This document specifies two methods for the determination of the specific surface area of types and grades of carbon black for use in the rubber industry: — method A: automatic gas chromatography method (carrier gas method); — method B: automatic volumetric method. Somewhat different results might be obtained from the two methods. The degassing procedure differs between method A and method B, and it is important to investigate the possibility of correcting the results by using standard reference blacks. The results might also differ from those obtained using the multipoint method specified in ISO 18852, which is the preferred method. These methods are not applicable to porous carbon blacks.

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This document specifies a general method for determining the aggregate size distribution (ASD) of silica by using a disc centrifuge according to the principle of sedimentation. As pre-stage the silica is de-agglomerated in water using strong ultrasonic power treatment. The method is used for precipitated silica.

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This document specifies methods of test for determining the main physical and chemical properties of sulfur used for compounding dry rubber. Several of these properties can be determined by more than one test method and the user can choose the most appropriate method following the description of the test method principles provided under the corresponding clauses. NOTE Typical levels for the relevant properties of sulfur for use as a rubber compounding ingredient are contained in Annex A, for information only.

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This document specifies a method for the determination of the light transmittance of the toluene extract from carbon black for use in the rubber industry, as a means of measuring the discolouration caused by the extractable matter. The light transmittance value provides an estimate of the degree of discolouration caused by the toluene-extractable matter present on the surface of the carbon black. This method might not be applicable to carbon blacks with a high extractable-matter content.

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This document specifies sampling and test methods for the determination of the general characteristics of organic chemicals such as accelerators, antidegradants (including wax) and vulcanizing agents (excluding peroxides).

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ISO 5435:2017 specifies a method for the determination of the tinting strength of carbon black relative to an industry tint reference black. The method is based on the use of five different commercial instruments. Other instruments can be used if the test results for the standard reference blacks are within the control limits given in ASTM D4821. NOTE The Densichron reflectometer and the Meeco Colormaster are no longer commercially available, but the procedures have been included for the benefit of those who still use these instruments.

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ISO 11236:2017 applies to a variety of substituted p-phenylenediamine antidegradants (PPDs) used in the rubber industry. The three general classes of PPDs are dialkyl, alkyl-aryl and diaryl, which are used to impart ozone resistance to rubber. The following test methods are of greatest significance in assessing the purity of production PPDs, and hence their suitability for use in rubber. They are specified in this document as follows: - determination of purity by gas chromatography (GC); - determination of purity by high-performance liquid chromatography (HPLC); - determination of ash; - determination of volatile matter.

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ISO 10638:2017 specifies a method using gas chromatography/mass spectrometry, for the identification of antidegradants in raw rubbers, latices, unvulcanized-rubber compounds and vulcanized-rubber products. It is applicable to the 31 types of antidegradant listed in Annex A. The method specified is qualitative and is not intended for quantitative analysis.

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ISO 6472:2017 establishes unambiguous abbreviated terms for commonly used rubber compounding ingredients of known, specific chemical composition.

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ISO 9298:2017 specifies the methods to be used for the evaluation of zinc oxide for use in the rubber industry. The analytical methods are applicable to all commercial zinc oxides, for example: - direct type (American process); - indirect type (French process); - other types produced by different chemical methods, i.e. precipitation and calcination. Zinc oxide can also be coated with organic materials, such as fatty acids, oil, wetting agents, etc., in order to improve the dispersion in rubber.

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ISO 15825:2017 specifies a method for determining the size distribution of carbon black aggregates, using a disc centrifuge photosedimentometer. This technique is based on the hydrodynamic behaviour of carbon black in a centrifugal field. The determination of the aggregate size distribution is important in the evaluation of carbon black used in the rubber industry.

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ISO 1437:2017 specifies a method for determining the water-wash sieve residue from regular, untreated carbon black for the rubber industry. It may not be applicable to oil-treated blacks because the oil could prevent proper wetting of the black by water.

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ISO 1304:2016 specifies methods for the determination of iodine adsorption number of carbon blacks for use in the rubber industry. Two titration methods are described: - method A: titration using a burette and starch as indicator; - method B: potentiometric titration with an automatic titrator. The iodine adsorption number is related to the surface area of a carbon black and is generally in agreement with the nitrogen surface area. However, it is significantly depressed in the presence of a high content of volatile or solvent-extractable materials; the iodine adsorption number therefore does not always provide a measure of the specific surface area of a carbon black. Ageing of carbon black can also influence the iodine number. In case of dispute, the preferred method is method B (potentiometric titration).

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ISO 11235:2016 specifies the methods to be used for the evaluation of sulfenamide accelerators: - MBTS: benzothiazyl disulphide; - CBS: N-cyclohexylbenzothiazole-2-sulfenamide; - TBBS: N-tert-butylbenzothiazole-2-sulfenamide; - DIBS: N,N'-diisopropylbenzothiazole-2-sulfenamide; - DCBS: N,N'-dicyclohexylbenzothiazole-2-sulfenamide; - MBS: N-oxydiethylenebenzothiazole-2-sulfenamide. NOTE Although MBTS is not a sulfenamide, it is the primary decomposition product of these accelerators and quantitatively determined by the method specified in 5.2. The analytical methods are applicable for most commercial sulfenamide accelerators: - sulfenamides of primary amines (type I); - sulfenamides of unhindered secondary amines (type II); - sulfenamides of hindered secondary amines (type III). The method (5.2) to determine purity by high performance liquid chromatography (HPLC) is the preferred method.

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ISO 8312:2015 defines stearic acid (including blends of stearic and palmitic acid) for use as a compounding ingredient in the rubber industry and specifies the test methods for describing its properties. Classification of stearic acid and stearic acid/palmitic acid blends according to iodine value and typical chemical and physical properties for such materials for use in the rubber industry are given in Annex L. Annex L is given for information only. In this International Standard, the atomic absorption spectrometric method is the preferred method.

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ISO 1126:2015 specifies methods for determining the loss on heating of carbon black for use in the rubber industry. This loss on heating is due primarily to loss of moisture, but traces of other volatile materials may also be lost. These methods are not applicable to treated carbon blacks which contain added volatile materials. One of the following three methods is used: - method 1: gravity-convection oven method; - method 2: moisture balance method; - method 3: infrared irradiation method (rapid method). Method 1 is the preferred method.

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ISO 1125:2015 specifies a method for determining the ash of all types of carbon black for use in the rubber industry.

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ISO 18852:2015 specifies a method for the determination of the nitrogen surface area (NSA) of carbon blacks and other rubber compounding ingredients, like silicas and zinc oxides, based on the Brunauer, Emmett and Teller (BET) theory of gas adsorption using a multipoint determination as well as the determination of the statistical thickness surface area (STSA), otherwise known as the external surface area. STSA, however, is not applicable to silica and zinc oxide. The method can also be used for verifying "single-point" procedures described in ISO 4652 and other standards.

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ISO 5794-2:2014 specifies the test formulation, equipment, procedure, and test methods for determining the physical properties of precipitated hydrated silica in a styrene-butadiene rubber mix.

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ISO/TR 16098;2012 specifies standard materials, standard test formulations, equipment and processing methods for evaluating the dispersion of reclaimed rubbers and reclaimed crumb rubbers in rubber mixes.

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Oil absorption number (OAN) is a measure of the ability of a carbon black to absorb liquids. This property is a function of the structure of the carbon black. Either dibutyl phthalate (DBP) or paraffin oil is acceptable for use with standard pelleted grades, including N‑series carbon blacks found in ASTM D1765, although OAN testing using paraffin oil on some speciality blacks and powder blacks might result in unacceptable differences as compared to OAN testing using DBP oil. While studies have shown the two oils to give comparable precision, paraffin oil offers the advantage of being non-hazardous. ISO 4656:2012 specifies a method using an absorptometer for the determination of the oil absorption number of carbon black for use in the rubber industry. The same method is used for the determination of the oil absorption number of compressed samples of carbon black. The procedure for the preparation of the compressed samples is described in an annex.

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ISO 14932:2012 specifies four methods for the determination of the content of the following groups of organic peroxides used as rubber vulcanizing agents. There are three titration methods and one using capillary gas-chromatography as given below. Titration method A for group a) peroxyketals: DTBPC: 1,1-Di(tert-butylperoxy)cyclohexane; DBPMC: 1,1-Di(tert-butylperoxy)-2-methylcyclohexane; DBPTC: 1,1-Di(tert-butylperoxy)-3,3,5-trimethylcylcohexane; DBPB: 2,2-Di(tert-butylperoxy)butane; BPV: Butyl-4,4-di(tert-butylperoxy)valerate. Titration method B for group b) diacylperoxides: Dibenzoyl peroxide; Di(2,4-dichlorobenzoyl) peroxide; Di(4-methylbenzoyl) peroxide. Titration method C for group c) diaralkyl and alkyl-aralkyl peroxides: Di(tert-butylperoxyisopropyl)benzene; Dicumyl peroxide; tert-Butyl cumyl peroxide. Capillary gas-chromatography for dialkyl peroxides: 2,5-Dimethyl-2,5-di(tert-butylperoxy)hexane.

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Carbon black for the rubber industry is generally pelletized to reduce dust and to improve handling and incorporation into polymers. Variations in pellet size distribution can affect dispersion in polymers, bulk handling, and conveying properties. ISO 8511:2011 specifies a method for the determination of the pellet size distribution of carbon black.

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ISO 5794-3:2011 specifies the test formulation, equipment, procedure and test methods for determining the physical properties of precipitated hydrated silica in a compound based on a blend of solution styrene-butadiene and butadiene rubber. The formulation can be regarded as a model compound for silica-based passenger car tyre treads.

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ISO 8942:2010 specifies two methods for the determination of the individual pellet crushing strength of carbon black for use in the rubber industry: method A: using pellets of size ranging from 1,4 mm to 1,7 mm; method B: using pellets of size 1 mm.

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ISO 28343:2010 specifies a method for the determination, by differential scanning calorimetry (DSC), of the glass transition temperature, Tg, of process oils used in rubber compounding.

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ISO 5794-1:2010 specifies methods of test for characterizing precipitated hydrated silica for use as a rubber compounding ingredient. A definition of precipitated hydrated silica is given.

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ISO 6209:2009 specifies a method for the quantitative determination of the solvent-extractable material in carbon black for use in the rubber industry. The method is applicable to all types of carbon black.

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ISO 1138:2007 specifies three methods for the determination of the total sulfur in all types of carbon black for use in the rubber industry: Method A, using an oxygen bomb calorimeter; Method B, using a combustion furnace; Method C, using an automatic analyser. With respect to safety aspects and test precision, it is preferable to use automatic systems. Classical chemical analysis (Method A and Method B) is acceptable if automatic equipment is not available.

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ISO 21869:2006 specifies the test methods to be used for magnesium oxide intended for use in the rubber industry as a stabilizer and vulcanizing agent.

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ISO 21870:2005 describes a method for quantitative determination of the loss on heating (pyrolysis) of carbon black due to the elimination of volatile materials other than those liberated when heating to 125 °C (ISO 1126). The method is applicable to carbon black for the rubber industry. It serves to assess the decomposition of functional groups and adsorbed substances (e.g. hydrocarbons) present on the surface of the carbon black.

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1.1 This International Standard specifies the methods to be used for the evaluation of natural calcium carbonate (chalk or limestone) ground to a dry powder for use in the rubber industry. NOTE 1 Classification of natural calcium carbonate according to fineness and chemical purity and typical physical and chemical properties for use in the rubber industry are given in informative annex D. NOTE 2 This International Standard does not cover calcium carbonates prepared by precipitation from solution. 1.2 There are two sets of analytical methods listed in this International Standard. In the body of the text (4.8.2 to 4.8.4), the traditional spectrophotometric methods are given; these are obsolescent, time-consuming and use a chlorinated solvent. It is recommended that these methods be phased out and replaced by the atomic absorption methods listed in annexes A, B and C.

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Describes a method for the determination of the fraction of a test portion of pelletized carbon black used in rubber industry that will pass through a sieve with 125 m nominal aperture size under specified conditions. Replaces the third edition.

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Specifies a method for the determination of the dust content of pelletized carbon blacks. Permits a differentiation to be made between micro-pellets and dust and is applicable to all pelletized carbon blacks for the rubber industry.

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Gives a method for the determination of the pour density of all types of pelletized carbonblacks for use in the rubber industry. Replaces the third edition which has been technically revised.

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Specifies procedures for the sampling of carbon black for use in the rubber industry, delivered in bulk, semi-bulk or packages.

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ISO 15825:2015 specifies a method for determining the size distribution of carbon black aggregates, using a disc centrifuge photosedimentometer. This technique is based on the hydrodynamic behaviour of carbon black in a centrifugal field. The determination of the aggregate size distribution is important in the evaluation of carbon black used in the rubber industry.

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This International Standard specifies four methods for the determination of the specific surface area of types and grades of carbon black for use in the rubber industry: — method A using the Ni‑Count‑1 apparatus (Clause 3); — method B using the Areameter apparatus (Clause 4); — method C using gas chromatography (Clause 5); — method D using the Monosorb surface-area analyser (Clause 6). Somewhat different results might be obtained from the four methods. The degassing procedure used differs from method to method, and it is important to investigate the possibility of correcting the results by using standard reference blacks. The results might also differ from those obtained using the multipoint method specified in ISO 18852, which is the preferred method.

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ISO 8332:2011 specifies methods of test for determining the main physical and chemical properties of sulfur used for compounding dry rubber. Typical levels for the relevant properties of sulfur for use as a rubber compounding ingredient are given in an annex.

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ISO/TS 16176:2011 specifies a method for determining the size distribution of carbon black aggregates dispersed in a liquid by means of a high-power ultrasonic device. The measurement is done with a disc centrifuge photosedimentometer. This technique is based on the hydrodynamic behaviour of carbon black in a centrifugal field. The determination of the aggregate-size distribution is important in the evaluation of carbon black used in the rubber industry.

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ISO 6472:2010 establishes unambiguous symbols and abbreviated terms for commonly used rubber compounding ingredients of known, specific chemical composition.

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ISO 10638:2010 specifies a qualitative method, using gas chromatography/mass spectrometry, for the identification of antidegradants in raw rubbers, latices, unvulcanized-rubber compounds and vulcanized-rubber products. It is applicable to 31 types of antidegradant. Users should note that the method specified is a qualitative one and is not intended for quantitative analysis.

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ISO 28641:2010 specifies sampling and test methods for the determination of the general characteristics of organic chemicals such as accelerators, antidegradants (including wax) and vulcanizing agents (excluding peroxides).

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ISO 5435:2008 specifies a method for the determination of the tinting strength of carbon black relative to an industry tint reference black. The method is based on the use of five different commercial instruments. Other instruments may be used if the test results for the standard reference blacks are within the control limits given in ASTM D 4821. NOTE The Densichron reflectometer and the Meeco Colormaster are no longer commercially available, but the methods have been included for the benefit of those who still use these instruments.

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ISO 3858:2008 specifies a method for the determination of the light transmittance of the toluene extract from carbon black for use in the rubber industry, as a means of measuring the discolouration caused by the extractable matter. The light transmittance value provides an estimate of the degree of discolouration caused by the toluene-extractable matter present on the surface of the carbon black. This method may not be applicable to carbon blacks with a high extractable-matter content.

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Oil absorption number (OAN) is a measure of the ability of a carbon black to absorb liquids. This property is a function of the structure of the carbon black. Either dibutyl phthalate (DBP) or paraffin oil is acceptable for use with standard pelleted grades, including N-series carbon blacks found in ASTM D 1765, although OAN testing using paraffin oil on some speciality blacks and powder blacks may result in unacceptable differences as compared to OAN testing using DBP oil. While studies have shown the two oils to give comparable precision, paraffin oil offers the advantage of being non-hazardous. ISO 4656:2007 specifies a method using an absorptometer for the determination of the oil absorption number of carbon black for use in the rubber industry. The same method is used for the determination of the oil absorption number of compressed samples of carbon black. The procedure for the preparation of the compressed samples is described in the standard.

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ISO 1437:2007 specifies a method for determining the water-wash sieve residue from regular, untreated carbon black for the rubber industry. It may not be applicable to oil-treated blacks because the oil could prevent proper wetting of the black by water.

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