BS ISO 28641-2010 en 5873 Rubber compounding ingredients - Organic chemicals - General test methods《橡胶合成配料 有机化学 一般试验方法》.pdf

1、BS ISO28641:2010ICS 83.040.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRubber compoundingingredients Organicchemicals Generaltest methodsThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 30 June2010 BSI 2

2、010ISBN 978 0 580 57896 0Amendments/corrigenda issued since publicationDate CommentsBS ISO 28641:2010National forewordThis British Standard is the UK implementation of ISO 28641:2010.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-b

3、lack compoundingingredients.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard ca

4、nnot confer immunityfrom legal obligations.BS ISO 28641:2010Reference numberISO 28641:2010(E)ISO 2010INTERNATIONAL STANDARD ISO28641First edition2010-06-01Rubber compounding ingredients Organic chemicals General test methods Ingrdients de mlange du caoutchouc Produits chimiques organiques Mthodes de

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8、l Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2010 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission i

9、n writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2010 All rights reservedBS I

10、SO 28641:2010ISO 28641:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Abbreviations.2 4 General requirements .2 4.1 Thermometer2 4.2 Dessicator 2 5 Sampling.2 5.1 Apparatus.2 5.2 Sampling method 2 6 Drying the sample .2 6.1 General .2 6.2 Drying

11、methods for liquid compounding ingredients .2 6.3 Drying methods for solid compounding ingredients 3 7 Test methods .4 7.1 Relative density .4 7.2 Loss on heating .8 7.3 Sieve residue .10 7.4 pH of water extract 12 7.5 Melting point 14 7.6 Temperature of solidification .17 7.7 Softening point 20 7.8

12、 Density of the bulk material .22 7.9 Ash 24 7.10 Refractive index.25 Annex A (informative) Examples of sampling apparatus .29 Annex B (informative) Examples of suitable drying apparatus31 Annex C (normative) Verification of accuracy of pH-meter34 Annex D (normative) Calibration of the pH-meter .38

13、Annex E (informative) Precision40 Bibliography47 BS ISO 28641:2010ISO 28641:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standar

14、ds is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take

15、 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is

16、to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility

17、 that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 28641 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) fo

18、r use in the rubber industry. BS ISO 28641:2010INTERNATIONAL STANDARD ISO 28641:2010(E) ISO 2010 All rights reserved 1Rubber compounding ingredients Organic chemicals General test methods WARNING Persons using this International Standard should be familiar with normal laboratory practice. This stand

19、ard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies sampl

20、ing and test methods for the determination of the general characteristics of organic chemicals such as accelerators, antidegradants (including wax) and vulcanizing agents (excluding peroxides). 2 Normative references The following referenced documents are indispensable for the application of this do

21、cument. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 649-1, Laboratory glassware Density hydrometers for general purposes Part 1: Specification ISO 649-2:1981, Laboratory glassware

22、Density hydrometers for general purposes Part 2: Test methods and use ISO 760, Determination of water Karl Fischer method (General method) ISO 976:1996, Rubber and plastics Polymer dispersions and rubber latices Determination of pH ISO 1770, Solid-stem general purpose thermometers ISO 3310-1, Test s

23、ieves Technical requirements and testing Part 1: Test sieves of metal wire cloth ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 3838, Crude petroleum and liquid or solid petroleum products Determination of density or relative density Capillary-stoppered pyknome

24、ter and graduated bicapillary pyknometer methods ISO 4625-1, Binders for paints and varnishes Determination of softening point Part 1: Ring-and-ball method ISO 6353-2, Reagents for chemical analysis Part 2: Specifications First series ISO 6353-3, Reagents for chemical analysis Part 3: Specifications

25、 Second series ISO 6472, Rubber compounding ingredients Abbreviations ISO 11235:1999, Rubber compounding ingredients Sulfenamide accelerators Test methods BS ISO 28641:2010ISO 28641:2010(E) 2 ISO 2010 All rights reservedISO 11236:2000, Rubber compounding ingredients p-Phenylenediamine (PPD) antidegr

26、adants Test methods ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling ISO 80000-1:2009, Quantities and units Part 1: General 3 Abbreviations The abbreviations of the chemical names of the organic accelerators and antidegradants used in this International Standard are i

27、n accordance with ISO 6472. 4 General requirements 4.1 Thermometer Where a thermometer is used, it shall be a solid-stem thermometer meeting the requirements of ISO 1770 and shall be chosen according to the intended purpose. It shall have been calibrated before use with a standard thermometer. 4.2 D

28、essicator Where a vacuum dessicator is used, the pressure reduction in the desiccator shall not be more than 2,0 kPa, unless otherwise specified. 5 Sampling 5.1 Apparatus The apparatus used for sampling (see Annex A) shall be suitable for each test method. 5.2 Sampling method Carry out sampling in a

29、ccordance with ISO 15528. To ensure homogeneity, thoroughly blend at least 250 g of the sample before taking any test portions. 6 Drying the sample 6.1 General The drying method used will depend on the nature of the sample. Select a suitable method from those specified in 6.2 and 6.3. The method cho

30、sen shall not have a deleterious effect on the sample. 6.2 Drying methods for liquid compounding ingredients 6.2.1 Apparatus 6.2.1.1 Vacuum desiccator (see Figure B.1), capable of withstanding the reduced pressure specified. 6.2.1.2 Apparatus for drying liquid samples by passing a dry gas through th

31、e boiling liquid (see Figure B.2), consisting of a flask with a reflux condenser, a dry-gas inlet tube and a heating bath. The top of the condenser is connected to a suction pump. A drying tube is connected between the suction pump and the top of the condenser. BS ISO 28641:2010ISO 28641:2010(E) ISO

32、 2010 All rights reserved 36.2.1.3 Apparatus for drying liquid samples by passing a dry gas through the liquid at ambient temperature (see Figure B.3), consisting of a flask and a dry-gas inlet tube. The top of the condenser is connected to a suction pump. A drying tube is connected between the suct

33、ion pump and the top of the condenser. 6.2.2 Method using a desiccator If carrying out the drying under ordinary pressure, dry the sample in a desiccator containing a suitable desiccant until the mass of the sample becomes constant, i.e. allow to dry for periods of 30 min until the loss in mass of t

34、he sample, unless otherwise specified, between two successive weighings is less than 3 mg. When carrying out the drying under reduced pressure, dry the sample in a vacuum desiccator (6.2.1.1) containing a suitable desiccant at a pressure reduction of no more than 2,0 kPa until the mass of the sample

35、 becomes constant, i.e. allow to dry for periods of 30 min until the loss in mass of the sample, unless otherwise specified, between two successive weighings is less than 3 mg. NOTE Examples of suitable desiccants are anhydrous calcium chloride, anhydrous sodium sulfate, anhydrous potassium carbonat

36、e, calcium oxide, aluminium oxide, potassium hydroxide, sodium hydroxide and silica gel. Phosphoric anhydride, concentrated sulfuric acid and metallic sodium may also be used. 6.2.3 Method using a dry gas Use the apparatus described in 6.2.1.2 if drying the sample by passing a dry gas through the bo

37、iling sample. Use the apparatus described in 6.2.1.3 if drying the sample at ambient temperature. Dry the sample until the water content is less than 0,05 % as determined by the most appropriate method in ISO 760 (Karl Fischer). NOTE Air, nitrogen or carbon dioxide is generally used as the drying ga

38、s. 6.2.4 Method using a desiccant added to the sample Add a suitable desiccant to the sample and disperse it well by shaking. Then, keeping the desiccant suspended, filter the sample through a dried filter paper. NOTE See the Note to 6.2.2. 6.2.5 Method using a solvent (suitable for viscous liquids)

39、 Dissolve the sample in a suitable solvent and add a suitable desiccant to the solution. Disperse the desiccant by shaking and then filter the suspension through a dried filter paper. Eliminate the solvent remaining in the sample by distillation or simple evaporation. 6.3 Drying methods for solid co

40、mpounding ingredients 6.3.1 Apparatus 6.3.1.1 Atmospheric-pressure or vacuum drying oven. 6.3.1.2 Apparatus for drying solid samples by passing a dry gas through the molten sample (see Figure B.4), consisting of a cylindrical flask fitted with a dry-gas inlet tube and a gas outlet tube which is conn

41、ected to a suction pump. A drying tube is connected between the suction pump and the gas outlet tube containing the desiccant. A suitable heating bath is required. 6.3.1.3 Apparatus for drying solid samples by passing a dry gas through the sample at ambient temperature (see Figure B.5), including a

42、cylindrical flask fitted with a perforated plate. Connected to the flask below the plate is a dry-gas inlet tube. Fitted to the top of the flask is a gas outlet tube which is connected to a suction pump. A drying tube containing a suitable desiccant is connected between the suction pump and the gas

43、outlet tube. BS ISO 28641:2010ISO 28641:2010(E) 4 ISO 2010 All rights reserved6.3.2 Method using a desiccator Carry out the drying, either at ordinary pressure or at reduced pressure, as described in 6.2.2. 6.3.3 Method using a drying oven Dry the sample in a drying oven (6.3.1.1), with or without v

44、acuum, to constant mass as defined in 6.2.2. 6.3.4 Method using a dry gas Use the apparatus described in 6.3.1.2 if drying the sample in the molten state. Use the apparatus described in 6.3.1.3 if drying the sample at ambient temperature. Dry the sample until the water content is less than 0,05 % as

45、 determined by the most appropriate method in ISO 760 (Karl Fischer). NOTE Air, nitrogen or carbon dioxide is generally used as the drying gas. 7 Test methods 7.1 Relative density 7.1.1 General Select one of the following two methods for the determination of relative density, depending the nature of

46、 the material under test (hereafter referred to as the “sample”), the quantity available and the accuracy required: a) hydrometer method (liquid sample); b) pyknometer method (liquid or solid sample). NOTE Relative density is generally measured at 20 C and expressed as relative density (20 C/20 C).

47、It represents the ratio of the mass of the sample in air at 20 C to the mass of an equal volume of water in air at the same temperature. 7.1.2 Hydrometer method 7.1.2.1 Apparatus 7.1.2.1.1 Hydrometer, made of a suitable transparent glass, graduated in relative density at 20 C, capable of measuring r

48、elative density at 20 C over the range 0,600 to 2,000 and meeting the requirements of ISO 649-1. The hydrometer shall have been calibrated before use with a standard hydrometer. 7.1.2.1.2 Thermometer, as specified in 4.1. 7.1.2.1.3 Hollow cylinder, made of glass, having an inside diameter which is a

49、t least 25 mm larger than the maximum diameter of the hydrometer. The height shall be such that, when the hydrometer comes to rest, its base is at least 25 mm above the bottom of the cylinder. 7.1.2.1.4 Constant-temperature water bath, capable of maintaining a temperature of (20 0,5) C. 7.1.2.2 Procedure a) Put the sample in the cylinder, avoiding the inclusion of air bubbles. Maintain the cylinder in the constant-temperature water bath. Stir the sample. Monitor the temperat