83.060 - Rubber

This document describes a method for the determination of the viscosity and stress relaxation of raw or compounded rubber under specified conditions. The viscosity determination consists of a constant strain, temperature and frequency test in which the elastic and the loss components of the complex shear modulus can be determined. The determination of stress relaxation consists of a constant static strain and temperature test in which the torque decrease can be determined.

This document establishes a framework for the characterization of physical and chemical properties of tyre and road wear particles (TRWP) using published analytical standards. It is applicable to laboratory-generated TRWP and TRWP collected in the environment. NOTE This framework focuses primarily on published International Standards, but also includes standards published by other entities such as ASTM and AFNOR. A brief summary and justification for each standard required to characterize the physical and chemical properties of interest are provided.

This document specifies the principles and procedures for estimating the thermal endurance of rubbers from the results of exposure to elevated temperatures for long periods. Two approaches are specified (see Introduction): — one using the Arrhenius equation; — the other using the WLF equation. In this document, the estimation of thermal endurance is based solely on the change in selected properties resulting from periods of exposure to elevated temperatures. The various properties of rubbers change at different rates on thermal ageing, hence comparison between different rubbers can only be made using the same properties.

This document specifies a method of thermal analysis of vulcanized rubber by differential scanning calorimetry (DSC). This method is intended for the observation and measurement of various properties and phenomena associated, such as physical transitions (glass transition, melting and crystallization, polymorphic transitions, etc.).

This document specifies a quantitative method, using proton (1H) nuclear magnetic resonance (NMR) spectrometry, for the determination of epoxidation and ring opening level of raw epoxidized natural rubber (ENR). This method applies to ENR of all grades available commercially.

This document specifies the physical and chemical requirements of epoxidized natural rubber (ENR) based on the epoxidation level of the natural rubber.

This document specifies: — physical and chemical tests on raw rubbers; — standard materials, standard test formulations, equipment, and processing methods for evaluating the vulcanization characteristics of emulsion- and solution-polymerized styrene-butadiene rubbers (SBRs), including oil-extended rubbers. It applies to those rubbers listed in Table 1 which are normally used in vulcanized form.

This document specifies four methods for the quantitative determination of the material extractable from raw rubbers, both natural and synthetic; two of the methods are also applicable to the unvulcanized and vulcanized rubber compounds. Method A measures the mass of the solvent extract, after evaporation of the solvent, relative to the mass of the original test portion. Method B measures the difference in the mass of the test portion before and after extraction. Method C, which is for raw rubbers only, measures the difference in the mass of the test portion before and after extraction using boiling solvent. Method D, which is for raw rubbers only, measures the difference in the mass of the test portion before and after extraction relative to the mass of the original test portion. NOTE 1 Depending on the test method used, the conditioning of the test portion and the solvent used, the test result is not necessarily the same. NOTE 2 Method C generally gives results which are lower than those obtained with methods A and B due to an equilibrium which is set up, particularly if large test portions are used, depending on the content and the nature of the extractable matter. Method C is, however, a quicker method than method A or method B. NOTE 3 Methods C and D are not suitable if the test portion disintegrates during the extraction. NOTE 4 Method D is normally used for production controls. Recommendations as to the solvent most appropriate for each type of rubber are given in Annex A.

ISO 9924-1:2016 specifies a thermogravimetric method for the determination of the total organic content, carbon black content and ash in vulcanizates and uncured compounds. The loss in mass at 300 °C is an approximate guide to the volatile-matter content of the compound. The method is suitable for the analysis of rubber compounds and vulcanizates containing the following rubbers occurring alone or as mixtures: a) polyisoprene of natural or synthetic origin; b) polybutadiene; c) styrene-butadiene copolymers; d) isobutylene-isoprene copolymers; e) ethylene-propylene copolymers and related terpolymers. NOTE The field of application of the method may be extended to the analysis of compounds containing rubbers different from those given in this subclause, provided that the applicability of the method is tested beforehand using known compounds or vulcanizates having a similar composition. Other compounds are covered in ISO 9924‑2. The method is not suitable for rubbers containing polymers which form a carbonaceous residue during pyrolysis, such as many chlorine- or nitrogen-containing rubbers. The method is also not suitable for materials containing additives which cause the formation of carbonaceous residues during pyrolysis, such as cobalt and lead salts or phenolic resins. The method is not suitable for compounds containing mineral fillers, such as carbonates or hydrated aluminium oxides, which decompose in the temperature range from 25 °C to 650 °C, unless suitable corrections based on prior knowledge of filler behaviour can be made. The method is not suitable for the determination of the total polymer content of compounds or vulcanizates containing non-rubber organic ingredients that cannot be completely removed by solvent extraction carried out in accordance with ISO 1407.

This document specifies accelerated ageing or heat resistance tests on vulcanized or thermoplastic rubbers/thermoplastic elastomers. Four methods are possible, they are detailed in Clause 5.

This document specifies an instrumental (automatic analyser) method for the determination of total sulfur in rubber and rubber products.

This document provides guidance on the determination of the abrasion resistance of vulcanized and thermoplastic rubbers. It covers both solid and loose abrasives. The guidelines given are intended to assist in the selection of an appropriate test method and appropriate test conditions for evaluating a material and assessing its suitability for a product subject to abrasion. Factors influencing the correlation between laboratory abrasion testing and product performance are considered, but, for example this document is not concerned with wear tests developed for specific finished rubber products, for example, trailer tests for tyres.

This document specifies a method for determining selected vulcanization characteristics of a rubber compound by means of a rotorless curemeter. An introduction to the use of curemeters is given in ISO 6502‑1.

This document describes two methods for measuring stress in tension under non-isothermal conditions. — Method A: The thermal stress is measured for various pre-strain and temperature conditions as a function of time. — Method B: The change of stress is measured in a test piece at a given strain and under variation of temperature at a given heating rate as a function of temperature. In this way, the determination of the thermal-mechanical behaviour of a rubber can be accelerated, e.g. for the purpose of comparative testing of aging or estimating the upper limit of the operating temperature. The measurement device, which is equipped with a suitable heating chamber, is used to record the stress as a function of time or temperature until the sample breaks or the stress has approached zero or for a certain time.

ISO 4666-3:2016 specifies the flexometer test with constant-strain amplitude for the determination of the temperature rise and resistance to fatigue of vulcanized rubber. The flexometer specified is known as the Goodrich flexometer, but any other apparatus giving equivalent performance can be used. ISO 4666-3:2016 gives directions for carrying out measurements which make possible predictions regarding the durability of rubbers in finished articles subject to dynamic flexing in service, such as tyres, bearings, supports, V-belts, and cable-pulley insert rings. However, owing to the wide variations in service conditions, no simple correlation between the accelerated tests described in the various parts of this document and service performance can be assumed. The method is not recommended for rubber having a hardness greater than 85 IRHD.

This document specifies methods for the determination of the modulus in shear and the strength of bonds of rubber to metal or other rigid plates, using rubber bonded between four parallel plates. Method A describes the determination of the modulus in shear. Method B describes the determination of the strength of the bonds. The methods are applicable primarily to test pieces prepared in the laboratory under standard conditions, such can be used to provide data for the development and control of rubber compounds and methods of manufacture of bonded shear units.

This document provides specifications for natural rubber latex concentrate which has low protein content [low protein natural rubber (LPNR) latex], as follows: — LPNR latex: field latex or concentrated latex pretreated with deproteinising agent, centrifuged and preserved after concentration with ammonia only, with an alkalinity of at least a mass fraction of 0,6 % calculated with respect to the latex. This document is applicable to medical rubber products and avoids the possibility of allergies. This document covers requirements for LPNR latex, type HA (high ammonia), and LPNR latex, type LA (low ammonia).

This document gives guidance on the determination of dynamic properties of vulcanized and thermoplastic rubbers. It includes both free- and forced-vibration methods carried out on both materials and products. It does not cover rebound resilience or cyclic tests in which the main objective is to fatigue the rubber.

This document provides guidelines and specifies requirements for estimating the precision of rubber test methods by means of interlaboratory test programmes based on the procedures given in: — Method A using ISO 5725 (all parts); — Method B using ASTM D4483

This document specifies three test methods for the determination of the tear strength of vulcanized or thermoplastic rubber, namely the following: — method A, using a trouser test piece; — method B, using an angle test piece, with or without a nick of specified depth; — method C, using a crescent test piece with a nick. The value of tear strength obtained depends on the shape of the test piece, speed of stretching, and temperature of test. It can also be susceptible to grain effects in rubber. NOTE A separate method for the determination of the tear strength of small test pieces of rubber (Delft test pieces) is specified in ISO 34-2.

This document specifies the procedures intended for use in estimating the resistance of vulcanized or thermoplastic rubbers to cracking when exposed, under static or dynamic tensile strain, to air containing a definite concentration of ozone, at a definite temperature and, if required, at a definite relative humidity in circumstances that exclude the effects of direct light. Visual observation and/or image analysis are used to evaluate the formation and growth of cracks. The changes in physical or chemical properties resulting from exposure can also be determined. Reference and alternative methods for determining the ozone concentration are described in ISO 1431-3.

This document specifies a method for the determination of the tear strength of small test pieces (Delft test pieces) of vulcanized or thermoplastic rubber. NOTE The method does not necessarily give results agreeing with those given by the method described in ISO 34-1, which uses trouser, angle and crescent test pieces. It is used in preference to ISO 34-1 when the amount of material available is limited, and can be particularly suitable for testing small finished products.

This document describes methods of evaluating the resistance of vulcanized and thermoplastic rubbers to the action of liquids by measurement of properties of the rubbers before and after immersion in test liquids. The liquids concerned include current service liquids, such as petroleum derivatives, organic solvents and chemical reagents, as well as reference test liquids.

This document describes two methods for identification of antidegradants (antioxidants, antiozonants and stabilizers) which can be present in raw rubber, unvulcanized compounded rubber, or rubber products, by thin layer chromatography. Method A is a simplified method that provides for the identification of known materials and can be used to check the presence or absence of a particular antidegradant which is expected to be present. Method B is a more detailed method that enables a greater degree of separation of the spots to be obtained and therefore can be used to detect and identify an unknown antidegradant. Antidegradants to which these methods are applicable include phosphited polyalkyl phenols, substituted bisphenols, secondary amines, substituted cresols and substituted p-phenylenediamines. Examination for other types of antidegradants is possible under the same condition when there is a standard chromatogram.

This document specifies an atomic absorption spectrometric method for the determination of the manganese content of rubbers. The method is applicable to raw rubber and rubber products having manganese content above 0,5 ppm. Manganese contents below this limit can be determined, provided that suitable adjustments are made either to the mass of the test portion or to the concentrations of the solutions used, or both. The use of the standard additions method can lower the bottom limit of detection.

This document specifies an atomic absorption spectrometric method for the determination of the copper content of rubbers. The method is applicable to raw rubber and rubber products having copper contents above 1 ppm. Copper contents below this limit can be determined, provided that suitable adjustments are made to either the mass of the test portion or to the concentrations of the solutions used, or both. The use of the standard additions method can lower the bottom limit of detection.

This document specifies three methods for the determination of the permeability to gases of vulcanized or thermoplastic rubber under a differential partial pressure. The three methods specified are as follows: — a pressure sensor method (using vacuum): for determining the gas transmission rate, gas permeability coefficient, gas diffusion coefficient and gas solubility coefficient; — a simplified sensor method (using applied pressure): for determining the gas permeability coefficient only; — a gas-chromatographic method: for determining the gas transmission rate and gas permeability coefficient. These methods apply to vulcanized and thermoplastic rubbers of hardness not less than 35 IRHD (international rubber hardness degrees) and to both single gases and mixtures of gases.

This document specifies — physical and chemical tests on raw natural rubbers; — standard materials, standard test formulae, equipment and processing methods for evaluating the vulcanization characteristics of natural rubber (NR).

This document specifies a quantitative test method to determine the 2-mercaptobenzothiazole content in rubber and rubber products by high performance liquid chromatography (HPLC). This document delivers a method for quantifying 2-mercaptobenzothiazole in rubber products for a better selection of curing conditions. This document provides a method to follow the curing of rubber with sulfur- and benzothiazole-based accelerators using a chemical measurement which is complementary to the classical rheometric technique.

This document specifies the standard test formulation, mixing procedure and test methods for evaluation of viscoelastic properties in a compound based on solution-polymerized styrene-butadiene rubber (S-SBR), including functionalized S-SBR.

This document specifies a method for the determination of the total sulfur content of raw rubber and unvulcanized or vulcanized rubber compounds by ion chromatography following the preparation of a sample solution using either a tubular furnace combustion or an oxygen combustion flask method. The tubular furnace combustion method is applicable for rubbers with sulfur content less than 0,1 % as it is possible that the oxygen combustion flask method will not give sufficiently accurate results. The oxygen combustion flask method is not applicable to rubbers containing a metal salt that forms an insoluble metal sulfate, such as barium sulfate (CAS 7727‑43‑7).

This document describes the method of determination of both major and trace levels of metal contents in rubber — raw, vulcanized — by ICP-OES.

This document specifies a method for the determination of the static adhesion of textile cord to vulcanized rubber using the H-pull test. It is applicable to cords made from natural or man-made fibres. The property levels obtained with this method are affected considerably by the history of the cord and the rubber compound. The method yields data, however, on which a judgement as to the service quality of the material can be based. The method is primarily intended for use with tyre cord. However, it can be applied, if desired, to similar cords for use in other rubber products, but it is limited to cords of linear density not exceeding 800 mg/m (tex).

This document specifies a method for the determination of the green strength of raw rubber or unvulcanized rubber compounds using a tensile stress-strain test, the test pieces being prepared following standard test conditions or cut from calendered sheets.

This document specifies a method for the determination of the tendency of vulcanized or thermoplastic rubbers to adhere to and to corrode metals when exposed to a specified test environment.

This document describes a procedure for the determination of the following antidegradants in vulcanized rubbers: — aminoketone group; — naphthylamine group; — diphenylamine group; — p-phenylenediamine; — monophenol group. The groups of antidegradants are summarized in Table A.1 with the chemical names, the abbreviated terms and the CAS registry numbers. Extender oils, when present, can interfere. For poly-2,2,4-trimethyl-1,2-dihydroquinoline, the method provides only an approximation because of its polymeric nature.

This document specifies a method for determining the glass transition temperature, Tg, of vulcanized rubbers in the hardness range from 30 IRHD to 80 IRHD. The dynamic properties are measured via temperature sweep in sinusoidal deformation at a defined strain and frequency and Tg is determined from the peak in the tan δ versus temperature curve. Glass transition temperature, Tg, determined in this way serves the purpose of a guideline to the service temperature of the material.

This document specifies a static procedure, known as the Gehman test, for determining the relative stiffness characteristics of vulcanized or thermoplastic rubbers over a temperature range from room temperature to approximately −120 °C.

This document establishes a vocabulary of and is limited to those terms in general use throughout the rubber industry. It does not define terms intended for particular rubber products, some of which are given in the vocabulary standards listed in the Bibliography. It does not define terms that are generally understood or adequately defined in other readily available sources such as general dictionaries. The terms are listed in the alphabetical order of the English terms, with an index to the corresponding English terms attached. Symbols are included under their full descriptions.

This document specifies: — the physical and chemical tests on raw rubbers, and — the standardized materials, a standardized test formulation, equipment, and processing methods for evaluating the vulcanization characteristics of all types of isobutene-isoprene rubber (IIR).

This document specifies: — the physical and chemical tests on raw rubbers; — the standard materials, standard test formulations, equipment, and processing methods for evaluating the vulcanization characteristics of ethylene-propylene-diene rubbers (EPDM), including oil-extended types.

This document specifies: — the physical and chemical tests on raw rubbers; — the standard materials, standard test formulations, equipment, and processing methods for evaluating the vulcanization characteristics of styrene-butadiene rubber masterbatches with carbon black or with carbon black and oil.

This document specifies, for acrylonitrile-butadiene rubbers (NBRs): — physical and chemical tests on raw rubbers; — standard materials, a standard test formulation, equipment and processing methods for evaluating the vulcanization characteristics. The mixing preferred method is the single stage mixing with LIM (laboratory internal mixer).

This document establishes guidelines for the specification of vulcanized rubber based on the properties of individual rubber types. This document helps users of rubber products, who are not rubber experts, to create a specification for the rubber materials they wish to use. It also describes a designation system to enable a line call-cut code to be devised for each specification. Since the properties of rubber depend on the type of rubber, such as composition, some rubbers are classified into several types and organized by hardness. Representative specifications for the following rubber types are given in Annexes B to M: natural rubber (NR), styrene butadiene rubber (SBR), nitrile rubber (NBR), hydrogenated nitrile rubber (HNBR), nitrile rubber mixed with PVC (NBR/PVC), chloroprene rubber (CR), ethylene acrylic rubber (AEM), fluorocarbon rubber (FKM), silicone rubber (VMQ), epichlorohydrin rubber (ECO) and ethylene propylene rubber (EPM and EPDM). In cases of mixed rubber polymers, the main polymer in the rubber material gives the name of the rubber type.

This document specifies a method using a differential scanning calorimeter to determine the glass transition temperature of raw rubber and rubber latex.

This document specifies a method for determining the pre-vulcanization characteristics of compounded rubber. The pre-vulcanization characteristics determined by this method provide a means of estimating how long compounded rubber can be maintained at high temperatures and remain processable.

This document specifies a method of test for measuring the force required to separate, by stripping, two plies of fabric bonded with rubber, or a rubber layer and a fabric ply bonded together. The method is applicable when the ply surfaces are approximately plane or when they are in the form of a cylinder having an internal diameter greater than approximately 50 mm. The method is not applicable when the ply surfaces contain sharp bends, angles or other gross irregularities which cannot be excluded when cutting out test pieces. This document does not apply to coated fabrics, which are tested in accordance with ISO 2411, or textile conveyor belts, which are tested in accordance with ISO 252.

This document specifies a test based on hardness measurements for determining the progressive stiffening of rubber with time, caused by crystallization. It is limited to materials having an initial hardness at a test temperature of from 10 IRHD to 85 IRHD. The method is applicable to raw, unvulcanized (compounded) and vulcanized rubber. It is mainly of interest for rubber with a marked crystallization tendency at temperatures experienced in cold climates, such as chloroprene and natural rubber. The method is not applicable to fast-crystallizing materials which crystallize to a considerable degree within the timespan of 15 min used for conditioning at test temperature.

This document specifies a method for the identification of polymers, or blends of polymers, in raw rubbers and in vulcanized or unvulcanized compounds from pyrograms (pyrolysis-gas chromatographic patterns) obtained under the same conditions. This allows qualitative identification of single rubbers or blends, with exceptions discussed below. This document is not intended for quantitative analysis. The method applies first and foremost to single polymers. When the pyrogram indicates a characteristic hydrocarbon, the method is also applicable to blends. For details, see Clause 5. The method can be also applicable to other types of polymer when verified by the analyst in each particular case. NOTE The use of this document pre-supposes sufficient working knowledge of the principles and techniques of gas chromatography to enable the analyst to carry out the operations described and to interpret the results correctly.