A SYNOPSIS OFANALYTICAL PROCEDURES

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Imerys Graphite & Carbon

Imerys Graphite & Carbon, member of the Imerys Group, is the reference for innovative capability in the field of carbon-powder-based solutions: natural graphite and synthetic graphite powders, conductive carbon blacks, as well as silicon-carbon composites and water dispersions.High standards in terms employee health and safety, social behaviour and environmental responsibility are core values of the company, which is capturing opportunities by developing new products and applications, investing in assets & people, and growing its commercial presence worldwide.

Profitable company, part of Imerys, the world leader in mineral-based specialty solutions for industry, listed on the Paris stock exchange

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A STRONG COMPANY

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Analytical Procedures for TIMREX Graphite, Coke and C-NERGY Graphite

Analytical Standard Operating Procedures (SOPs) must comply with international (Interna-tional Organization for Standardization, ISO) or national (Deutsches Institut für Normung (DIN) norms whenever possible. Where no dedicated norms exist, analytical SOPs are derived from similar or compatible norms. Similarly, for calibration and verification, exist-ing international primary or secondary standards are used, where these standards do not exist, internal standards are in place.

The Imerys Graphite & Carbon product portfolio is well-established as most products have been on the market for decades. The specification values are derived from a mean sam-ple of lots, which includes lot-to-lot variations. The analysis performed on each individual product depends on the application field, therefore there is no overall screening test in place. It must be noted that the majority of products are globally distributed over a period of months, therefore statistical data derived from a series of supplied lots could produce insignificant values.

References:- ASTM MNL1: Significance of Tests for Petroleum Products (chapter Properties of Petroleum Coke, Pitch, and Manufactured Carbon and

Graphite)

Each single lot undergoes a series of tests to ensure the accomplishment of all requested characteristics, these values are then stated in a Certificate of Analysis (CoA). These analy-ses are performed on the mean sample of the lot, which is homogeneously collected over the whole lot during the packing step. For each lot the retention sample is stored for a minimum of 10 years. Graphite is supplied in powder form. Therefore, it must be consid-ered a bulk material.

Differing from gas and liquids, powders present a residual intra-lot inhomogeneity. Gases and liquids can be almost perfectly blended. Powders undergo several physical effects that avoid an effective homogenisation. Such effects depend mainly on the particle size distri-bution (PSD) as well as on the flowability of the product, which is also influenced by the equipment used, as well as the dimension (tons) of the lot itself. It is therefore possible to have single spot samples which deviate from the certified analytical value. Statistics on such values are only relevant when a large number of samples are collected for a given lot.

References:- ANSI/ASQ Z1.9-2003 SAMPLING PROCEDURES AND TABLES FOR INSPECTION BY VARIABLES FOR PERCENT NONCONFORMING

(former MIL-STD-414)

Ash is assessed by gravimetric loss. A low-walled ceramic crucible is heated to 800° C in a muffle furnace and cooled to room temperature in a desiccator. A sample of 10 g of dry powder (accuracy 0.1 mg) is weighed in a low-walled ceramic crucible. The powder is combusted at a temperature of 810° C (at least 8 h) until a constant weight is reached. The residual corresponds to the ash content and is reported as a percentage of the initial weight of the sample.

Note: Considering the moisture content of the sample is usually <0.5%, the values can be considered as

measured on a dry sample. Regarding temperature, it is important that it is above 750° C to allow the ignition

of the material to burn. ISO and ASTM normally have slightly different temperature ranges. It is important to

ensure complete combustion while ensuring sufficient material remains for the ash content to be accurately

weighted.

References:- ISO 1171 Solid mineral fuels -- Determination of ash- ISO 6245 Petroleum products -- Determination of ash- ISO 8005 Carbonaceous materials used in the production of aluminium -- Green and calcined coke -- Determination of ash content- DIN 51903 Prüfung von Kohlenstoffmaterialien - Bestimmung des Aschewertes - Feststoffe- ASTM C561 Standard Test Method for Ash in a Graphite Sample

FOREWORD

ASH CONTENT

SAMPLING AND CERTIFICATION

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Synthetic graphite undergoes a thermal process of more than 3000° C, which eliminates all impurities and volatiles. With such high purity products it is very difficult to directly measure the Carbon Content as well as the Fixed Carbon amount, due to the high level of precision required (at least a ratio of 0.01%). Therefore, the measurement process is based on Ash, which can be assessed with the necessary precision and the Fixed Carbon Content is calculated as the following: Carbon Content = 100% - Ash

Note: Synthetic graphite undergoes a thermal process exceeding 3’000°C, which eliminates all impurities and

volatiles. Due to the extremely high purity of Imerys products (E.g.: TIMREX® or C-NERGY™) it is very difficult

to measure the carbon content or fixed carbon directly, as this measurement requires a resolution of 1 to

100,000 (0.001%). Therefore, measurement is based on Ash content, assessed with the necessary precision

and the fixed carbon content is calculated as follows: Carbon Content = 100% - Ash

Alternative measurement systems used to evaluate Carbon Content below 99.5% are basically not suitable

to assess this characteristic of Imerys products.

References:- See Ash content

Water content is assessed by Coulometric Karl Fischer Titration. A sample of 1 g of powder (accuracy 0.1 mg) is placed in a vial and the vial is closed and heated up to 120° C. During the heating process the evaporated water is collected in a iodine-sulphur dioxide solution. The water content is determined by a coulometric titration of this solution and is reported as a percentage of the initial weight of the sample.

References:- ISO 760 Determination of water -- Karl Fischer method (General method) - ISO 12937 Petroleum products -- Determination of water -- Coulometric Karl Fischer titration method- DIN 51777-1 Prüfung von Mineralöl-Kohlenwasserstoffen und Lösemitteln; Bestimmung des Wassergehaltes nach Karl Fischer; Direktes

Verfahren- DIN 51777-2 Prüfung von Mineralöl-Kohlenwasserstoffen und Lösungsmitteln; Bestimmung des Wassergehaltes, nach Karl Fischer,

Indirektes Verfahren- ASTM E203 Standard Test Method for Water Using Volumetric Karl Fischer Titration

Trace elements are assessed by Spark Discharge in Argon (SD Ar) and Optical Emission Spectrometry (OES). A graphite powder sample is ground to a maximum particle size of 75 μm by means of a vibrated mill and then pressed into a pill. The sample-pill is placed onto the excitation stand of the spectrometer. Under argon atmosphere spark discharges generate an emission of light, which is collected by the spectrometer. From the collected emission spectrum the concentration of the different elements is calculated and then reported in ppm.

Note: ICP (Induced Coupled Plasma) is not well suited for the contamination measurement of graphite due

to the impossibility to leach contaminants inside of individual grains as well as carbides. Therefore, analysis

of such products using standard ICP delivers values which are at least an order of magnitude less than the

real value.

References:- DIN 51008 -1 Optische Emissionsspektrometrie (OES) - Teil 1: Begriffe für Systeme mit Funken und Niederdruckentladungen- K. Slickers, Automatic Emission Spectroscopy. Brühl Druck und Presshaus Giessen (D) (1992)- ASTM D5029 - 98(2009) Standard Test Method for Water Soluble in Activated Carbon

The crystalline structure is analysed by means of an X-ray powder diffraction (XRD). A graphite powder sample is ground to a maximum particle size of 75 μm with a vibrating mill and is then mixed with a silicon standard. The mix is then placed in the sample holder in a thin layer of approx. 150 μm. The sample is irradiated using a Cu(K) X-ray beam at dif-ferent angle, the diffracted beam is collected by a detector. The angular position of the peak maximum of the (002) and (004) reflection profiles are determined and the interlayer spacing (c/2) is calculated by applying the Bragg equation. The crystallite size is deter-mined by means of the Iwashita’s algorithm, developed for carbon materials, and then by applying the Scherrer’s equation. The calculated values are reported in nm.

Note: Both values should be considered as informative of the characteristics of the material. Many years of

experience have shown that, the crystallographic characteristics of the products are very stable, due to this

evidence analytic portion is usually guaranteed, but not shown on the CoA. In any case, the analysis is per-

formed on products throughout the year. The results of c/2 and Lc are expressed in nm (nanometer, 1x10-9 m)

CARBON CONTENT

INTERLAYER SPAC-ING C/2 AND CRYS-TALLITE SIZE LC

MOISTURE PER K.F.

TRACE ELEMENTS – (SD AR – OES)

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or in Å (Ångström, 1x10-10 m) as they represent real dimensions of a crystal and not fractions. Therefore,

neither of the crystallinity values are expressed as percentages (%) or similar expressions. The value of Lc

correlates with the level of crystallization: none (amorphous), low, medium, high, very high. Considering a

value as a limit for a pass/no-pass test does not make sense. The value of c/2 confirms that it is graphite.

Values deviating from the expected values would just confirm the evidence that all other parameters (PSD,

densities, purity, morphology, …) are totally different. Therefore, considering these value as specifications

does not make sense.

References:- ISO 20203 Carbonaceous materials used in the production of aluminium -- Calcined coke -- Determination of crystallite size of calcined

petroleum coke by X-ray diffraction- ASTM D5187 Standard Test Method for Determination of Crystallite Size - Lc of Calcined Petroleum Coke by X-Ray Diffraction- Klug and Alexander, X-Ray diffraction Procedures, John Wiley and Sons Inc., New York London (1967)- P. Scherrer, Göttinger-Nachrichten 2 (1918) S.98, - N. Iwashita, C. Rae Park, H. Fujimoto, M. Shiraishi and M. Inagaki, Carbon 42, 701-714 (2004).

The density is obtained by xylene displacement. Approx. 2.5 g (accuracy 0.1 mg) of powder is weighed in a pycnometer. Xylene is added under a vacuum. After a few hours under nor-mal pressure, the pycnometer is filled, conditioned and weighed. The density represents the ratio between the mass of graphite and the displaced volume of xylene. The values are reported in g/cm3.

Note: Xylene Density is the short definition of the Real Density and erroneously called Specific Gravity,

Specific Density or similar.

References:- ISO 8004 Carbonaceous materials for the production of aluminium -- Calcined coke and calcined carbon products -- Determination of -

the density in xylene -- Pyknometric method- ISO 9088 Carbonaceous materials used for the production of aluminium -- Cathode blocks and prebaked anodes -- Determination of the

density in xylene by a pyknometric method- DIN 51901 Prüfung von Kohlenstoffmaterialien - Bestimmung der Dichte nach dem Xylolverfahren - Fest stoffe - ASTM D5004 Standard Test Method for Real Density of Calcined Petroleum Coke by Xylene Displacement

This measure is carried out by measuring the adsorption-desorption isotherm of nitrogen on the surface of the material by means of the Brunauer-Emmet-Teller (BET) algorithm. A definite amount (accuracy 0.01 mg) of powder is weighed in a sample tube. Then the sample undergoes a series of heating and cooling, from the evolution of the pressure in the sample tube the amount of absorbed nitrogen during the different steps is calculated; from this data the specific surface is calculated and reported in m2/g.

References:- ISO 9277 Determination of the specific surface area of solids by gas adsorption -- BET method - ISO 15901-3 Pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption -- Part 3: Analysis of

micropores by gas adsorption- ASTM C1069 Standard Test Method for Specific Surface Area of Alumina or Quartz by Nitrogen Adsorption

The spring-back is measured by compacting the graphite powders. Approximately 5 g (ac-curacy 0.1 mg) of graphite powder is poured into a die, then the punch is inserted and the air is evacuated. The sample undergoes a compression cycle by which the height of the pill is collected under full pressure and after pressure released. The spring-back is the ratio between height difference and minimal height and is reported in %.

References:- ISO 4492 Metallic powders, excluding powders for hardmetals -- Determination of dimensional changes associated with compacting

and sintering- ASTM B331 Standard Test Method for Compressibility of Metal Powders in Uniaxial Compaction

This measure is performed using a Scott Volumeter. The sample is free flowing through a Scott Volumeter and is collected in a 1 in3 vessel and weighed to 0.1 mg accuracy. The measure is performed three times and the average value is used. The ratio of average weight to volume (16.39 cm3) is the Scott density and is reported in g/cm3.

Note: This measurement should be performed with a completely de-agglomerated sample. Therefore, a sam-

ple from a paper bag or a Bigbag are compact and will always present higher values. These values are indi-

cated as Scott Density (bagged) and the magnitude of the measure depends on the material itself as well as

on the sampling point and method. In addition, the values for Scott Density (bagged) are obtained by sampling

one or more bag. Therefore, they represent spot or mean-spot values rather than a mean sample.

XYLENE DENSITY

SPECIFIC SURFACE AREA BY B.E.T. NITROGEN ADSORPTION

SPRING-BACK

APPARENT DENSITY BY SCOTT

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Scott Density, as reported in CoA, is measured on a mean sample of loose material, collected during the

packaging process.

References:- ISO 3923-2 Metallic powders -- Determination of apparent density -- Part 2: Scott volumeter method - ASTM B329 Standard Test Method for Apparent Density of Metal Powders and Compounds Using the Scott Volumeter

Loose and Tapped densities are also called Bulk & Tap. These measures are performed using a graduated cylinder and a tapping unit. 100 g (accuracy 1 mg) of dry graphite powder is carefully poured into a graduated cylinder. The loose volume is recorded, then the cylinder is fixed on the tapping machine and the tapping cycle is started, at the end the tapped volume is recorded. Both densities are calculated and reported in g/cm3.

Note: Loose/Tap density for fine graphitic powders is impossible to be measured. The sample adheres to the

wall of the measuring cylinder and during the tapping procedure it tends to fly away rather than stay com-

pacted together. Applying weight to the sample is ineffective, because the material will then be compacted

creating some artifacts. Density for fine graphitic powders are measured by means of the Scott method.

References:- ISO 567 Coke -- Determination of bulk density in a small container- ISO 787-11 General methods of test for pigments and extenders -- Part 11: Determination of tamped volume and apparent density after

tamping- ISO 3953 Metallic powders -- Determination of tap density- ISO 10236 Carbonaceous materials for the production of aluminium -- Green coke and calcined coke for electrodes -- Determination of

bulk density (tapped)- DIN 51705 Prüfung fester Brennstoffe - Bestimmung der Schüttdichte- DIN 51916 Prüfung von Kohlenstoffmaterialien - Bestimmung der Stampfdichte - Feststoffe- DIN 51918 Prüfung von Kohlenstoffmaterialien - Bestimmung der Rohdichte und der offenen Porosität

The measurement is performed by pressing a powder sample into a die and measur-ing mass and volume of the resulting specimen. About 40 g (accuracy 0.01 g) of graphite powder is poured into a die. Then a punch inserted and a compression force is applied. After the compression cycle, the specimen is weighed (accuracy 0.1 mg) and the volume calculated by the external masses (accuracy 1 μm3). The pressed density is the ratio of the mass to the volume and is reported in g/cm3.

References:- ISO 2738 Sintered metal materials, excluding hardmetals -- Permeable sintered metal materials -- Determination of density, oil content

and open porosity- ISO 3369 Impermeable sintered metal materials and hardmetals -- Determination of density- ISO 14427 Carbonaceous materials used in the production of aluminium -- Cold and tepid ramming pastes -- Preparation of unbaked test

specimens and determination of apparent density after compaction- DIN 51918 Prüfung von Kohlenstoffmaterialien - Bestimmung der Rohdichte und der offenen Porosität- DIN 51925 Prüfung von Kohlenstoffmaterialien - Herstellung von Probekörpern aus kohlenstoffhaltigen Stampfmassen und Bestimmung

ihrer Rohdichte - Binde- und Imprägniermittel- ASTM B962 Standard Test Methods for Density of Compacted or Sintered Powder Metallurgy (PM) Products Using Archimedes’ Principle

A laser beam lights up a cell which contains the sample of graphite suspended in water, the generated diffraction pattern is collected by the system and interpreted by Mie light scattering theory. The particle size distribution is calculated and reported in μm for the three quantiles: 10% (d10), 50% (d50) and 90% (d90).

Note: In laser Diffraction Measurement the Maximal diameter (Dmax) is irrelevant. By increasing the diam-

eter the cumulative percentage of the distribution becomes asymptotic towards 100%, but it will never be

100%. In other words Dmax will correspond to an infinite diameter. Please note, that is intrinsic to each Laser

Diffraction Instrument independently from model and producer.

References:- ISO 8130 -13:2001 Coating powders -- Part 13: Particle size analysis by laser diffraction- ISO 13320 Particle size analysis -- Laser diffraction methods- ISO 14887 Sample preparation -- Dispersing procedures for powders in liquids- ASTM D4464 Standard Test Method for Particle Size Distribution of Catalytic Material by

Laser Light Scattering- ASTM E1458 Standard Test Method for Calibration Verification of Laser Diffraction Particle Sizing Instruments Using Photomask Reticles- ASTM E2651 Standard Guide for Powder Particle Size Analysis

PRESSED DENSITY

LOOSE AND TAPPED DENSITIES

PARTICLE SIZE DISTRIBUTION BY LASER DIFFRACTION

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The measure is performed using a pile of sieves with descending mesh size on a sieving machine. 100 g (accuracy 0.01 g) of graphite sample is poured onto the top screen, then a vibration cycle is started. The residue on the screens and in the bottom pan is weighed and the particle size distribution (PSD) is calculated and reported in %.

Note: Extreme values, such as 0% or 100%, are insignificant. The sensitivity and precision of the method

present uncertainty, which in the best case is around ± 0.05%. Additionally, oversized particles will always be

present in the product. Vibrating sieving is suitable for the measurement of PSD, for PSD-tails and Oversize

assessment are more reliable Air-Jet-Sieving and Wet-Sieving, respectively.

References:- ISO 1953 Hard coal -- Size analysis by sieving- ISO 4497 Metallic powders -- Determination of particle size by dry sieving- DIN 51938 Prüfung von Kohlenstoffmaterialien; Bestimmung der Korngrößenverteilung durch Sieben; Feststoffe- DIN 66165-2 Partikelgrößenanalyse; Siebanalyse; Durchführung- ASTM D4749 Standard Test Method for Performing the Sieve Analysis of Coal and Designating Coal Size- ASTM E2651Standard Guide for Powder Particle Size Analysis- ASTM MNL32 Manual on Test Sieving Methods- ASTM STP447A Manual on Test Sieving Methods

The measurement is performed using a single sieve, through which air flow keeps the powder in constant movement and transports the fine particles through the screen. 20 g (accuracy 0.01 g) of a graphite sample is inserted into a sieve of desired mesh size and the sieving cycle is then started. The residue on the screen is then weighed and the fraction is calculated and reported in %.

Note: Extreme values, like 0% or 100%, are insignificant. The sensitivity and precision of the method present

uncertainty, which in the best case is around ± 0.05%. Additionally, oversized particles will always be present

in the product. Vibrating sieving is suitable for the measurement of the PSD, for PSD-tails and Oversize as-

sessment are more reliable Air-Jet-Sieving and Wet-Sieving, respectively.

References:- ASTM D5158-98(2005) Standard Test Method for Determination of Particle Size of Powdered Activated Carbon by Air Jet Sieving

The measure is performed using a single sieve, through which water flow transports the fine particles through the screen. About 1 g of graphite powder (accuracy 0.1 mg) is dispersed in 500 ml water. In order to achieve complete de-agglomeration a wetting agent is added. The dispersion is poured in the wet sieving unit holding a pre-weighted sieve. Then the equip-ment runs and is rinsed for 10 min with running tap water. The sieve is removed, dried and weighed. The amount of particles on the screen is determined and the fraction is calculated and reported in %.

Note: Extreme values, like 0% or 100%, are insignificant. The sensitivity and precision of the method present

uncertainty, which in the best case is around ± 0.05%. Additionally, oversized particles will always be present in

the product. Vibrating sieving is suitable for the measurement of the PSD, for PSD-tails and Oversize assessment

are more reliable Air-Jet-Sieving and Wet-Sieving, respectively.

References:- ISO 787-18 General methods of test for pigments and extenders -- Part 18: Determination of residue on sieve -- Mechanical flushing procedure- ISO 23202:2006 Aluminium oxide used for the production of aluminium -- Determination of particles passing a 20 micrometre aperture sieve- ISO 24369 Fine ceramics (advanced ceramics, advanced technical ceramics) -- Determination of content of coarse particles in ceramic powders by wet sieving method

- DIN 66165-2 Partikelgrößenanalyse; Siebanalyse; Durchführung- ASTM C925 Standard Guide for Precision Electroformed Wet Sieve Analysis of Nonplastic Ceramic Powders

The pH is measured using a Digital pH Meter with a calibrated pH electrode. The clean electrode is immersed in liquid. After stabilization, pH reading is recorded.

Note: pH is usually measured as a control value of the cleanliness of chemical purified Graphite. Therefore,

as no chemical step is applied in synthetic graphite production similar measurements are irrelevant. For some

special applications it may be helpful to know the interaction of the material with water.

References:- ISO 10390:2005 Soil quality - Determination of pH- ASTM D3838 - 05 Standard Test Method for pH of Activated Carbon- ASTM D5029 - 98(2009) Standard Test Method for Water Solubles in Activated Carbon

PARTICLE SIZE DISTRIBUTION BY VIBRATION SIEVES

PARTICLE SIZE BY AIR JET SIEVING

OVERSIZE BY WET SIEVING

PH VALUE

8

Analytical Standard Operating Procedures (SOPs) must comply with international (Interna-tional Organization for Standardization, ISO) or national (Deutsches Institut für Normung (DIN) norms whenever possible. Where no dedicated norms exist, analytical SOPs are derived from similar or compatible norms. Similarly, for calibration and verification, exist-ing international primary or secondary standards are used, where these standards do not exist, internal standards are in place.

The solid content is measured using a Halogen Moisture Determination thermobalance. About 2 g of the dispersion is placed on the sample holder and dried at 120° C until a con-stant weight is achieved. The remaining weight is recorded and expressed as a percent-age.

References:- ISO 248-2 Rubber, raw -- Determination of volatile-matter content -- Part 2: Thermogravimetric methods using an automatic analyser

with an infrared drying unit- ASTM D5368-13 Standard Test Methods for Gravimetric Determination of Total Solvent Extractable Content (TSEC) of Solid Waste

Samples- ASTM E2402-11 Standard Test Method for Mass Loss and Residue Measurement Validation of Thermogravimetric Analyzers

The water content is measured by weight difference between before and after drying cycles at 120° C. About 50 g (accuracy 0.1 mg) of powder is weighed in a glass beaker and dried at 120°C until constant weight is reached (at least 8 h). The weight loss corresponds to the water content and it is expressed as a %.

References:- DIN 51718 Prüfung fester Brennstoffe - Bestimmung des Wassergehaltes und der Analysenfeuchtigkeit- DIN 51904 Prüfung von Kohlenstoffmaterialien - Bestimmung des Wassergehaltes – Feststoffe- ASTM C562 Standard Test Method for Moisture in a Graphite Sample- ASTM D4959 Standard Test Method for Determination of Water (Moisture) Content of Soil By Direct Heating

Viscosity is measured in a steady state as a function of the shear rate as well as in oscillating mode as a function of the amplitude with a constant frequency. Thixotropic behaviour is meas-ured by observing the viscosity in an oscillating test as a function of the time. A rotational rheometer with a cone-plate setup is used and the measurements are performed at room temperature. About 2 g of liquid sample are put in the gap between a stationary plane and a rotating cone. A laminar flow of layers is created. The viscosity is obtained from measuring the internal resistance and a flow curve is obtained.

References:- ISO 2555 Plastics -- Resins in the liquid state or as emulsions or dispersions -- Determination of apparent viscosity by the Brookfield

Test method- ISO 3219 Plastics -- Polymers/resins in the liquid state or as emulsions or dispersions -- Determination of viscosity using a rotational

viscometer with defined shear rate- ISO 6388 Surface active agents -- Determination of flow properties using a rotational viscometer- DIN 51810-1 Prüfung von Schmierstoffen - Bestimmung der Scherviskosität von Schmierfetten mit dem Rotationsviskosimeter - Teil 1:

Messsystem Kegel/Platte- DIN 51810-2 Prüfung von Schmierstoffen - Prüfung der rheologischen Eigenschaften von Schmierfetten - Teil 2: Bestimmung der

Fließgrenze mit dem Oszillationsrheometer und dem Messsystem Platte/Platte- DIN 53019-1 Viskosimetrie - Messung von Viskositäten und Fließkurven mit Rotationsviskosimetern - Teil 1: Grundlagen und Messge-

ometrie- DIN 53019-2 Viskosimetrie - Messung von Viskositäten und Fließkurven mit Rotationsviskosimetern - Teil 2: Viskosimeterkalibrierung und

Ermittlung der Messunsicherheit- DIN 53019-3 Viskosimetrie - Messung von Viskositäten und Fließkurven mit Rotationsviskosimetern - Teil 3: Messabweichungen und

Korrektionen- ASTM D2196 Standard Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) Viscometer- ASTM D7867-13 Standard Test Methods for Measurement of the Rotational Viscosity of Paints, Inks and Related Liquid Materials as a

Function of Temperature- ASTM D2983-09 Standard Test Method for Low-Temperature Viscosity of Lubricants Measured by Brookfield Viscometer1, 2

The pH is measured using a Digital pH Meter with a calibrated pH electrode. The clean electrode is immersed in the liquid. After stabilization of the reading the pH is recorded.

References:- ISO 10390:2005 Soil quality - Determination of pH- ASTM D3838 - 05 Standard Test Method for pH of Activated Carbon- ASTM D5029 - 98(2009) Standard Test Method for Water Soluble in Activated Carbon

Analytical procedures for TIMREX® Dispersions

FOREWORD

SOLID CONTENT

MOISTURE

VISCOSITY

PH VALUE

9

Analytical Procedures for ENSACO®, SUPER P® and C-NERGY™ Conductive Carbon Black

A platinum crucible is ignited for 1 h at 550° C ± 25° C in a muffle furnace. An adequate amount of carbon black is dried at 125° C for 1 h. A sample of ± 10 g of the dried carbon black is weighed into the crucible and placed in the muffle furnace for 16 h at 550° C. The residue corresponds to the ash content. It is expressed as a percentage of the initial weight of the dried sample.

References:- ASTM D1506

The residue obtained after the determination of the ash content is dissolved in an acid mixture and transferred to a volumetric flask and diluted to the 100 ml mark. Metal impu-rities are analyzed by atomizing the liquid into the Argon plasma of an ICP analyzer and determining the different components by using a spectrophotometric technique.

References:- IMERYS method

A sample of 2 g of carbon black (accuracy 0.1 mg) is placed in a dried weighing bottle.The bottle is heated for 1 h at 125° C together with a stopper. The heating loss is expressed as a percentage of the initial weight of the sample.

References:- ASTM D1509 (method A)

A suitable amount of pre-dried (125° C) sample is weighed in a proper vessel and placed in-side a nitrogen flushed tubular furnace. The furnace is heated up to 950° C for 30 minutes. After cooling in a nitrogen atmosphere, the loss of weight of the sample is determined and expressed as a percentage of the initial weight of the sample. Afterwards, a blank deter-mination is carried out in the same way on the treated sample, and the result subtracted.

References:- IMERYS method

Carbon black is burned in a tube furnace at a minimum operating temperature of 1350° C in a stream of oxygen to oxidize the sulfur. The gas stream is passed through a cell in which sulfur dioxide is measured by an infrared (IR) absorption detector. The result is expressed in percent.

References:- ASTM D1619

This analysis is based on solvent (toluene) extraction of an adequate amount of dried (at 125° C for 1 h) carbon black. Extraction time is 48 h (or other time if specified). After extrac-tion the solvent is evaporated from the residue until constant weight. A blank determina-tion on the solvent is also performed. The result is expressed as a percentage of the initial weight of the sample.

References: - ASTM D4527

A sample of 1.5 g of carbon black is dispersed in distilled water with the aid of a few drops of acetone and of an alternating stirring and ultrasonic treatment. Then the pH electrode is placed in the stirring slurry and after a stabilization time of 2 minutes the pH value is recorded to the nearest 0.05 units.

References:- ASTM D1512 (method B)

ASH CONTENT

METAL IMPURITIES

HEATING LOSS (MOISTURE)

VOLATILE MATTER

SULFUR CONTENT

SOLVENT EXTRACTABLE

PH VALUE

10

Paraffin oil is added by means of a constant rate burette to a dried (1 h at 125° C) carbon black sample in the mixer chamber of the absorptometer. As the sample absorbs the oil, the mixture changes from a free-flowing state to one of a semi-plastic agglomeration, with an accompanying increase in viscosity. This increased viscosity is transmitted to the torque-sensing system. When the viscosity reaches a predetermined torque level, the absorptometer and burette will shut off simultaneously. The volume of the added oil is read from the burette. The volume of oil per unit mass of carbon black is the oil absorption number.

References: - ASTM D2414

A sample of carbon black is compressed 4 times at a pressure of 165 MPa and is then tested in an absorptometer to determine the oil absorption number according to method ASTM D2414. The difference between the initial OAN number and the OAN number of the compressed sample reflects the stability of the structure of the carbon black.

References: - ASTM D3493

This test determines the amount of liquid (10% of acetone in water) which can be ab-sorbed by 5 g of carbon black. The carbon black is placed in a 500 ml Erlenmeyer flask. While shaking vigorously with a rotating motion, small quantities of liquid are added to the carbon until finally one ball is formed. At first, this ball is fragile and breaks when shak-ing but at the end the ball resists to fairly vigorous shaking without disintegrating. The quantity of liquid added during this time is determined and the test is expressed as ml/5 g.

References: - IMERYS method

This test determines the amount of liquid (2N hydrochloric acid) which can be absorbed by 5 g of carbon black. The method used is the Japanese test JIS K 1469:1984 whose proce-dure is rather similar but less practical than the one used in the AS Test method.

References: - JIS K 1469:1984

A sample of carbon black is washed with water through a sieve of 45 μm or 20 μm until only coarse particles remain on the sieve. This residue is dried, weighed and the amount of residue is expressed as mg/kg (ppm) of the original sample.

References: - ASTM D1514

50 g of carbon black is weighed onto two 0.125 mm sieves, each with a receiver beneath and the assembled stack is placed into a Ro-Tap sieve shaker. After shaking for 3 minutes the carbon in the receivers is weighed to the nearest 0.1 g. The result is expressed as a percent.

References: - ASTM D1508

From a height of max. 50 mm above the rim, carbon black is poured in excess into the center of a tared cylindrical container with a volume of 624 ml. The surface is leveled with a single sweep and the filled container is weighed to the nearest 0.1 g. The calculated result is expressed in g/l.

References: - ASTM D 1513

OIL ABSORPTION NUMBER

OIL ABSORPTION NUMBER OF A COMPRESSED CARBON BLACK SAMPLE

ABSORPTION STIFFNESS (AS TEST)

HYDROCHLORIC ACID ABSORPTION NUMBER

GRIT

FINES

POUR DENSITY OF GRANULATED CARBON BLACK

11

The method covers the determination of the total surface area by the Brunauer, Emmet, and Teller (BET NSA) theory of multilayer gas absorption behavior. Following the model proposed by Brunauer, Emmet and Teller (BET), the monolayer capacity can be deter-mined. Based on the cross-sectional area of the nitrogen molecule, the monolayer capac-ity and the weight of the sample, the total surface area can be calculated. The result is expressed in m2/g.

References: - ASTM D3037-89

A carbon black sample of 0.5 g is placed between two copper electrodes in a nonconduc-tive mould and compressed by means of a pneumatic driven piston at pressures of 50 kg/cm2 and 100 kg/cm2 respectively. The electrical resistance and the thickness of the carbon black are measured at the two pressures and the electrical resistivity is calculated and expressed in ohm x cm.

References: - IMERYS method

In a Brabender roller mixer of 50 ml the HDPE is melted at 160° C for 2 minutes at a rotating speed of 60 rpm. Then the carbon is added and the compounding continues for 5 minutes. The compound plate(s) is(are) pressed at 180° C for 2 minutes applying a force of 200 kN. The measurement uses 10 samples of polymer/carbon black compounds with thickness of about 2 mm, having a minimum length of 4 cm and a width of +/- 2 cm. Each sample is measured by using a 4 point contacts method in a sample holder respecting ASTM D4496. The electrical resistivity of the compound is the average of the 10 resistivities calculated from the electrical resistances of the samples and their geometrical shapes. If the resist-ance of the sample or the contact resistances are larger than +/- 1010 ohm the measure-ment is performed with an electrometer with respect to ASTM D257. In this case the sample should have a minimum diameter of 6.5 cm.

References: - IMERYS method

TOTAL SURFACE AREA BY BET

SPECIFIC ELECTRICAL RESISTANCE

VOLUME RESISTIVITY

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