CP:PMB–1 Code of Practice: Manufacture, Storage and Handling...

First Edition

Promoting best practice in the use of polymer modified binders

Code of Practice:Manufacture, Storage

and Handling ofPolymer Modified Binders

June 2004

CP:PMB–1

http://www.austroads.com.au/

advisory note 7Guide to the Selection, Heating and Storage of

Binders for Sprayed Sealing and Hot Mixed Asphalt

August 2003

A general guide to the selection, heating and storage of bituminous binders used in sprayed sealing and hot mixed asphaltapplications is provided in the tables on the following pages. Bitumens produced by refining crude petroleum oil and bitumensmodified by the addition of polymeric or other similar materials are included. Although the information provided in the tablewas correct at the time of publication, potential users of bituminous products are advised to contact suppliers for currentinformation and Material Safety Data Sheets prior to using any particular product. While the tabulated storage times andtemperatures are considered acceptable, users are strongly advised to store bituminous materials at the lowestpractical temperature and for the shortest possible duration.

Head Office: Level 2, 5 Wellington Street, KEW Victoria 3101Tel: (03) 9853 3595 Fax: (03) 9853 3484 E-mail: [email protected] Web: www.aapa.asn.au

Modified Binder Classification SystemPolymer Modified Binders (PMBs)(a) The PMB classification system is based on the application of the binder, the minimum Consistency at 60°C and

where appropriate, the predominant polymer group represented in the binder.(b) Binder systems are coded by application as “S” (for sealing classes) or “A” (for asphalt classes).(c) Polymer groups are coded as “E” (for elastomeric polymer types), “P” (for plastomeric polymer types) or “R” (for

granulated crumb rubber materials). Code E includes SBS (styrene-butadiene-styrene), SIS (styrene-isoprene-styrene), SBR (styrene-butadiene rubber), natural rubber, PBD (polybutadiene), chloroprene and other similar polymertypes. Code P includes EVA (ethylene vinyl acetate), EMA (ethylene methacrylate), APP (atactic polypropylene),various forms of PE (polyethylene) and other similar polymer types. Code R includes crumbed rubber, usually fromold tyres. The binder may be blended in the sprayer immediately prior to use, or it may be pre-blended in a mixingfacility. Where the binder is prepared in the field, the code RF is used.

For example, S45R is a sealing class PMB based predominantly on crumb rubber and designated by its minimum Consistencyat 60°C (4,000 Pa.s). Similarly, A20E is an elastomeric asphalt class PMB designated by its minimum Consistency at 60°C(8,000 Pa.s).Multigrade BindersThe Multigrade binder classification system is based on the approach used in AS2008 for unmodified binders. For example,C600/170 is a multigrade binder with high temperature (60°C) properties of C600 bitumen and low temperature properties(penetration at 25°C) of C170 bitumen.

Service Condition Binder Class

Application Cracking Traffic

Activity Width Site Loading/Severity Severity

SAMI All NA All

Slow

SAM Rapid High

Low

Severe All

HSS Mod Heavy

Medium

Adequate Binder

S45R S55R C600/ 170S10E S20E S25E S35E

Guide to the Selection of Sprayed Seal Modified Binders

Guide to the Heating and Storage of Bindersfor Sprayed Sealing and Hot Mixed Asphalt – page 2

aapa advisory note 7

Guide to the Heating and Storage of Binders for Sprayed Sealing

Note 1: Adjustments in temperature at the point of spraying may be required to allow for prevailing conditions, such as pavement temperatureand wind speed, but must not exceed 2000C. The listed temperature ranges apply to the binder before the addition of any cutteror other additive. For further information refer to Austroads 'Sprayed Sealing Safety Guide'.

Note 2: All polymer modified binders must be stirred prior to use and regularly circulated during storage due to possible polymer segregation.For storage of binders for periods longer than shown, refer to binder manufacturer.

Note 3: Longer storage times apply to lower storage temperatures.Note 4: Dilutions can be produced to meet S10E, S15E, S20E and S25E.Note 5: These products require continuous slow agitation during storage.Note 6: Dilution will meet S35E. continued on page 3

BINDER SEALING BINDER Austroads Binder Holding Temperature Medium-term SUPPLIER PMB Temperature (°C) Time at for Medium-term Storage Time

Grade at Point of Spraying Storage (days) Spraying (Note 1) Temperature (°C) (Notes 2 & 3)

BITUMEN TO AS2008 BP, Shell (WA only) Class 50 175 – 185 7 days 130 – 150 30 days All bitumen suppliers Class 170, Class 320 175 – 185 7 days 130 – 150 30 days

SPECIALTY SEALING BINDERS Bituminous Products Pty. Ltd. Bitulastic SBS S10E S10E 190 – 200 2 days 130 – 140 14 days

Bitulastic SBS S15E S15E 190 – 200 2 days 130 – 140 14 days Bitulastic SBS S20E S20E 190 – 200 2 days 130 – 140 14 days Bitulastic SBS S25E S25E 190 – 200 2 days 130 – 140 14 days Bitulastic SBS S30E S30E 190 – 200 2 days 130 – 140 14 days Bitulastic SBS S35E S35E 190 – 200 2 days 130 – 140 14 days Bitulastic Crumb S40R S40R 190 – 200 3 days 130 – 160 14 days Bitulastic Crumb S50R S50R 190 – 200 3 days 130 – 160 14 days Bitulastic Crumb S60R S60R 190 – 200 3 days 130 – 160 14 days

BP Australia Pty. Ltd. OLEXOBIT SP 180 – 190 1 day 120 – 160 60 – 7 days OLEXOBIT SAM S35E 180 – 190 1 day 120 – 160 60 – 7 days OLEXOBIT S15 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S30 S10E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S40 S15E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S45 S20E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S50 S20E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S60 S25E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S70 S30E 180 – 190 1 day 120 – 140 14 – 7 days OLEXOBIT S75 S30E 180 – 190 1 day 120 – 140 14 – 7 days MULTIBIT SBM 175 – 185 7 days 135 – 155 30 days

Mobil Oil Australia Ltd. Flexxipave 451E S15E 180 – 190 2 days 120 – 140 10 days Flexxipave 551E (All Dilutions) (Note 4)

S10E, S15E, S20E, S25E

180 – 190 2 days 120 – 140 10 days

Flexxipave 401 (Note 5) S40R 180 – 190 2 days (Note 5) 130 – 140 10 days (Note 5) Flexxipave 402 (Note 5) N/A 180 – 190 2 days (Note 5) 130 – 140 10 days (Note 5) Flexxipave 403 (Note 5) S45R 180 – 190 2 days (Note 5) 130 – 140 10 days (Note 5) Flexxipave 473E S35E 180 – 190 2 days 120 -160 90 – 7 days Flexxipave 573E (Dilution) S35E (Note 6) 180 – 190 2 days 120 -160 90 – 7 days Multipave 600/170 175 185 7 days 135 -155 30 days

Pioneer Road Services Pty. Ltd. Flexibit S25E S25E 185 – 195 1 day 140 – 160 10 – 7 days Flexibit S30E S30E 185 – 195 1 day 140 – 160 10 – 7 days Flexibit S10E S10E 180 – 190 2 days 140 – 160 10 – 7 days Flexibit S15E S15E 180 – 190 2 days 140 – 160 10 – 7 days Flexibit S20E S20E 180 – 190 2 days 140 – 160 10 – 7 days Flexibit SSR S35E 180 – 190 4 days 140 – 160 14 – 7 days

Disclaimer:Although the information contained in this Advisory Note is believed to be fundamentally correct, the Australian Asphalt Pavement Association does notaccept any contractual tortious or other form of liability for its contents or for any consequences arising from its use. Advice should be sought fromsuppliers prior to handling, applying or storing products outside the recommended ranges. Date of Issue: August 2003



Guide to the Heating and Storage of Binders for Sprayed Sealing

Note 1: Adjustments in temperature at the point of spraying may be required to allow for prevailing conditions, such as pavement temperatureand wind speed, but must not exceed 2000C. The listed temperature ranges apply to the binder before the addition of any cutteror other additive. For further information refer to Austroads 'Sprayed Sealing Safety Guide'.


Note 3: Longer storage times apply to lower storage temperatures.Note 4: Dilutions can be produced to meet S10E, S15E, S20E and S25E.

SERVICE CONDITION Note 1

A27RFA40R

RUTTING Very heavy High or Medium

RESISTANCE Low(Marginal Pavement)

Heavy All

RUTTING Very heavy High or Medium

RESISTANCE Low(Adequate Pavement)

Heavy All

FATIGUE Very heavy All

RESISTANCE High or Medium

Low

RUTTING & FATIGUEVery Heavy to Heavy

(Marginal Pavement) Medium

RUTTING & FATIGUE High or Medium(Adequate Pavement)

Low

OPEN High

GRADED Medium or Low

ASPHALT < Heavy All

Stone Mastic Asphalt Heavy All

A30PAPPLICATION

Heavy

All

A25E

Adequate Binder

Binder Class

Very Heavy to Heavy

Very Heavy to Heavy

Traffic Temperature C600/ 170

C1000/ 320 A15E A20E

continued on page 4

continued from page 2

Guide to the Selection of Asphalt Modified Binders

The Shell Co. of Australia Ltd. Multiphalte 600/170 175 – 185 7 days 135 – 155 30 days

Cariphalte S30E S30E 185 – 195 1 day 140 – 160 10 – 7 days Cariphalte S25E S25E 185 – 195 1 day 140 – 160 10 – 7 days Cariphalte S20E S20E 180 – 190 2 days 140 – 160 10 – 7 days Cariphalte S15E S15E 180 – 190 2 days 140 – 160 10 – 7 days Cariphalte S10E S10E 180 – 190 2 days 140 – 160 10 – 7 days Cariphalte S5E N/A 175 -185 3 days 140 – 160 10 – 7 days

BINDER SEALING BINDER Austroads Binder Holding Temperature Medium-term SUPPLIER PMB Temperature (°C) Time at for Medium-term Storage Time

Grade at Point of Spraying Storage (days) Spraying (Note 1) Temperature (°C) (Notes 2 & 3)

SAMI Pty. Ltd. Samiseal 3 S10E 175 – 185 2 days 120 – 140 14 days

Samiseal 4 S15E 175 – 185 2 days 120 – 140 14 days Samiseal 5 S20E 180 – 190 2 days 120 – 140 14 days Samiseal 6/7 S25E / S30E 185 – 195 2 days 120 – 140 14 days Samiseal 45R (Note 4) S45R 185 – 195 3 days (Note 4) 120 – 140 14 days (Note 4) Samiseal 50R (Note 4) S50R 185 – 195 3 days (Note 4) 120 – 140 14 days (Note 4) Samiseal PBD S35E 175 – 185 7 days 120 – 160 30 days Polyseal HSS S35E 175 – 185 14 days 120 – 160 30 days Polyseal SAM S35E 175 – 185 14 days 120 – 160 30 days



Guide to the Heating and Storage of Binders for Asphalt

Note 1: The temperature at the point of mixing and the holding time at mixing temperature refer to the binder prior to its introduction to themixing process. Adjustments to temperatures at the point of mixing may be required to allow for prevailing conditions such aspavement surface temperature, wind speed, asphalt mix type and haulage distance.


Note 3: Longer storage times apply to lower storage temperatures.

BINDER ASPHALT BINDER Austroads Binder Holding Time Temperature Medium-term SUPPLIER PMB Temperature (°C) at Mixing for Medium-term Storage Time

Grade at Point of Mixing Temperature Storage (°C) (Note 1) (Notes 2 & 3) (Notes 2 & 3)

BITUMEN TO AS2008 All bitumen suppliers Class 170, Class 320 140 - 165 14 days 130 - 150 30 days BP, Mobil, Shell Class 600 165 - 175 14 days 130 - 150 30 days

SPECIALTY ASPHALT BINDERS

Bituminous Products Pty. Ltd.

Bitulastic SBS A10E, A15E, A20E 160 - 170 4 days 130 -140 14 days

Bitulastic Gilsonite 160 - 170 30 days 160 - 175 30 days Bitulastic Crumb A40R A40R 190 - 200 3 days 130 - 160 14 days

Bitulastic A30P A30P 180 - 190 7 days 130 - 150 30 days

Bitulastic A35P A35P 180 - 190 7 days 130 - 150 30 days

BP Australia Pty. Ltd. OLEXOBIT ADG A25E 150 - 170 7 days 120 -160 60 - 7 days OLEXOBIT AOG A25E 150 - 160 7 days 120 -160 60 - 7 days

OLEXOBIT AB4 A20E 155 - 165 4 days 120 - 140 14 - 7 days

OLEXOBIT AB5 A15E 160 - 175 4 days 120 -140 14 - 7 days

OLEXOBIT AB6 A10E 160 - 175 4 days 120 -140 14 - 7 days

OLEXOBIT SMA A25E 150 - 170 7 days 120 - 160 60 - 7 days

MULTIBIT ABM 150 - 175 14 days 135 - 155 30 days

Mobil Oil Australia Ltd. Flexxipave 351E A15E 165 - 175 7 days 130 - 140 30 days

Flexxipave 352E A10E 165 - 175 7 days 130 - 140 30 days Flexxipave 452E A20E 165 - 175 7 days 130 - 140 30 days Flexxipave 204 A30P 160 - 175 14 days 140 - 160 30 days Multipave 600/170 160 - 175 14 days 135 - 155 30 days

Pioneer Road Services Pty. Ltd.

Flexibit A10E A10E 165 - 175 3 days 140 - 160 10 - 7 days

Flexibit A15E A15E 165 - 175 3 days 140 - 160 10 - 7 days Flexibit A20E A20E 165 - 175 3 days 140 - 160 10 - 7 days Flexibit A25E A25E 165 - 175 3 days 140 - 160 10 - 7 days Flexibit A30P A30P 160 - 175 30 days 140 - 160 10 - 7 days

Flexibit A35P A35P 160 - 175 30 days 140 - 160 10 - 7 days Flexibit ADR A25E 165 - 175 7 days 140 - 160 10 - 7 days

SAMI Pty. Ltd. Sealoflex U A20E 140 - 165 4 days 120 - 140 14 days

Sealoflex 2 A10E 165 - 175 4 days 120 - 140 14 days Samifalt AB6 A10E 165 - 175 4 days 120 - 140 14 days Samifalt 60 A15E 165 - 175 4 days 120 - 140 14 days Samifalt D A30P 160 - 175 30 days 120 - 160 30 days

Samifalt AB2 A35P 160 - 175 30 days 120 - 160 30 days Polyphalt HM A25E 160 - 175 30 days 120 - 160 30 days Polyphalt FR A25E 160 - 175 30 days 120 - 160 30 days

The Shell Co. of Australia Ltd.

Multiphalte 600/170 160 - 175 14 days 135 - 155 30 days

Multiphalte 1000/320 160 - 175 14 days 135 - 155 30 days

Cariphalte A20E A20E 165 - 175 4 - 3 days 140 - 160 10- 7 days Cariphalte A15E A15E 165 - 175 4 - 3 days 140 - 160 10- 7 days Cariphalte A10E A10E 165 - 175 4 - 3 days 140 - 160 10- 7 days

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:(#;/13%71;.'6?%@"67>#=@>'"6K<=>>'6?%(#;@>'@17%4"#%-25%71;.7G%&1@P6'@;.%)">1G%C=7>#";37%ALL8*

Q#;01R"#$%7(1@'4'@;>'"67%4"#%("./01#%0"3'4'13%S'631#7G%D1("#>%)"%C-T&L9G%C=7>#";37%ALLL*

Class of PMBPavementTemperature4

(°C)

Traffic(veh/lane/day

based on AADT) S15E S20ES25E

S35E S45RS50R5, 6

S55R5, 6

20 to 25 <1000≥1000

6-86

86-8

64

108

1210

26 to 32 <1000≥1000

4-64

64-6

42

8-106-8

10-128-10

33 to 38 <1000

≥100042

4-53-4

22

6-86

86-8

39 to 45 <1000≥1000

Min 2 Min 3 0-2 4-64-6

64-6

> 45 All Min 2 Min 3 0-2 Min 4 Min 5

March 2001 – Version 1 Page 1 of 6

AUSTROADS Modified Binder Test MBT 01:2001

Method of sampling polymer modified binders, polymers and crumb rubber

PREFACE

This Modified Binder Test Method was prepared by an APRG Working Group on behalf of AUSTROADS. Representatives of AUSTROADS, ARRB Transport Research and Industry through the Australian Asphalt Pavement Association (AAPA) have been involved in the development and review of this test method.

____________________

FOREWORD

Specification limits for polymer modified binders (PMBs) have been set on the basis of a representative sample taken at the point of delivery for use and reheated to enable testing in accordance with the test methods set out by AUSTROADS. The adoption of a uniform and practical sampling method will ensure consistent and reliably representative samples are obtained.

____________________

METHOD

1 SCOPE

This test method applies to polymer modified binders, polymers and crumb rubber. Materials are sampled according to this protocol to ensure that correct sampling procedures are followed and that test results provide the required information on consignment quality. The purpose of sampling is to enable subsequent testing to:

(a) Represent, as nearly as practicable, an average of a consignment or batch, or

(b) Detect any variation within a consignment or batch.

2 REFERENCED DOCUMENTS

The following documents are referred to in this test method:

Appendix 3

AUSTROADS MBT 01:2001


AUSTROADS

• MBT 02 Protocol for handling polymer modified binders in the laboratory

3 SAFETY PRECAUTIONS

Strict precautions shall be taken to avoid injury or fire at all times when handling hot bituminous materials, such as bitumen and polymer modified binders. Such precautions include, but are not limited to, the following requirements:

(a) Eye protection, such as safety glasses and/or face shields, shall be worn while sampling.

(b) Heat-resistant gloves, with close-fitting cuffs, and other suitable protective clothing, shall be worn while sampling and sealing containers.

(c) There shall be no smoking while sampling.

(d) Containers shall not be held in the hand while sampling and sealing. Tongs, or some other device, shall be used to hold the containers while the sample is being taken.

(e) The sampler shall, as far as practical, stand above and away from the sampling valve or outlet and on the windward side.

(f) The sample shall be taken slowly and carefully to prevent splashing of the material.

(g) The container shall be placed on a firm, level surface to prevent splashing, dropping or

4 SAMPLING PRECAUTIONS

The following sampling precautions shall be observed:

(a) Care shall be taken to prevent contamination of the samples with solvents, cleaning fluids, or different types of bituminous materials.

(b) Between sampling and testing, the sample shall not be transferred from one container to another if this involves reheating of the sample after cooling, except as specified in MBT 02.

(c) Where a tin is used, the sample container shall be tightly and positively sealed immediately after the sample is taken.

(c) The sample container shall not be submerged in solvent, nor shall it be wiped with a solvent-saturated cloth. Any spilled materials on the outside of the container shall be wiped with a clean dry cloth immediately after the container is sealed.

5 SAMPLE CONTAINERS



Containers for PMB samples shall be clean, dry, nominal 1 L or 2 L capacity, friction-top cans, unless otherwise specified. Dry polymers and crumb rubber samples may be placed in a closed plastic bag. Where the moisture content of a crumb rubber sample is to be determined, the sample shall be placed in a hermetically sealed container.

6 PROCEDURES

6.1 General

Sampling may be carried out at the point of loading, or at the point of delivery, as appropriate.

6.2 Sample size

The size of the sample shall be at least 1 L or 1 kg, unless otherwise specified.

6.3 Sampling of PMBs

(a) Sampling from bulk storage

The procedure shall be as follows:

(i) The material shall be thoroughly mixed and the sample drawn from a sampling cock in the side of the tank.

(ii) The initial material withdrawn (about 4 L) shall be discarded prior to collection of the sample. It is recommended that the product run-off and any product intended to be discarded be returned to the bulk product to avoid contamination of the environment.

(b) Sampling during loading


(i) When rail tankers, road tankers, sprayers or drums are being filled, the material shall be thoroughly mixed prior to loading. Sampling shall be carried out as the material flows through the pipeline.

(ii) When the material is being discharged under pressure, the sample shall be taken from the discharge line by a suitable sampling cock capable of providing a sufficient flow rate, or from the discharge end of a small filling line.

(iii) When the material is being discharged by flowing under gravity, either the procedure described in (ii) above shall be followed, if the pipeline has a rising section completely filled by the outflowing material and provided the pressure is sufficient, or sampling shall be carried out by taking containers-full of material from the outlet, if the pipeline is not completely filled, or the pressure is not great enough.

(iv) The sample shall be taken from near the middle of discharge.

(v) About 4 L of the initial material withdrawn in each increment shall be discarded. It is recommended that the product run-off and any product intended to be discarded be returned to the bulk product to avoid contamination of the environment.



(vi) The sample shall be transferred without delay to the sample container, allowing at least 5 percent ullage, and the container shall be immediately sealed after filling.

(c) Sampling from rail and road tankers


(i) The material shall be thoroughly mixed and the sample drawn from a sampling cock in the delivery line. The sample shall be taken near the middle of the discharge.

(ii) The initial material withdrawn (about 4 L) shall be discarded prior to collection of the sample. It is recommended that the product run-off and any product intended to be discarded be returned to the bulk product to avoid contamination of the environment.

(iii) Where there is no suitable sampling cock available, a sample shall be taken from near the top of the tanker by lowering a weighted sampling can or thief sampling can, as appropriate, into the material.

(iv) The sample shall be transferred without delay to the sample container, allowing at least 5 percent ullage, and the container shall be immediately sealed after filling.

(d) Sampling from sprayers


(i) The contents of the sprayer shall be thoroughly circulated for at least 15 minutes prior to sampling.

(ii) The sample shall be taken either from the spray bar, or by sampling cock, or by using a weighted can or thief sampling can, as appropriate.

(iii) The initial material withdrawn (about 4 L) shall be discarded prior to collection of the sample. It is recommended that the product run-off and any product intended to be discarded be returned to the bulk product to avoid contamination of the environment.

(iv) The sample shall be transferred without delay to the sample container, allowing at least 5 percent ullage, and the container shall be immediately sealed after filling.

(e) Sampling from drums


(i) A number of drums shall be selected at random, with the number being not less than the appropriate number shown in Table 1.

(ii) The contents of each drum selected shall be mixed thoroughly by turning end over end, rolling and stirring with a rod.

(iii) As the stirring rod is withdrawn, it shall be closely examined for the presence of extraneous matter.

(iv) The sample shall be collected by pouring, or by the use of a pump, or by thief sampling can.



(v) Where the material is known to be from a single production run or batch, the samples may be combined and thoroughly mixed to form a bulk sample, from which a sample of about 1 L shall be drawn for testing. In the case of a small consignment, the sizes of samples shall be increased as necessary to yield a combined sample of at least 1 L.

(vi) The consistency of each sample may be determined to detect variations in the material delivered.

6.4 Sampling of polymers and crumb rubber

(a) Sampling of liquids from drums


(i) A number of drums shall be selected at random, with the number being not less than the appropriate number shown in Table 1.

(ii) The contents of each drum selected shall be mixed thoroughly by turning end over end, rolling and stirring with a rod.

(iii) As the stirring rod is withdrawn, it shall be closely examined for the presence of extraneous matter.

(iv) The sample shall be collected by pouring, or by the use of a pump, or by thief sampling can.

(v) Where the material is known to be from a single production run or batch, the samples may be combined and thoroughly mixed to form a bulk sample, from which a sample of about 1 L shall be drawn for testing. In the case of a small consignment, the sizes of samples shall be increased as necessary to yield a combined sample of at least 1 L.

(vi) The consistency of each sample may be determined to detect variations in the material delivered.

(b) Sampling of solids from packs (drums, bags, or other containers)


(i) A number of packs shall be selected at random, with the number being not less than the appropriate number shown in Table 1.

(ii) From each pack, a sample not less than 100 g in mass shall be taken from at least 100 mm below the surface and at least 100 mm from the side of the pack.

(iii) Where the material is known to be from a single production run or batch, the samples may be combined and thoroughly mixed to form a bulk sample, from which a sample of about 1 L shall be drawn for testing. In the case of a small consignment, the sizes of samples shall be increased as necessary to yield a combined sample of at least 1 L.

(iv) The consistency of each sample may be determined to detect variations in the material delivered.



Table 1 - Number of samples

Number of drums or packs

in consignment

Number of drums or packs

to be sampled

1- 10 11 - 50 51 - 100 101 - 200 201 - 400 401 - 700 701 - 1000

Over 1000

1 2 4 5 6 7 8

8 plus 1 for each 500 drums or packs above 1000

7 LABELLING

Samples shall be securely packed for transport to the testing laboratory and shall be clearly identified by markings on the body and lid of the container. The following information shall be shown on the container, or label:

(a) Designation or classification of the material.

(b) Identification mark.

(c) Date and time of sampling.

(d) Sampling temperature.

(e) Further information required for identification of the samples shall be supplied on a separate sampling form. The additional information shall include the following:

(i) Name of supplier.

(ii) Place and date of sampling.

(iii) Quantity of material represented by the sample.

(iv) Type, batch number and identifying number of container, or vehicle, from which the sample was taken.

(v) Name of the sampler.

(vi) If the sampling procedure (especially temperature) was contrary to the manufacturer'srecommended procedure and/or industry guidelines.



(vi) If the sampling procedure (especially temperature) was contrary to the manufacturer's recommended procedure and/or industry guidelines.

March 2001 - Version 1 Page 1 of 10

AUSTROADS Modified Binder Test MBT 02:2001

Protocol for handling polymer modified binders in the laboratory

PREFACE

This test method was prepared by an APRG Working Group on behalf of the AUSTROADS. Representatives of AUSTROADS, ARRB Transport Research and the Australian Asphalt Pavement Association have been involved in the development and review of this test method.

____________________

FOREWORD

Polymer modified binders (PMBs) are heat-sensitive materials and may undergo significant changes to their properties as a result of exposure to high temperatures for extended periods where added polymer can be damaged and/or separate from the PMB dispersion. Improper heating of samples can, therefore, affect the properties of PMBs, resulting in sample test results which may not truly represent the characteristics of the original material.

Recent PMB testing experience, particularly with those binders formulated with SBS polymer at concentrations greater than 3 percent suggest that binder handling prior to testing can contribute significantly to measured binder performance. This laboratory handling protocols reflects the range of approaches to binder handling used in Australian laboratories and includes a reference protocol representing agreed best practice. Where SBS modified binders are tested it is strongly recommended that the reference protocol be adopted. This procedure is also recommended where two laboratories report conflicting results with any PMB.

It should also be noted that the estimates of precision reported by AUSTROADS and included in the 2000 release of the test methods were obtained on binders that were handled using the reference protocol. It is expected that testing precision associated with the other protocols will be degraded, particularly between laboratory reproducibility.

____________________

METHOD

1. SCOPE This test method is based on AS 2341.21 and applies to polymer modified binders (PMBs) which are to be tested in accordance with the test methods set out by AUSTROADS.

Appendix 4



2. REFERENCED DOCUMENTS The following documents are referred to in this test method:

AS 2341 Methods of testing bitumen and related road making products

2341.21 Method 21: Sample preparation

ASTM E 1 Standard specification for ASTM thermometers

AUSTROADS MBT 01 Method of sampling polymer modified binders, polymers and crumb rubber

3. PRINCIPLE The objective of this procedure is to ensure that PMB samples, when tested, are representative of the product used in the field. To achieve this, samples undergo a minimum and controlled amount of heating. Three methods have been adopted for heating the materials during sample preparation. Method one uses a hotplate in conjunction with a pre-heating oven and the second method uses a forced convection oven for the complete heating process. The third method uses a strict sample heating, mixing and subdivision protocol to ensure consistent inter-laboratory practices. Method three is described as the reference method and has been used to derive the measures of method precision where given, for various other AUSTROADS MBTs.

4. APPARATUS 4.1 Hotplate Method The items of apparatus are as follows:

4.1.1 Essential items The essential items of apparatus are as follows:

(a) Conditioning oven - able to maintain a temperature in the range 130 to 180°C with a setpoint accuracy of at least ± 5°C.

(b) Hotplate - able to maintain a surface temperature of no higher than 320°C, or 25 kW/m2 for hotplates with switched power settings.

(c) Pre-heating oven - able to maintain a temperature of 100 ± 10°C. May be fitted with a timer switch.

(d) Stirrer – Flat blade spatula, suitable for the containers used.

(e) Thermometer - conventional mercury-in-glass, partial immersion thermometer for hotplate use and oven monitoring, accurate to 0.5°C. A suitable thermometer is IP 61 C or ASTM 16C, as specified in ASTM E 1, for use at around 200°C.

(f) Mechanical Stirrer with paddle described in Appendix B

4.1.2 Optional items The optional items of apparatus are as follows:

(a) Beaker(s) - 400 mL to fit heating block (or equivalent container), with suitable lid.

(b) Heating block - aluminium block, approximately 150 mm diameter, 100 mm high, with a cavity able to accept 400 mL beakers with a clearance up to 0.5 mm.



(c) Thermoset hotplate - able to maintain a temperature in the range 135 - 180°C, with a setpoint accuracy of ± 5°C.

(d) Temperature Controller - An alternative to the temperature controlled hotplate is described in Appendix C. This system uses a modern oven temperature controller with Pt100 remote temperature sensor. Better temperature control is provided along with a direct temperature readout. No monitoring thermometer is required.

4.2 Oven Method The items of apparatus are as follows:

(a) Forced convection oven - able to maintain a temperature in the range 130 - 180°C, with a setpoint accuracy better than ± 5°C.

(b) Mechanical Stirrer with impeller described in Appendix B

(c) Stirrer – Flat blade spatula, suitable for the containers used.

(d) Temperature probe - a suitable probe based on a thermocouple or Pt100 used in conjunction with a corresponding readout device, with an accuracy of ± 2°C. Alternatively, a suitable thermometer (or equivalent) may be used.

4.3 Reference Method The items of apparatus are as follows:

(a) Forced convection oven - able to maintain a temperature in the range 130 - 180°C, with a setpoint accuracy better than ± 5°C.

(b) Mechanical Stirrer with impeller described in Appendix B

(c) Beaker(s) - 250 - 300 mL sub-sample containers (4 required for a 1 Litre sample)

5. PROCEDURES 5.1 General PMBs are complex mixtures of polymers and a variety of petroleum products. If handled in accordance with the directions of the suppliers, there should be no significant risk. The hazard of burns with PMBs is greater than with standard bitumens, due to the (normally) higher handling temperatures. It is recommended that notices, describing the action to be taken in the event of bitumen or PMB burns, should be displayed in the laboratory in the areas where bitumen, multigrade and PMBs are handled. A suitable warning could be as follows:

WARNING: HOT BITUMEN MULTIGRADE & PMBs CAN CAUSE BURNS

The following precautions should be taken when handling bitumen, multigrade or PMBs:

(a) Eye protection, such as safety glasses and/or face shields, shall be worn when handling hot bitumen, multigrade or PMBs.

(b) Heat-resistant gloves, with close-fitting cuffs, and other suitable protective clothing, shall be worn when handling hot bitumen, multigrade or PMBs.



(c) There shall be no smoking while handling hot bitumen, multigrade or PMBs.

(d) While the material is still cold, loosen the lid of the sample container (invert the can and warm the lid, if necessary), or punch a hole in the lid.

(e) Examine the cold sample for the presence of water. If water is thought to be present, drain most of it out, or blow with clean compressed air to evaporate the free water.

5.2 Sampling

(a) An original sample shall be obtained in accordance with the procedures set out in MBT 01.

Note 1 Samples taken from bulk storage, transport tankers, or during transfer from or into these vessels, shall be treated as original samples.

(b) If the original sample has just been taken and the viscosity is low enough, it can be reduced, after suitable stirring, into sub-samples. These smaller, sub-samples shall be re-heated only once prior to testing.

5.3 HOTPLATE METHOD When using a hotplate, the procedure should be conducted in a fume cupboard and shall be as follows:

(a) Sample reduction from bulk The procedure shall be as follows:

(i) Preheat the bulk sample to 100 ± 10°C in the oven.

Note 2 Heating times vary according to oven type, sample size and initial temperature. A minimum of 4 hours is generally required if the samples are larger than 4 L. Samples should not be heated for more than 10 hours at 100°C.

(ii) Place the sample on the hotplate and commence stirring without entraining air. Occasionally, scrape the sides and bottom of the container with the stirrer blade. When the sample is of a uniform consistency, replace the stirrer with the general purpose thermometer.

(iii) When the sample reaches 160°C, divide the bulk sample into sub-samples using smaller containers of 1 L, or less. Remove the bulk sample from the hotplate.

Note 3 At this stage, check the material for any unusual or unexpected physical properties, such as extreme fluidity, cutter odour, or high consistency. If the presence of cutter, or other volatile oil, is suspected, a thin film dish or RTFO treatment bottle may be poured at this stage for further testing (mass loss determination).



(b) Subsample preparation The procedure shall be as follow:

(i) Maintain the conditioning oven at 160°C.

(ii) Pre-heat any required moulds or other test containers as required by the MBT method.

(iii) Heat the subsample until it is 180°C. Heating can be done as follows:

Note 4 Since the measured properties of PMBs, particularly those modified with SBS polymer can be influenced by their thermal history prior to testing, it is preferable for the sample presented for subsample preparation to be at room temperature.

(A) Hotplate and heating block (temperature-controlled) Set the thermoset hotplate and heating block to the required temperature and heat the sample in the beaker, covered with a suitable lid. The sample may be left unattended during heating, but shall be stirred gently before pouring. Carry out the pouring or filling operation in Step (iv) within 30 minutes of the sample reaching temperature.

Note 5 When a mechanical stirrer is used, the impellor speed shall be maintained at a sufficiently low speed so as to avoid cavitation and consequent entrainment of air in the sample. See Figure B2 in Appendix B.

Note 6 When using the aluminium block, significant temperature differences can occur between the binder sample and the block and hotplate. For reasonable temperature maintenance, the sample temperature in the beaker should be monitored during a typical heating cycle.

(B) Hotplate (without temperature control) Heat the subsample(s) on the hotplate to the required temperature, while stirring constantly. Carry out the pouring or filling operation, as required in subsequent testing, within 5 minutes of the sample reaching the required temperature.

Note 7 Do not leave the container on the hotplate without stirring constantly. If the stirring is to be interrupted, transfer the container to a thermally insulating surface until stirring can be resumed.

(iv) Fill the test containers as required by the MBT method.

(v) Discard the heated subsample(s). Do not use them again, or pour them back into the bulk sample.



5.4 OVEN METHOD When using a forced convection oven, the procedure shall be as follows:


(i) Maintain the oven at 160°C.

(ii) Heat the bulk sample to 160°C, allowing sufficient time to reach this temperature. The temperature is checked using the temperature probe which can be inserted into the sample.

(iii) Remove the sample from the oven and thoroughly stir it for 30 seconds with a spatula without entraining air.

(iv) Divide the bulk sample into sub-samples using smaller containers of 1 L, or less. Remove the bulk sample from the oven.

Note 8 When using the Oven method the bulk sample should be cold before further sample reduction is undertaken. It is preferable that samples not be taken directly from a hot supply and further reduced while hot.

(b) Subsample preparation The procedure shall be as follows:

(i) Maintain the oven at a temperature of 180°C.

(ii) Heat the subsample(s) to 180°C. Note 9 Ensure the correct temperature is reached, using the temperature probe, or heat for

the minimum time as determined in Appendix A.

(iii) Remove the subsample(s) from the oven and stir with a mechanical stirrer and suitable paddle for 30 seconds without entraining air. Note 5

(iv) Fill the required test containers.

(v) Discard the heated subsample(s). Do not use again, or pour back into the bulk sample.

5.5 REFERENCE METHOD


(i) Maintain the oven at 160°C.

(ii) Heat the bulk sample (>2 L) to 160°C, allowing sufficient time to reach this temperature. The temperature is checked using the temperature probe , which can be inserted into the sample. Alternatively, the sample is heated for a minimum period, which has been previously established (according to Appendix A) as being required for the particular sample size being used.

Note 10 When using the Reference method the bulk sample shall be cold before further sample reduction is undertaken. It is essential that samples not be taken directly from a hot supply and further reduced while hot.

(iii) Remove the sample from the oven and thoroughly stir it for 30 seconds with a mechanical stirrer and suitable paddle without entraining air.



(iv) Divide the bulk sample into samples using 1 L containers. These samples can be further divided into sub-samples by the following procedure. Note 11 At this stage, check the material for any unusual or unexpected physical properties,

such as extreme fluidity, cutter odour, or high consistency.

Note 12 If the presence of cutter, or other volatile oil, is suspected, a thin film dish or RTFO bottle may be poured at this stage for further testing (mass loss determination).

(b) Subsample preparation The procedure shall be as follows:

(i) The binders should be provided in 1 L cans (approximately 900 mL net). Check the condition of the sample (water, etc.) and quantity prior to testing.

(ii) Set a forced convection oven to 180° and allow temperature to stabilise.

(iii) Heat the sample tin in the oven for 4 hours at 180°C ±5 °C.

(iv) Stir the contents of the tin with a mechanical stirrer and impeller for 30 seconds. Note 5.

(v) After the 30 second stir, quickly pour the binder into the four subsample containers.

(vi) Cover each sub-sample with foil and allow to cool to room temperature. Label the containers 1 to 4 (plus sample designation). Store the sub-samples at room temperature.

(vii) These sub-samples are now ready for re-heating and testing using the appropriate test methods.

6. REPORT The following information shall be reported:

(a) Sample history including the preparation method (b) The presence of fumes or cutter odour. (c) The presence of foaming. (d) Unusually high consistency.



APPENDIX A

(Normative)

HEAT-UP RATE OF SAMPLE IN FORCED CONVECTION OVEN

A1 GENERAL During the preparation of bulk samples for sub-sampling, the minimum time required for a bulk sample to reach 160°C must be known.

In preparing sub-samples for testing, the minimum time required for the particular size of container to attain the filling temperature must be known.

The procedure below shall be carried out, as required, for each size of container used during the forced convection oven sample preparation in this method.

A2 PROCEDURE The procedure shall be as follows:

(a) Insert a thermocouple into the sample as follows:

(i) Punch a hole through the lid of the container.

(ii) Fill the container with the sample and secure on the lid.

(iii) Allow the sample to cool until it is semi-solid.

(iv) Insert the temperature probe to half the sample depth and secure it.

(v) Cool the sample to room temperature.

(b) Set the oven to the required temperature, viz. 160°C when using bulk samples, or 180°C when using sub-samples.

(c) When the temperature has stabilised, place the sample in the oven on the shelf normally used for heating bitumen samples. Leave the temperature probe in place and close the door on the wire.

(d) Monitor the temperature with time and establish the minimum time required for the sample container to reach temperature.

(e) Remove the container, cool it to room temperature and repeat Steps (c) and (d). Note A1: Alternatively, a suitable thermometer can be used in place of the temperature probe.

Note A2: If the laboratory sometimes tests several samples at the one time, the above procedure should also be carried out with the monitored sample surrounded by bitumen-filled dummy containers.

Note A3: Glass beakers and metal containers with cut-off rims will require lids.

A3 RECORDING The following information shall be recorded:

(a) The time required for a particular size of bulk sample container to reach 160°C.

(b) The time required for subsample containers intended to be used to reach 180°C.



APPENDIX B

(Normative)

Mechanical Stirrer and Impeller

B1 GENERAL For sample mixing to be repeatable and reproducible between laboratories, the rotational speed, paddle design and sample container should be adequately defined. By defining the sample size at 1 Litre, and specifying the impeller the geometry of the system is established. The chosen system is described as a low shear rate mixer and is not intended to blend the polymer into the binder. Its purpose is to ensure a homogeneous system for well manufactured binders by overcoming any segregation which may have occurred in the original sample.

B2 EQUIPMENT DEFINITION For the 1997 PMB inter-laboratory precision exercise, a commercial paint stirrer (impeller) was chosen for its availability and simple design. Figure B1 describes the paddle and provides the important dimensions. This impeller (or its equivalent) is recommended. At the time of the precision exercise the paddle described was available from Kmart stores.

The mechanical stirrer is a general purpose laboratory stirrer with variable speeds. The combination of stirrer and paddle with an appropriate rotational speed ensures that during the stirring process, the surface of the sample will be on the verge of forming a vortex. The maintenance of this incipient vortex ensures adequate mixing without the entrapment of air into the sample. Figure B2 describes the ideal mixing condition.

50 mm

30 mm

Angle ~ 30 degrees

Shaft 6 mm diam 250 mm long

Vortex must not be turbulent at any stage in the stirring process. Speed of stirrer motor

adjusted to point short of air entrapment.

Figure B1. Impeller assembly (Informative)

Figure B2. Incipient Vortex



APPENDIX C

(Informative)

Electronic Temperature Controller

C1 GENERAL Sample heating using the temperature controlled hotplate, heating block and thermometer can be difficult to manage both in terms of control precision and temperature stability. The lack of a direct temperature measurement link between the sample and the hotplate is the primary cause of these deficiencies.

C2 EQUIPMENT Several electronic controller manufacturers have released cost effective modules for temperature control in a variety of application. These devices can be seen in recently manufactured laboratory ovens, MATTA test cabinets and Durability ovens and provide a high level of stability through the use of a Platinum resistance (Pt100) sensor. Other features are:

• Low noise (Zero crossing) power switching to eliminate interference with other laboratory equipment (computers etc.)

• Direct selection of program temperature set point

• Display of actual sample temperature to 0.1°C (can be calibrated to ensure precision).

• Long term stability

Although not commercially available, the arrangement presented in Figure C1 can be readily assembled. This module can be applied to a variety of temperature control applications and can serve as a temperature monitor without the using the control function.

180.0Temperature Controller

Hot Plate

Pt100 temperature sensor

Figure C1. Temperature Control Module and Hotplate Assembly

The Australian Asphalt Pavement Association is a non-profit organisationformed to promote the economic use of asphalt and bitumen bound productsbased on sound technical and commercial grounds.

Throughout its history, AAPA has maintained as its major objective thedissemination of technical knowledge aimed at continual improvement inasphalt technology.

AAPA Members include manufacturers of asphalt and other bitumen boundproducts, State Road Authorities, Local Government, pavement engineeringconsultants, material suppliers, plant and machinery manufacturers, pavingand sealing contractors and individuals interested in asphalt technology.

Level 2, 5 Wellington StreetKew Victoria 3101 AUSTRALIA

Telephone: (03) 9853 3595Fax: (03) 9853 3484E-mail: [email protected]: www.aapa.asn.au

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