ISO 21084:2019 纺织品 烷基酚(AP)的测定方法.pdf
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1、INTERNATIONAL STANDARD ISO 21084 First edition 2019-02 Textiles-Method for determination of alkylphenols(AP)!II Textiles-Methode de determination de la teneur en alkylphenols rAP)Reference number ISO 21084:2019(E)ISO 2019 I,.ISO 21084:2019(E)COPYRIGHT PROTECTED DOCUMENT ISO 2019 All rights reserved.
2、Unless otherwise specified,or required in the context of its implementation,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.Permi
3、ssion can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright office CP 401 Ch.de Blandonnet 8 CH-1214 Vernier,Geneva Phone:+41 22 749 0111 Fa+41 22 749 09 47 Email:copyrightiso,org Website:www.iso.org Published in Switzerland ii ISO 20
4、19-All rights reserved ISO 21084:2019(E)Contents Page Foreword.iv 1 2 Scope.Normative references.1.1 3 Terms and definitions.1 4 5 6 7 8 Principle.1 Reagents.1 Apparatus.2 6.1 Genera!.2 6.2 Apparatus and auxiliaries for preparing the sample.2 6.3 Chromatographic equipment.2 Procedure.2 7.1 Standard
5、preparation.2 7.2 Sample preparation.2 7.3 Sample extraction.3 7.4 Sample analysis.3 Calculation and calibration.3 8.1 Calibration curve.3 8.2 External calibration.3 8.3 Calculation of each AP in sample.4 8.4 Reliability of the method.4 9 Test report.4 Annex A(informative)Examples of chromatographic
6、 condition-GC-MSjMS.5 Annex B(informative)Examples of chromatographic condition-LC-MSjMS and LC-FLD.8 Annex C(informative)Reliability of the method.10 ISO 2019-All rights reserved iii ISO 21084:2019(E)Foreword ISO(the International Organization for Standardization)is a worldwide federation of nation
7、al standards 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
8、organizations,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 fu
9、rther 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.jso,org/djrectjves)
10、.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 Introduc
11、tion and/or on the ISO list of patent declarations received(see wwwjsnnrg/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 terms a
12、nd 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:wwwjsQ,org/jso/foreword btml.This document was prepared by Technical Committee ISO/TC 38,Textiles.An
13、y feedback or questions on this document should be directed to the users national standards body.A complete listing of these bodies can be found at wwwjsn nrg/members,html.iv ISO 2019-All rights reserved I INTERNATIONAL STANDARD ISO 21084:2019(E)Textiles-Method for determination of alkylphenols(AP)W
14、ARNING-This document calls for the use of substances/procedures that may be injurious to the health/environment if appropriate conditions are not observed.It refers only to technical suitability and does not absolve the user from legal obligations relating to health and safety/environment at any sta
15、ge.1 Scope This document specifies the method for the determination of extractable alkyl phenols(AP)without derivatization step in textile and textile products.2 Normative references There are no normative references in this document.3 Terms and definitions No terms and definitions are listed in thi
16、s document.ISO and IEC maintain terminological databases for use in standardization at the following addresses:ISO Online browsing platform:available at https:/!wwwisoorg/Ohp IEC Electropedia:available at http/!wwwelectropedia org I 4 Principle The test specimen is cut into small pieces,transferred
17、to a sample vial and treated with methanol in ultrasonic water bath.The extract is filtered and collected.Subsequently,the collected extract is analysed by gas chromatograph with mass selective detector(GC-MS),liquid chromatograph with mass selective detector(LC-MS)or liquid chromatograph with fluor
18、escence detector(LC-FLD).5 Reagents Unless otherwise specified,analytical grade chemicals shall be used.5.1 4-n-Octylphenol,CAS No.1806-26-4.5.2 4-tert-Octylphenol,CAS No.140-66-9.5.3 4-n-Nonylphenol,CAS No.104-405.5.4 4-Nonylphenol.CAS No.84852-153.5.5 Methanol,(HPLC grade).5.6 Acetone.5.7 Acetonit
19、rile,(HPLC grade).ISO 2019-All rights reserved 1.ISO 21084:2019(E)5.8 Water,(HPLC grade).6 Apparatus 6.1 General Clean all glassware by rinsing with acetone(5.6)prior to use.6.2 Apparatus and auxiliaries for preparing the sample 6.2.1 Standard laboratory equipment and the following.6.2.2 Analytical
20、balance with resolution of 0,01 g(for test specimen preparation).6.2.3 Analytical balance with resolution of 0,001 g(for standard preparation).6.2.4 Glass vial with screw cap(e.g.40 ml).6.2.5 Ultrasonic water bath to be set up at(70 5)C).6.2.6 Disposable syringe and membrane filter(with pore size of
21、 0,45 m or less).6.2.7 Glass vial with septum cap(for chromatographic instrument).6.3 Chromatographic equipment 6.3.1 Gas chromatograph with mass selective detector(GC-MS),or 6.3.2 Liquid chromatograph with mass selective detector(LC-MS),or 6.3.3 Liquid chromatograph with fluorescence detector(LC-FL
22、D).6.3.4 Capillary column for gas chromatograph,(5%-phenyl)-methylpolysiloxane phase,non-polar,bonded and cross-linked,low bleed.6.3.5 C18 reverse phase column for liquid chromatograph.7 Procedure 7.1 Standard preparation Octylphenols and nonylphenols are weighed accurately with analytical balance(2
23、.U)and dissolved with methanol(5.5.)containing 1 000 mg!1 for stock solution.The stock solution can be preserved in the dark at less than 4C.7.2 Sample preparation The test specimen is cut into pieces with 5 mm x 5 mm and pieces are mixed homogeneously.The specimen is weighed 1 g to the nearest 0,01
24、 g with analytical balance(li.Z.Z)and put into the 40 ml glass vial(6.Z.1)for extraction.2 ISO 2019-All rights reserved ISO 21084:2019(E)7.3 Sample extraction 10 ml of methanol(5.5)are added to glass vial(6.2A)for extraction.If sample is not sufficiently immersed in the extraction solvent,add more m
25、ethanol and record the final volume for calculation of eachAP described in aJ.Then the sample vial is sonicated for extraction in ultrasonic water bath(6.2.S.)at 70C for 60 min.Subsequently,the extract is cooled down to room temperature,approximately 1 ml to 2 ml of extract is filtered into sample v
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