1、Rubber compounding ingredients p-Phenylenediamine antidegradants (PPDs) Test methodsBS ISO 11236:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 ISO 2017Rubber compounding ingredients p-Phenylenediamine antidegradants (PPDs) Test methodsIngrdients de mlange du c
2、aoutchouc Antidgradants du type p-phnylnediamine (PPDs) Mthodes dessaiINTERNATIONAL STANDARDISO11236Second edition2017-08Reference numberISO 11236:2017(E)National forewordThis British Standard is the UK implementation of ISO 11236:2017.The UK participation in its preparation was entrusted to Technic
3、al Committee PRI/50, Raw materials (including latex) for use in the rubber industry.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its
4、 correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 92857 4ICS 83.040.20; 01.040.83Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards
5、Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS ISO 11236:2017 ISO 2017Rubber compounding ingredients p-Phenylenediamine antidegradants (PPDs) Test methodsIngrdients de mlange du caoutchouc Antidgradants du type p-
6、phnylnediamine (PPDs) Mthodes dessaiINTERNATIONAL STANDARDISO11236Second edition2017-08Reference numberISO 11236:2017(E)BS ISO 11236:2017ISO 11236:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no
7、part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member
8、 body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 11236:2017ISO 11236:2017(E)ii ISO 2017 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2017, Publishe
9、d in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission
10、can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 22 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgISO 11236:2017(E)Foreword iv1 Scope . 12 Nor
11、mative references 13 Terms and definitions . 14 Abbreviated terms 25 Use and classification 26 Sampling and repeat determinations . 37 Determination of purity by gas chromatography (GC) . 37.1 General . 37.2 Interference . 37.3 Apparatus 37.4 Calibration and standardization 57.5 Procedure 57.5.1 Sam
12、ple preparation . 57.5.2 Procedure A 57.6 Calculation . 117.7 Precision and bias . 117.8 Test report 118 Determination of purity by high-performance liquid chromatography (HPLC) .118.1 General 118.2 Apparatus . 118.3 Reagents. 128.4 Procedure . 128.5 Calculation . 148.6 Precision and bias . 148.7 Te
13、st report 159 Determination of ash 159.1 General 159.2 Apparatus . 159.3 Procedure . 159.4 Calculation . 169.5 Precision and bias . 169.6 Test report 1610 Determination of volatile matter .1610.1 General 1610.2 Apparatus . 1710.3 Preparation of sample 1710.4 Procedure . 1710.5 Calculation . 1710.6 P
14、recision and bias . 1710.7 Test report 18Annex A (informative) Precision and bias .19Bibliography .22 ISO 2017 All rights reserved iiiContents PageBS ISO 11236:2017ISO 11236:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
15、 (ISO member bodies). The work of preparing International Standards 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,
16、governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further mai
17、ntenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).
18、Attention is drawn to the possibility 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. Details of any patent rights identified during the development of the document will be in the Introdu
19、ction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of ISO specific
20、 terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee I
21、SO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This second edition cancels and replaces the first edition (ISO 11236:2000), which has been technically revised. It also incorporates the Technical Corrigendum ISO 11236:2000/Cor.1
22、:2006.The main changes compared to the previous version are as follows: removal of DTPD (N,N-ditolyl-p-phenylenediamine), which is widely acknowledged to be hazardous to health and environment; transfer in an informative Annex A of the precision and bias for the determination of purity by gas chroma
23、tography by procedure A, for the determination of ash and for the determination of volatile matter; addition of a Bibliography.iv ISO 2017 All rights reservedBS ISO 11236:2017ISO 11236:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national stand
24、ards bodies (ISO member bodies). The work of preparing International Standards 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 orga
25、nizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its
26、further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ d
27、irectives).Attention is drawn to the possibility 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. Details of any patent rights identified during the development of the document will be in
28、the Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the voluntary nature of standards, the meaning of I
29、SO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical
30、Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 3, Raw materials (including latex) for use in the rubber industry.This second edition cancels and replaces the first edition (ISO 11236:2000), which has been technically revised. It also incorporates the Technical Corrigendum ISO 11236
31、:2000/Cor.1:2006.The main changes compared to the previous version are as follows: removal of DTPD (N,N-ditolyl-p-phenylenediamine), which is widely acknowledged to be hazardous to health and environment; transfer in an informative Annex A of the precision and bias for the determination of purity by
32、 gas chromatography by procedure A, for the determination of ash and for the determination of volatile matter; addition of a Bibliography.iv ISO 2017 All rights reserved INTERNATIONAL STANDARD ISO 11236:2017(E)Rubber compounding ingredients p-Phenylenediamine antidegradants (PPDs) Test methodsWARNIN
33、G Persons using this document should be familiar with normal laboratory practice. This document 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
34、with any national regulatory conditions.1 ScopeThis document 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 followi
35、ng 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 chromatograph
36、y (HPLC); determination of ash; determination of volatile matter.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated refe
37、rences, the latest edition of the referenced document (including any amendments) applies.ISO 1042, Laboratory glassware One-mark volumetric flasksISO 1772, Laboratory crucibles in porcelain and silicaISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling3 Terms and definiti
38、onsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: ISO Online browsing platform: available at http:/ www. iso. org/ obp IEC Electropedia: available at http:/ www .electro
39、pedia. org/ 3.1area normalizationmethod of calculating the percent composition by measuring the area of each component peak observed in a chromatogram and dividing the area of the peak by the total peak area for all the components observed3.2lot sampleproduction sample representative of a standard p
40、roduction unit ISO 2017 All rights reserved 1BS ISO 11236:2017ISO 11236:2017(E)3.3test portionactual material used in the analysisNote 1 to entry: The test portion shall be representative of the lot sample.4 Abbreviated termsPPDs substituted p-phenylenediamine antidegradantsThe following abbreviatio
41、ns, taken from ISO 6472, are used in the text.77PD N,N-bis(1,4-dimethylpentyl)-p-phenylenediamineIPPD N-isopropyl-N-phenyl-p-phenylenediamine6PPD N-1,3-dimethylbutyl-N-phenyl-p-phenylenediamine5 Use and classificationPPDs represent the primary additive used in tyres and other mechanical rubber goods
42、 to impart ozone protection and to improve resistance to fatigue cracking. PPDs are also used as antioxidants in a number of applications.Although all PPDs exhibit similar performance characteristics, particular types are frequently preferred for certain end-use conditions, for example, the type and
43、 degree of flexing experienced by the rubber article.PPDs are classified into the following types.a) Type I: N,N-dialkyl PPDs (see Figure 1)R and R are secondary alkyl groups, usually C6or larger. These materials are generally liquids at ambient conditions and consist for the most part (90 %) of a s
44、ingle chemical component.b) Type II: N-alkyl-N-aryl PPDs (see Figure 2)R is a secondary alkyl group and R is an aryl substituent (usually phenyl). These materials generally consist of a single component or a mixture containing two or more major components (mainly isomers).c) Type III: N, N-diaryl PP
45、Ds (see Figure 3)R and R can be the same aryl group or different (usually phenyl or p-tolyl) and can be single components or mixtures of three or more isomers. This type of PPDs is generally solid at ambient conditions.Figure 1 Type I: N,N-dialkyl p-phenylenediaminesFigure 2 Type II: N-alkyl-N-aryl
46、p-phenylenediamines2 ISO 2017 All rights reservedBS ISO 11236:2017ISO 11236:2017(E)3.3test portionactual material used in the analysisNote 1 to entry: The test portion shall be representative of the lot sample.4 Abbreviated termsPPDs substituted p-phenylenediamine antidegradantsThe following abbrevi
47、ations, taken from ISO 6472, are used in the text.77PD N,N-bis(1,4-dimethylpentyl)-p-phenylenediamineIPPD N-isopropyl-N-phenyl-p-phenylenediamine6PPD N-1,3-dimethylbutyl-N-phenyl-p-phenylenediamine5 Use and classificationPPDs represent the primary additive used in tyres and other mechanical rubber g
48、oods to impart ozone protection and to improve resistance to fatigue cracking. PPDs are also used as antioxidants in a number of applications.Although all PPDs exhibit similar performance characteristics, particular types are frequently preferred for certain end-use conditions, for example, the type
49、 and degree of flexing experienced by the rubber article.PPDs are classified into the following types.a) Type I: N,N-dialkyl PPDs (see Figure 1)R and R are secondary alkyl groups, usually C6or larger. These materials are generally liquids at ambient conditions and consist for the most part (90 %) of a single chemical component.b) Type II: N-alkyl-N-aryl PPDs (see Figure 2)R is a secondary alkyl group and R is an aryl substituent (usually phenyl). These materials generall
