325 336FUEL TANK, 56FUNCTIONAL GROUP, 36 83 274

331FUNGUS, 5FURAN RESIN, 199FURNITURE, 274

GGAMMA-IRRADIATION, 4 99

133 393GAS, 67 80 277 311GAS BARRIER, 56 57 168GAS CHROMATOGRAPHY, 3 4

30 34 39 53 56 66 71 72 75 7680 81 84 87 90 96 107 112 119120 124 128 132 141 143 160174 183 185 186 191 194 195198 208 217 218 221 232 235250 270 273 278 303 307 311339 349 353 373 382 383 390392 398

GAS DIFFUSION, 274GAS LIQUID

CHROMATOGRAPHY, 97GAS-PHASE, 67 80 277 311GAS PIPE, 277GAS TRANSMISSION, 311GEL, 46 319 326GEL ELECTROPHORESIS, 97GEL PERMEATION

CHROMATOGRAPHY, 50 107113 137 152 169 172 190 200233 259 264 295 310 325 334356 376 383 388 396 399

GELATION, 7 73 134 161 294GLASS, 145 167 276 351GLASS CONTENT, 296GLASS FIBRE, 76 176 197GLASS FIBRE-REINFORCED

PLASTIC, 17 179 202 211 231271 288 296 333

GLASS TRANSITIONTEMPERATURE, 12 15 18 2029 36 49 51 56 74 77 81 85 94101 106 110 114 117 122 135

149 155 161 163 164 170 179207 213 220 249 261 269 280282 287 290 305 308 309 323328 338 357 367 377 382 390394

GLOW DISCHARGE, 343GLOW DISCHARGE

SPECTROSCOPY, 202GRAVIMETRIC ANALYSIS, 23

82 85 93 94 152 189 196 211244 258 296 317 347 377 380

HHEADSPACE ANALYSIS, 311HEADSPACE

CHROMATOGRAPHY, 185HEAT CAPACITY, 20 74 78 125

161 179 220 253 261 276 280287 290 309 324 336 394

HEAT DEGRADATION, 23 26 2975 76 83 152 160 163 189 192194 196 244 266 273 318 325380 381

HEAT FLOW, 36 155 245 252 261276 309 324

HEAT INSULATION, 80 276HEAT RESISTANCE, 11 24 26 57

85 126 163 196 228 266 267269 295 317 377

HEAT STABILITY, 146 196HEAT TREATMENT, 57 119HEATING, 36 179 187 244 266

309 323 348 354HEATING RATE, 36 54 144 179

309 328 332 348 380HELIUM, 57HETEROGENEITY, 25 217 268HETEROGENEOUS, 129 146 170HEXANE, 240 319HIGH DENSITY

POLYETHYLENE, 52 56 57 6387 91 102 109 112 128 132 143164 195 212 214 307 357 372392

HIGH IMPACT PS, 48HIGH PERFORMANCE LIQUID

CHROMATOGRAPHY, 21 3539 46 76 97 165 171 183 195200 222 233 238 239 242 247264 266 286 304 337 366 375383 399 400

HIGH TEMPERATURE, 62 107277 381

HIGH RESOLUTION, 179 209289 340 354 363 389

HINDERED AMINE, 3 31 66 123225

Subject Index


HINDERED PHENOL, 41HIP JOINT, 42HOMOGENEITY, 100 289 340HOT STAGE MICROSCOPY, 2

181HUMIDITY, 44 56 57 309HYDROFLUOROCARBON, 321HYDROGEN BONDING, 77 94

99 114 342 364HYDROGEN CHLORIDE, 34 48

194 228HYDROLYSIS, 34 58 59 165 319

341 352HYDROPHILICITY, 46 51 360HYDROPHOBICITY, 37 46 360

375HYDROXYBENZENE, 75 297

300HYDROXYETHYL

METHACRYLATECOPOLYMER, 46

HYDROXYL GROUP, 36 69

IIDENTIFICATION, 30 79 121 128

132 212 214 353 370 397ILLUMINATION, 311IMAGING, 13 67 88 168 179 275

289 346IMIDAZOLE, 262IMIDISATION, 8 355IMMERSION, 178 223 237IMMISCIBLE, 188 367 394IMMUNOELECTROPHORESIS,

97IMPACT PROPERTIES, 56 63 231

370 388IMPLANT, 219 262 393IMPURITY, 221INDUCTION PERIOD, 41 88INDUCTIVELY COUPLED

PLASMA SPECTROMETRY,351

INELASTIC NEUTRONSCATTERING, 361

INFRARED ABSORPTION, 36274 362

INFRARED CAMERA, 67INFRARED DICHROISM, 284INFRARED SPECTROSCOPY, 1 3

8 11 14 17 24 26 29 33 34 36 3941 43 51 60 63 66 69 72 77 7985 88 92 93 94 98 108 113 126135 142 150 153 156 160 161163 164 165 169 172 173 181184 186 188 189 207 215 216225 226 228 230 244 246 249

250 256 257 259 262 264 269271 274 275 277 284 294 297301 306 316 318 321 328 341343 344 345 353 360 362 364365 371 374 381 383 385 386387 393 399

INFRARED THERMOGRAPHY,67

INJECTION MOULDING, 67 160231 296 357

INK, 239INSULATION, 80 276INTERACTION, 90 167 178 235

249 285 311 318 341 342 364INTERACTION PARAMETER,

220 235 285INTERCHAIN PACKING, 135INTERFACE, 178 179 182 206 229

236 322 341 342 346 367 394INTERFACIAL ADHESION, 333INTERFACIAL DEBONDING, 167INTERFACIAL INTERACTION,

90 167 178INTERFACIAL PROPERTIES, 81

90 111 141 167 178 249 320 342INTERFEROMETRY, 13 275 363INTERNAL MOULD RELEASE,

202INTRINSIC VISCOSITY, 29 172

266 330INVERSE GAS

CHROMATOGRAPHY, 81 90141 143 191 217 235 339 382390

ION CHROMATOGRAPHY, 97218

ION CYCLOTRON RESONANCE,397

ION EXCHANGE, 50 97 351IONISATION, 46 50 206 222 379IRON OXIDE, 112IRRADIATION, 4 40 92 153 358IRRADIATION DEGRADATION,

133ISOELECTRIC POINT, 46 333ISOMERISATION, 11 288ISOPHORONE DIISOCYANATE,

121ISOTACHOPHORESIS, 46ISOTACTIC, 129 133 274 314ISOTHERM, 67 178 309 339ISOTHERMAL, 36 78 117 125 276

317 338 348 375ISOTROPY, 117

KKAOLIN, 226 306

KEVLAR, 191KINETIC, 8 10 45 73 83 125 377KINETICS, 3 23 52 73 75 94 144

149 302 317 323 332 363 380381

LLAC RESIN, 352LACQUER, 185LAMELLAE, 78 139LAMINATE, 56 57 168 182 266

342LAMINATED FILM, 57 168 266

293LANGIVIN EQUATION, 3 46 50

60 75LASER, 62 212 236 298 351 397LASER INDUCED

DECOHESIONSPECTROSCOPY, 236

LASER INTERFEROMETRY, 363LASER IONISATION MASS

SPECTROMETRY, 6LASER LIGHT SCATTERING, 35

200LASER RAMAN

SPECTROSCOPY, 168LATERAL FORCE

MICROSCOPY, 308LATEX, 46 156 174 193 198LEACHING, 183LEAD, 201LEAST-SQUARES ANALYSIS,

70 214 345LENS, 219 265LIFETIME PREDICTION, 108

255 377LIGHT ABSORPTION, 229 274LIGHT DEGRADATION, 3 40 129

153 196 274 288LIGHT MICROSCOPY, 181 295LIGHT SCATTERING, 111 116

117 172 203 238 260 310 396LIGHT STABILISER, 3 31 123

132 288LIGHT STABILITY, 3 288LIGNOCELLULOSE, 82LINEAR LOW DENSITY

POLYETHYLENE, 57 92 107139 186 216 225 324 386

LINEAR REGRESSIONANALYSIS, 144

LIQUID CHROMATOGRAPHY,21 25 35 39 46 50 55 76 97 103105 108 124 159 165 171 183195 200 203 206 210 222 229233 238 239 240 241 242 243

Subject Index


247 264 266 285 286 299 304319 337 353 355 366 375 379383 384 395

LIQUID CRYSTAL POLYMER,309 367 387

LIQUID NITROGEN, 358LOW DENSITY

POLYETHYLENE, 3 57 86 87139 143 164 168 186 207 214266 324 325 348 372 373 386

LOW FREQUENCY, 126 363LOW MOLECULAR WEIGHT,

128 375

MMAGIC ANGLE, 209 268 283 291

300 340MAGNESIUM-25, 359MALDI-TOF SPECTROSCOPY,

28 103 127 137 158 159 166 204310 322 335 356 376

MALEIC ANHYDRIDE, 82MALEIC ANHYDRIDE

COPOLYMER, 28 341MAPPING, 69 275 289 339 342

344MASS SELECTIVE DETECTOR,

76 218MASS SPECTROMETRY, 4 6 13

28 30 50 75 103 107 112 127132 178 186 192 194 204 222229 266 278 307 311 376 379382 392 396 397 398

MASS SPECTROSCOPY, 28 66 7284 86 103 121 124 127 128 137153 158 159 166 177 185 190195 202 204 206 244 250 270273 303 310 312 322 335 356376 399

MATRIX, 36 82 141 178 182 351359

MATRIX-ASSISTED LASERDESORPTION, 28 103 127 137158 159 166 204 310 322 335356 376

MDI, 9MECHANICAL DEGRADATION,

266MECHANICAL PROPERTIES, 9

40 41 56 61 62 63 65 67 82 8486 91 114 115 126 151 163 168178 179 182 207 231 249 256269 271 277 281 288 289 296309 315 316 324 325 333 353365 370 388

MECHANICAL RECYCLING, 195MECHANICAL SPECTROSCOPY,

325MEDICAL APPLICATION, 42 262MELAMINE-FORMALDEHYDE

RESIN, 159 365MELT, 54 170 254 282 290 354MELT TRANSITION, 267MELTING, 2 24 54 78 79 136 155

179 209 252 309 332MELTING POINT, 12 52 56 63 94

114 164 266 295 324MELTING TEMPERATURE, 20 57

179 207 309 323 332 370MEMBRANE OSMOMETRY, 396METAL, 177 179 298 341METAL ADHESION, 62 223 341METAL COATING, 62 255METAL SALT, 352METALLISED FILM, 168 266 387METHACRYLATE COPOLYMER,

190METHACRYLIC ACID

COPOLYMER, 15 63 259METHACRYLIC ESTER

COPOLYMER, 190METHACRYLIC ESTER

POLYMER, 45 245METHANOL, 39 56 76 171 266METHANOLYSIS, 39METHYL ACETATE, 185METHYL ACRYLATE

COPOLYMER, 33 172 299 395METHYL ETHYL KETONE, 285METHYL METHACRYLATE, 288METHYL METHACRYLATE

COPOLYMER, 28 33 166 198308 384

METHYLBENZENE, 56 185 241261

METHYLENE CHLORIDE, 266MICROANALYSIS, 179 231 289MICROBIAL DEGRADATION, 5MICROCALORIMETRY, 154MICRODIELECTROMETRY, 9MICROEXTRACTION, 71 185MICRORAMAN

SPECTROSCOPY, 168 346MICROSCOPY, 2 13 16 27 38 41

58 59 61 98 111 125 126 142145 168 179 181 213 231 256257 277 289 295 308 324 387

MICROSTRUCTURE, 13 58 60168 170 198 274 370 388 392

MICROTOMY, 168MICROWAVE, 112 128 262MICROWAVEABLE, 266 387MID-INFRARED

SPECTROSCOPY, 362MIGRATION, 46 65 183 264 266

288 387MINERAL FILLER, 45 288 289

324MISCIBILITY, 12 64 77 98 125 146

209 213 220 309 367 390 391394

MOBILE PHASE, 50 375 395MODEL, 28 105 149 152 172 216

290 311 319 336 341 360 381382 394

MODULATED DIFFERENTIALSCANNING CALORIMETRY,10 36 74 125 131 135 161 220261 282 309 377 394

MODULATED TEMPERATURETHERMOMECHANICALANALYSIS, 20

MOISTURE CONTENT, 6 51 148266 309

MOLAR MASS, 25 35 102 103 107140 159

MOLECULARCONFIGURATION, 117 130135 168 328 338 355 367

MOLECULAR INTERACTION,178 220 342 375

MOLECULAR MOBILITY, 26 268301 389

MOLECULAR ORIENTATION,257 281 284 327 360

MOLECULAR STRUCTURE, 1 812 16 25 31 47 49 51 53 56 6668 72 73 77 80 83 89 93 98 101102 103 107 114 130 133 140146 152 158 159 164 166 168172 180 197 198 200 211 213222 228 229 232 243 264 268269 274 275 277 283 284 286289 291 300 301 308 310 317318 328 331 334 337 355 356364 365 368 370 376 382 391

MOLECULAR WEIGHT, 1 28 2942 46 50 52 54 55 62 73 89 102112 113 114 116 120 127 128130 158 164 166 172 185 190200 204 210 222 224 235 239243 285 310 314 319 322 323325 330 332 334 337 355 356375 376 378 381 382 388 395396

MOLECULAR WEIGHTDISTRIBUTION, 102 116 190200 204 224 310 314 319 322325 356 375 381 396

MONITORING, 5 70 149 174 188223 261 272 298 311 321 348

MONOETHYLENE GLYCOL, 39266

Subject Index


MONOMER, 124 229 269 270 387MORPHOLOGY, 2 13 54 61 63 98

115 118 136 191 213 256 309319 346 367 391 394

MOULDING, 134 225 343MULTI-ANGLE LASER LIGHT

SCATTERING, 35 200MULTILAYER, 168 266 344 387MULTILAYER FILM, 57 168MULTIPLE PULSE NMR, 291MULTIVARIATE ANALYSIS, 216MUNICIPAL WASTE, 128

NN-METHYL-2-PYRROLIDONE,

355NANOCOMPOSITE, 62NAPHTHA, 215NATURAL FIBRE, 82NATURAL FIBRE-REINFORCED

PLASTIC, 141NATURAL POLYMER, 232 352NEAR-INFRARED

CORRELATIONSPECTROSCOPY, 364

NEAR-INFRAREDSPECTROSCOPY, 14 36 215225 362 371

NITROCELLULOSE, 46 79 185NITROGEN, 57 76 95NITROGEN-CONTAINING

POLYMER, 250NON-DESTRUCTIVE TEST, 19

32 67 106 126 157 327NOVOLAC RESIN, 73 300NUCLEAR MAGNETIC

RESONANCE, 1 22 28 30 3132 34 57 60 68 73 77 100 108113 114 123 130 138 148 162169 172 180 189 193 201 209212 246 248 251 265 268 272283 291 297 300 314 331 334340 350 359 370 372 376 383388 389 391 392

NUMBER-AVERAGEMOLECULAR WEIGHT, 130375 378

NYLON, 33 56 57 79 125 164 168192 199 207 225 231 309 331

NYLON 1010, 24NYLON-12, 294 364NYLON-6, 33 56 57 132 207 387NYLON-6,6, 17 33 57 130 231 329

OODOUR, 57 183 307

OIL, 194 277OLIGOMER, 26 46 103 124 172

190 192 238 242 264 266 335ON-LINE MEASUREMENT, 314OPTICAL FIBRE, 36 188 292OPTICAL MICROSCOPY, 2 13 41

98 125 142 181 213 289 324387

OPTICAL PROPERTIES, 1 3 4757 162 181 199 200 206 263274 288 292 293 323 332 350362 375

OPTIMISATION, 50 102 105 171233 318 373

ORGANOLEPTIC PROPERTIES,57 183

ORIENTED, 104 117 283 284 361387

ORTHOPAEDIC APPLICATION,393

OSCILLATING DIFFERENTIALSCANNING CALORIMETRY,7

OSMOMETRY, 29 46 200 378OVEN STABILITY, 266OXIDATION, 40 41 61 66 88 94

104 129 152 153 205 266 269274 288 325 329 348 381 393

OXYGEN, 57 104 153 262 274311

OXYGEN ABSORPTION, 104387

OXYGEN BARRIER, 56 57 168

PPACKAGING, 5 57 128 131 168

212 264 266 278 323 387PACKAGING FILM, 57 168 266

387PAINT, 62 174 185 217 255 298PAPER, 266 387PAPER CHROMATOGRAPHY, 97PARACRYSTALLINE, 102 207

213 315PARTIAL LEAST SQUARES, 215

216PARTICLE BEAM ANALYSIS,

206PARTICLE PACKING, 324PARTICLE SIZE, 13 45 50 81 225

233 319 324 372 375PARTICLE SIZE

DISTRIBUTION, 62 324PEAK INTENSITY, 168 178 260

289 392PELLET, 216 266 296 373PERMEABILITY, 56 57 168 237

PERMITTIVITY, 338PEROXIDE, 294 326PEROXY COMPOUND, 393PESTICIDE, 373PH, 46 50 130 183PHARMACEUTICAL

APPLICATION, 46 221PHASE BEHAVIOUR, 267 340

365PHASE SEPARATION, 110 125

156 391 394PHENOL, 75 297 300PHENOL-FORMALDEHYDE

RESIN, 73 297 300PHENOLIC ANTIOXIDANT, 183PHENOLIC RESIN, 83 199 300PHOSPHORUS, 95 312 373PHOTOACOUSTIC

SPECTROSCOPY, 249 288 344PHOTOCALORIMETRY, 377PHOTOCHEMICAL

DEGRADATION, 288PHOTOCROSSLINKING, 45 187PHOTODEGRADATION, 16 19

65 66 274 279PHOTOELECTRON

SPECTROSCOPY, 13 37 48100 104 121 167 175 176 196197 202 205 277 279 298 308312 316 320 333 343

PHOTOINITIATOR, 27 312PHOTOISOMERISATION, 288PHOTOLYSIS, 153PHOTON CORRELATION

SPECTROSCOPY, 224PHOTOOXIDATION, 40 129 153

274 288PHOTOVOLTAIC PROPERTIES,

38PHTHALATE, 288PHTHALOCYANINE GREEN, 65PHYSICAL AGEING, 101 135 213

309 338PHYSICAL PROPERTIES, 12 42

52 56 63 94 114 164 188 215216 236 259 266 295 324 353382

PIGMENT, 65 121 181 217 225236 237 325 399

PIPE, 52 183 277 307 329PLANT FIBRE, 82PLASMA TREATMENT, 61 69

106 230 262 298 343PLASTICISATION, 36 56 301 348PLASTICISER, 33 34 120 184 258

277 353 387 399PLASTICS WASTE, 87 211 212PLATE-OUT, 6

Subject Index


POLARISATION, 256 257 284POLARISED CONFOCAL

RAMAN MICROSCOPY, 257POLARISED FLUORESCENCE,

284POLARISED LIGHT

MICROSCOPY, 181POLARISED OPTICAL

MICROSCOPY, 13POLARISING MICROSCOPY,

168POLARITY, 50 203 339POLYACETAL, 164POLYACRYLAMIDE, 46 240POLYACRYLATE, 245 269POLYACRYLIC, 249 343POLYACRYLIC ACID, 46 172 342POLYACRYLIC IMIDE, 387POLYACRYLONITRILE, 33 79

119 342POLYALPHA-

METHYLSTYRENE, 153POLYAMIC ACID, 355POLYAMIDE, 33 56 57 79 125

164 168 192 199 207 225 231309 331

POLYAMIDE-1010, 24POLYAMIDE-12, 159POLYAMIDE-6, 33 56 57 132 165

207 387POLYAMIDE-6,6, 17 130POLYAMIDE-IMIDE, 316POLYAMINE, 46 272POLYANILINE, 46 115POLYARAMIDE, 191 339POLYARYL ETHER KETONE,

213POLYARYLATE, 367POLYBENZIMIDAZOLE, 79POLYBENZYL

METHACRYLATE, 35POLYBIBENZOATE, 309POLYBISGLYCIDYL

METHACRYLATE, 247POLYBUTYL ACRYLATE, 156

394POLYBUTYL METHACRYLATE,

21 376POLYBUTYL THIOPHENE, 327POLYBUTYLENE

NAPHTHALATE, 98POLYBUTYLENE

TEREPHTHALATE, 164 273POLYCAPROLACTONE, 147 267

390POLYCARBONATE, 14 57 62 72

79 99 101 199 207 245 273 280309 340 356 363 367 382 398

POLYCYANATE, 11POLYCYANURATE, 317POLYDEUTEROPOLYETHYLENE,

361POLYDICYANATE, 11POLYDIMETHYLPHENYLENE

OXIDE, 356POLYDIMETHYLSILOXANE,

140POLYDISPERSITY, 29 35 127 137

204 224 325 335 356POLYEPICHLOROHYDRIN, 390POLYEPOXIDE, 10 20 32 36 47

62 68 144 145 149 151 157 161178 179 182 199 200 222 249255 269 272 282 292 305 309312 320

POLYESTER RESIN, 199 204 288POLYESTER-URETHANE, 114POLYESTERIMIDE, 355POLYETHER, 54 66 158 235 238

242 384 398POLYETHER SULPHONE, 75

125 151 356POLYETHER-ETHERKETONE,

54 79 126 213 295 315POLYETHER-URETHANE, 90POLYETHERETHERKETONE, 79

126POLYETHERIMIDE, 64 79 98 192

296 367 387POLYETHERSULPHONE, 75 125

151 356POLYETHYL ACRYLATE, 58POLYETHYL METHACRYLATE,

390POLYETHYLENE, 42 52 56 57 60

61 63 65 79 87 91 92 99 102107 109 112 128 132 139 143146 148 154 157 164 168 181186 188 195 199 207 212 214216 225 249 256 260 263 266267 283 293 307 315 324 325344 348 357 361 365 366 368370 372 373 386 392 393 398400

POLYETHYLENE GLYCOL, 46233 310 369 378

POLYETHYLENE GLYCOLTEREPHTHALATE, 26

POLYETHYLENENAPHTHALATE, 387

POLYETHYLENE OXIDE, 125154 235 337

POLYETHYLENETEREPHTHALATE, 2 12 2639 40 57 63 64 74 76 79 106117 118 131 136 157 164 168

207 212 214 257 261 263 266269 283 293 309 323 336 357358 382 388 398

POLYFLUOROETHYLENE, 79164 180 279 296

POLYHYDROXYBUTYRATE, 59POLYHYDROXYBUTYRIC

ACID, 246POLYHYDROXYETHYL

METHACRYLATE, 172 248POLYHYDROXYKETONE, 349POLYHYDROXYSTYRENE, 77

367POLYIMIDE, 5 23 79 196 199 320

355POLYIONENE, 57 276POLYISOCYANATE, 9POLYKETONE, 54POLYLACTIC ACID, 267POLYMERIC FLAME

RETARDANT, 218 273POLYMERIC MOULD RELEASE

AGENT, 202POLYMETHACRYLATE, 45 245

398POLYMETHACRYLIC ACID, 15

141POLYMETHACRYLONITRILE,

141POLYMETHYL

METHACRYLATE, 14 21 116132 137 141 159 166 178 204219 220 221 224 229 240 241284 285 289 299 301 304 314319 335 338 343 363 375 382384 394 397 398

POLYMETHYLENE OXIDE, 79POLYOL, 84 110POLYOXYETHYLENE, 154POLYOXYMETHYLENE, 79POLYPHENYLENE, 398POLYPHENYLENE ETHER, 79

152 220 367POLYPHENYLENE OXIDE, 79

152 220 357 367 394POLYPHENYLENE SULPHIDE,

79 170 296 320 328POLYPHENYLENE

TEREPHTHALAMIDE, 339POLYPHENYLMETHACRYLATE,

367POLYPHENYLSULPHONE, 79POLYPROPYLENE, 31 41 57 59

79 87 88 91 102 104 109 112118 123 128 129 132 133 168171 183 188 205 206 207 212214 249 264 281 284 289 293329 330 370 380 381 398

Subject Index


POLYPROPYLENE GLYCOL,334

POLYPROPYLENE GLYCOLMALEATE, 288

POLYPROPYLENE OXIDE, 103POLYPYRROLE, 46POLYSTYRENE, 14 21 35 46 48

57 58 79 82 85 87 118 141 153156 159 160 164 166 203 207212 214 220 230 245 278 290299 304 308 315 334 351 363367 375 382 394 395 398

POLYSULPHONE, 75 79 99 125331

POLYTETRAFLUOROETHYLENE,79 164 180 279 296 363

POLYTETRAMETHYLENEOXIDE, 384

POLYTHIOPHENE, 38POLYURETHANE, 19 66 79 80 84

89 110 157 158 163 169 187199 207 255

POLYVINYL ACETATE, 79 199209 220 268 270 367 394

POLYVINYL ALCOHOL, 1 46 5157 284 342

POLYVINYL CARBAZOLE, 162POLYVINYL CHLORIDE, 6 7 17

57 79 87 108 141 145 146 167184 194 201 207 212 214 227228 254 262 315 326 353 374385 392 394

POLYVINYL ESTER, 320POLYVINYL METHYL ETHER,

363POLYVINYL PHENOL, 77 367POLYVINYL PYRROLIDONE, 46

77 248 250 340POLYVINYLBENZENE, 79 85 87

118 153 212 290 315POLYVINYLCARBAZOLE, 162POLYVINYLIDENE CHLORIDE,

57 168 387POLYVINYLIDENE FLUORIDE,

12 79 277 390POLYVINYLPYRROLIDONE, 46

77 248 250 340PORE SIZE, 50 241 285 319 375POROSITY, 50 126 142 203 241

285 319 367 375POSITRON ANNIHILATION

LIFETIME SPECTROSCOPY,19 99 338 367

POST-CONSUMER, 195 214 266373

POTABLE WATER, 183 307POTASSIUM BROMIDE, 262 271POWDER, 126 175 194

POWDER COATING, 222PRE-TREATMENT, 176 197 215

223 351PRECIPITATION, 35 266PRESSURE, 50 56 171 194 206

222 236 395PRINCIPAL COMPONENTS

ANALYSIS, 216PROBE, 179 339 382PROBLEM PREVENTION, 30

181 296 303PROCESSING, 115 168 199 207

209 231 254 261 323 325 329373 388

PROPYLENE, 264PROPYLENE COPOLYMER, 18

22 69 102PROPYLENE-ETHYLENE

COPOLYMER, 69 274 370PROTECTIVE COATING, 217

255PROTON MAGNETIC

RESONANCE, 265 291 314388

PROTON SPIN RELAXATION,209 268

PULSED NMR, 272PURITY, 120 192PYROLYSIS, 4 75 83 87 119 192

194 212 234 270 273 296 303374 380 392

PYROLYSIS GASCHROMATOGRAPHY, 4 96107 132 198 218 221 232 250270 392

PYROLYSIS-IRSPECTROPHOTOMETRY, 4

PYROLYSIS MASSSPECTROMETRY, 4 192

QQUALITATIVE ANALYSIS, 195QUALITY, 183 311 361QUALITY CONTROL, 67 131 329

347 353 357 386QUANTITATIVE ANALYSIS, 102

171 179 184 195 221 278 373QUENCHING, 101 117 135 261

363

RRADIATION CURING, 269RADIO FREQUENCY

DISCHARGE, 343RADIOLYSIS, 4RAMAN SPECTROSCOPY, 16 27

30 33 42 47 69 70 108 109 129140 151 168 182 212 214 215216 256 257 263 281 284 288293 300 342 346 365 369 393

RAPID SCAN, 344 345REACTIVITY, 151 274 388 392REARVIEW MIRROR, 67RECLAIM, 289RECOVERY, 319RECRYSTALLISATION, 54 136

309 332RECYCLABILITY, 57 88 266 387RECYCLATE, 64 91 122 195 329

373RECYCLING, 39 57 64 88 91 122

128 165 195 211 212 231 266373 387

REFLECTANCESPECTROSCOPY, 257 343

REFRACTIVE INDEX, 1 106 190200 229 292 375

REFRIGERATOR, 80REGRESSION ANALYSIS, 144

214 215 216 224 345REINFORCED PLASTIC, 13 17

36 79 81 90 100 134 141 176178 179 182 196 197 199 202211 231 234 271 281 288 296318 320 333 339 357 377

RELATIVE HUMIDITY, 44 56 57309

RELAXATION, 74 282 287 290309 363

RELAXATION MAP ANALYSISSPECTROSCOPY, 377

RELAXATION SPECTRA, 325RELAXATION TIME, 209 291

340RELAXATION TRANSITION,

290RELEASE AGENT, 202REPEATABILITY, 347REPRODUCIBILITY, 6 46 347

375RESIDENCE TIME, 266 325 357RESIDUAL ADDITIVE, 221RESIDUAL CATALYST, 129RESIDUAL STRESS, 67 316RESOLUTION, 50 118 229RETENTION TIME, 119 222RETENTION VOLUME, 143 375REVERSE OSMOSIS, 97REVERSE-PHASE

CHROMATOGRAPHY, 50 195233

REVIEW, 13 55 59 71 79 107 199205 212 283 284 310 350 363364 365 367 372 377 383 387

Subject Index


390 391 396RHEOLOGICAL PROPERTIES,

10 20 29 41 46 73 149 161 163217 266 295 324 325 338 354

RHEOMETRY, 10 324 325RHEOPHOTOACOUSTIC

SPECTROSCOPY, 249ROPE, 281ROTATING FRAME, 209 268 340ROUND ROBIN TEST, 173

SSAMPLE PREPARATION, 13 72

123 124 207SAMPLE SIZE, 72 124 143SAMPLING, 13 71 72 123 124 207

233 351SAN, 110 147 207 220 284 315

345SATURATED POLYESTER, 26 49

106 114 204 229 267 322 336367 376 388 398

SCANNING ELECTRONMICROSCOPY, 2 5 6 13 59 6162 63 82 98 108 129 181 202231 289 316 324 358

SCANNING PROBEMICROSCOPY, 59 179

SCISSION, 4 152 274 380SCRAP POLYMER, 122 128 214

231SEALANT, 247SEALING, 387SEAT, 274SECONDARY AMINE, 36 151SECONDARY ANTIOXIDANT,

93SECONDARY ION MASS

SPECTROSCOPY, 13 121 178202 312

SECONDARY STABILISER, 228SEMICONDUCTOR, 321SEMICRYSTALLINE, 102 106

122 207 213 235 315SENSITIVITY, 118 291SENSOR, 20 292SEPARATION, 35 55 97 105 128

243 341 351 370 375 384SEQUENCE ANALYSIS, 50SHEAR, 9 178 182 324 325 333SHEET, 186SHEET MOULDING

COMPOUND, 202 211SHELF LIFE, 57 311 387SHELLAC, 232 352SHIFT FACTOR, 209SIDING, 385

SILICA, 6 21 40 45 46 90 203 289319 375

SILICA GEL, 241 319SILICATE, 65 81SILICONE POLYMER, 204 284SIMULATED BODY FLUID, 34SIMULATION, 34 134 149 323

362 367SIZE EXCLUSION

CHROMATOGRAPHY, 28 2934 35 40 50 52 55 60 97 102103 108 112 114 116 158 166204 229 239 240 243 299 314322 334 375 381

SIZING, 176SMALL-ANGLE, 117 291 354SMOKE EMISSION, 76 150 173SOFTENING TEMPERATURE,

179SOFTWARE, 67 195 344SOL-GEL, 53SOLAR ENERGY

APPLICATION, 38SOLID STATE, 193 209 268 283

291 300 340 359 389SOLUBILITY, 56 79 90 97 114

115 160 372 375SOLUTE, 50 235 382SOLUTION, 21 46 55 77 115 116

130 178 224 268 291 351 367389

SOLUTION CASTING, 94 262367

SOLUTION VISCOSITY, 396SOLVENT, 21 29 35 56 113 124

130 185 203 210 235 259 261266 285 349 360 366 369 375388

SOLVENT EXTRACTION, 266331

SOLVENT PERMEABILITY, 56SOXHLET EXTRACTION, 112SPECIFIC HEAT, 20 122 207 309

324 354SPECIFIC VOLUME, 18SPIN-PROBE ANALYSIS, 45SPIN RELAXATION, 209 268 300SPOILAGE INDICATOR, 311STABILISER, 3 40 41 66 86 183

184 201 225 228 288 372STABILITY, 24 26 57 85 126 163

196 228 266 267 269 295 317324 377

STANDARD, 120 183 184 392STAR-BRANCHED, 35STARCH, 112 267 348STARCH POLYMER,STATIC HEAD SPACE GAS

CHROMATOGRAPHY, 71STATIONARY PHASE, 50 203

235 375STEEL, 223 341STEP-SCAN PHOTOACOUSTIC

SPECTROSCOPY, 344STEREOREGULARITY, 168STERIC EXCLUSION

CHROMATOGRAPHY, 41STERILISATION, 42 393STORAGE, 309 311STORAGE TIME, 311STRAIN, 315 325 365STRENGTH, 9 167 269 315STRESS, 67 168 182 281 289 315

316 325STRESS CRACKING, 271STRESS-STRAIN PROPERTIES,

61 231 281 325STRUCTURAL ADHESIVE, 62STRUCTURAL ANALYSIS, 168STRUCTURE-PROPERTY

RELATIONSHIP, 209 269 389STYRENE, 199 278 288STYRENE-ACRYLONITRILE

COPOLYMER, 72 110 147 207220 284 315 345

STYRENE COPOLYMER, 28 69127 198 299 308 363 395

STYRENE-ISOPRENE-STYRENE BLOCKCOPOLYMER, 394

STYRENE-METHACRYLICACID COPOLYMER, 81

SUB-GLASS TRANSITION, 170SUBSTRATE, 126 223 236 262

285 298SULPHUR DIOXIDE, 75SUPERCRITICAL, 39SUPERCRITICAL FLUID

CHROMATOGRAPHY, 50 372SUPERCRITICAL FLUID

EXTRACTION, 97 171 372373

SUPERCRITICAL GAS, 301SURFACE ANALYSIS, 19 30 37

38 44 58 59 62 67 69 118 175178 179 202 219 289 324 333

SURFACE AREA, 197 324SURFACE CHEMISTRY, 93 298

319SURFACE ENERGY, 52 141 217

235 277 339SURFACE PROPERTIES, 42 44

106 118 179 191 196 217 219277 308 312 360 383

SURFACE TREATMENT, 61 6281 168 176 178 182 197 205

Subject Index


223 230 262 277 298 343 371SURFACTANT, 46 65 233SURGICAL APPLICATION, 219

393SWELLING, 15 237 250 326 360SYNCHROTRON RADIATION,

291SYNTHETIC FIBRE-

REINFORCED PLASTIC, 281

TTALC, 65 318 324TAPE, 284TAPPING MODE ATOMIC

FORCE MICROSCOPY, 58TASTE, 57TEMPERATURE DEPENDENCE,

49 99 135 146 147 170 196 259269 308 336 354 364 382

TEMPERATURE GRADIENTINTERACTIONCHROMATOGRAPHY, 304375

TEMPERATURE MODULATEDDIFFERENTIAL SCANNINGCALORIMETRY, 54 78 136252 253 280 287 290 309 336

TEMPERATURE PROFILE, 67324

TEMPERATUREPROGRAMMEDANALYTICAL PYROLYSIS,273

TEMPERATURE RANGE, 207317 364 380 382

TEMPERATURE RISINGELUTION FRACTIONATION,370 396

TENSILE PROPERTIES, 40 41 6163 65 86 114 115 231 277 315333

TEREPHTHALIC ACID, 76TERTIARY AMINE, 36 151TEST SPECIMEN, 236 346 351

358TESTING, 19 43 58 59 62 71 79

96 108 112 120 123 124 134145 174 182 183 184 185 195206 208 254 255 270 288 293304 315 321 329 332 345 347357 363 365 379 382 398

TETRAHYDROFURAN, 29 35240 241 319 395

TEXTILE APPLICATION, 371THERMAL AGEING, 88 152THERMAL ANALYSIS, 7 20 26

36 54 56 67 78 83 92 95 110

133 134 144 147 149 154 155170 179 186 187 189 207 245252 258 267 269 270 305 309313 324 325 367 377 383 386394

THERMAL CONDUCTIVITY, 80179 309 324 377

THERMAL DEGRADATION, 2326 29 75 76 83 85 152 160 163189 192 194 196 244 258 266273 318 325 380 381

THERMAL DIFFUSIVITY, 179324 394

THERMAL FIELD-FLOWFRACTIONATION, 35

THERMAL HISTORY, 57 135 136207 245 254 262 287 309

THERMAL IMAGING, 67THERMAL INSULATION, 80 276THERMAL MECHANICAL

ANALYSIS, 196 377THERMAL RELAXATION, 282

290THERMAL RESISTANCE, 196THERMAL STABILITY, 11 24 26

57 85 126 163 196 228 266 267269 295 317 377

THERMAL TRANSITION, 56 78220 282 290 309

THERMAL VOLATILISATIONANALYSIS, 189

THERMALLY STIMULATEDCURRENT, 323 377

THERMOANALYTICAL, 348THERMODYNAMIC

PROPERTIES, 21 90 122 155169 172 220 235 290 339

THERMOGRAM, 36 67 323 348370

THERMOGRAVIMETRICANALYSIS, 2 8 12 15 17 23 2426 29 48 82 83 85 93 94 98 146152 163 164 189 192 194 196211 228 231 244 258 267 269295 296 316 317 318 326 330347 348 377 380 381 398

THERMOLYSIS, 189THERMOMECHANICAL

DEGRADATION, 266THERMOMECHANICAL

PROPERTIES, 179 269THERMOOXIDATIVE

DEGRADATION, 41 94 152269 348

THERMORHEOLOGICALPROPERTIES, 338

THICKNESS, 27 56 62 67 168 179236 255 257 263

THIN LAYERCHROMATOGRAPHY, 97 399

TIE LAYER, 168TIME, 54 61 94 135 209 223 253

261 268 277 289 317 338 354394

TIME DEPENDENCE, 125 196360

TIME OF FLIGHT, 103 127 137158 159 166 178 202 204 229310 312 322 335 356 376

TIME RESOLVEDSPECTROSCOPY, 170

TITANIUM DIOXIDE, 40 65 217237 325

TOLUENE, 56 185 241 261 319TOTAL ORGANIC CARBON, 183TOXICITY, 173 195TRACE ELEMENT, 177TRANSITION PHENOMENA,

254TRANSITION PROPERTIES, 203

269 340 354TRANSITION TEMPERATURE,

179TRANSMISSION ELECTRON

MICROSCOPY, 2 5 13 59 6382 108 129 181 213 289 331358

TRANSMISSIONSPECTROSCOPY, 234 292 362

TRANSPARENCY, 57 236 323TRANSPORT PROPERTIES, 56

115TRIAZINE, 40TRICHLOROBENZENE, 29TRICHLOROMETHANE, 29TRIETHYLAMINE, 298TRIFLUOROACETIC ACID, 388TROUBLESHOOTING, 30 181

296 303TWO-DIMENSIONAL, 55 58 209

233 242 275 283 344 345 364365

UUHMWPE, 260 393ULTRA-HIGH RESOLUTION

SPECTROSCOPY, 363ULTRASONIC, 112 126 272ULTRAVIOLET ABSORPTION,

229 274ULTRAVIOLET CURING, 27 269

349ULTRAVIOLET DEGRADATION,

16 19 196ULTRAVIOLET IRRADIATION,

Subject Index


19 40 44 196ULTRAVIOLET RESISTANCE,

57 196ULTRAVIOLET SPECTRA, 3 41

65 86 157 264 372 383 399ULTRAVIOLET

SPECTROSCOPY, 1 3 41 46 6586 115 157 288 372

ULTRAVIOLET STABILISER,225 288 399

UNIT CELL, 13 168UNPLASTICISED POLYVINYL

CHLORIDE, 254UNSATURATED POLYESTER,

82 199 204 288 333UV VIS SPECTROSCOPY, 1 46

115 288

VVACUUM DISTILLATION, 97

185VACUUM PYROLYSIS, 87 194VAPOUR PERMEABILITY, 56

168VAPOUR PHASE OSMOMETRY,

396VAPOUR PRESSURE

OSMOMETRY, 29 200 378VARNISH, 174VEHICLE BONNET, 329VEHICLE MIRROR, 67VIBRATIONAL

SPECTROSCOPY, 14 16 17 2627 30 33 36 39 42 43 47 51 6970 85 108 109 129 140 142 150151 156 164 168 172 173 182184 186 188 207 212 214 215216 225 226 230 244 256 257263 269 274 281 284 288 293297 300 318 342 345 346 353365 369 393

VINYL ACETATE, 251 270VINYL ACETATE COPOLYMER,

209 359 389VINYL ACETATE-ETHYLENE

COPOLYMER, 100 270 341359

VINYL CHLORIDE, 199 392VINYL CYANIDE, 119VINYL CYANIDE COPOLYMER,

57

VINYL ESTER RESIN, 320VINYL GROUP, 274VINYL PYRROLIDONE

COPOLYMER, 46VISCOELASTICITY, 20 219 308VISCOMETRY, 29 200 203 355VISCOSITY, 10 29 46 149 172 266

324 325 330VISIBLE SPECTROSCOPY, 1 46

115 288VITRIFICATION, 78 161 290VOLATILE CONTENT, 72 185VOLATILE ORGANIC

COMPOUND, 84 174 185 255278 321

VOLATILISATION, 72 97VOLUME FRACTION, 13 227

231 324 332 367

WWASTE, 87 122 128 211 212 266

387WATER, 39 56 61 266 360WATER ABSORPTION, 51 56 237

309WATER CONTENT, 6 51 148WATER PERMEABILITY, 56 237WATER PIPE, 307 329WATER TREE GROWTH RATE,

148WATER VAPOUR

PERMEABILITY, 56 168WAVE NUMBER, 168WAVELENGTH, 44 207 288WAX, 232WEATHERING, 44 62 86 92 222

385WEIGHT AVERAGE

MOLECULAR WEIGHT, 375WEIGHT CHANGE, 348WEIGHT FRACTION, 176 394WEIGHT GAIN, 56WEIGHT LOSS, 56 94 164 267

296 347 380WETTABILITY, 37 343WIDE ANGLE, 117 213 260WIDE ANGLE X-RAY

SCATTERING, 24WINDOW, 7WOOD FIBRE-REINFORCED

PLASTIC, 9 82 141 258

XX-RAY ANALYSIS, 6 108 129 212

231 289 328 383X-RAY DIFFRACTION, 13 41 57

83 92 95 117 213 260 277 291327 328 398 399

X-RAY FLUORESCENCE, 17 399X-RAY FLUORESCENCE

SPECTROSCOPY, 108X-RAY NEAR EDGE

ABSORPTIONSPECTROSCOPY, 358

X-RAY PHOTOELECTRONSPECTROSCOPY, 13 37 48100 121 145 167 175 176 196197 202 277 279 298 308 312316 320 333 343

X-RAY RESISTANCE, 104 279X-RAY SCATTERING, 13 24 41

57 83 92 95 117 213 260 277291 327 328

X-RAY SPECTROSCOPY, 13 3748 63 100 108 121 167 175 176196 197 202 277 279 298 308312 316 320 328 333 343 354358

XENON LIGHT, 274

YYELLOWING, 288YOGHURT POT, 278YOUNG’S MODULUS, 40 114

168 231 256 269 309 365

ZZEOLITE, 307ZIEGLER CATALYST, 102 129ZINC, 298ZINC BORATE, 359ZIRCONOCENE, 365

Subject Index


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(Rapra Technology Limited) ISBN 1-85957-333-9 · Rapra Technology Limited, Shawbury, ... Abstract...

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