EN ISO 14362-3-2017 en Textiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3 Detection of the use of certain azo colorants which may r.pdf

1、BS EN ISO 14362-3:2017T e x t i l e s M e t h o d s f o r determination of certain aromatic amines derived from azo colorantsPart 3: Detection of the use of certain azo colorants, which may release 4-aminoazobenzene (ISO 14362-3:2017)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 1

2、5/05/2013 15:06BS EN ISO 14362-3:2017 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 14362-3:2017. It supersedes BS EN 14362-3:2012 which iswithdrawn.The UK participation in its preparation was entrusted to Technical Committee TCI/80, Chemical testing of te

3、xtiles.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 correct application. The British Standards Institution 2017.Published by BSI

4、 Standards Limited 2017ISBN 978 0 580 85043 1 ICS 59.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since p

5、ublicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14362-3 February 2017 ICS 59.060.01 Supersedes EN 14362-3:2012English Version Textiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3: Detection of the use of ce

6、rtain azo colorants, which may release 4-aminoazobenzene (ISO 14362-3:2017) Textiles - Mthodes de dtermination de certaines amines aromatiques drives de colorants azoques - Partie 3: Dtection de lutilisation de certains colorants azoques susceptibles de librer du 4-aminoazobenzne (ISO 14362-3:2017)

7、Textilien - Verfahren fr die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 3: Nachweis der Verwendung gewisser Azofarbstoffe, die 4-Aminoazobenzol freisetzen knnen (ISO 14362-3:2017) This European Standard was approved by CEN on 21 December 2016. CEN members are bound to comply

8、with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Ma

9、nagement Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same

10、status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, M

11、alta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brusse

12、ls 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14362-3:2017 EBS EN ISO 14362-3:2017EN ISO 14362-3:2017 (E) 3 European foreword This document (EN ISO 14362-3:2017) has been prepared by Technical Committee ISO/TC 38 “Tex

13、tiles“ in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2017, an

14、d conflicting national standards shall be withdrawn at the latest by August 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This

15、 document supersedes EN 14362-3:2012. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugos

16、lav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14362-

17、3:2017 has been approved by CEN as EN ISO 14362-3:2017 without any modification. BS EN ISO 14362-3:2017ISO 14362-3:2017(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definition 14 General 25 Principle 26 Safety precautions 27 Reagents 28 Apparatus . 39 Procedure. 49.1 General . 49.2 Pr

18、eparation of test specimens . 49.3 Colorant extraction for disperse dyes Preparation with extraction 59.4 Textiles dyed with dyes other than disperse dyes Preparation without extraction . 59.5 Reductive cleavage . 59.6 Separation and concentration of 4-aminoazobenzene . 59.7 Calibration solution 69.

19、7.1 Calibration solution for sample preparation without extraction . 69.7.2 Calibration solution for sample preparation with extraction . 69.8 Check of the analytical system . 69.8.1 Sample preparation without extraction 69.8.2 Sample preparation with extraction . 69.9 Chromatographic analyses . 610

20、 Evaluation 710.1 Calculation 710.2 Reliability of the method 711 Test report . 7Annex A (informative) Chromatographic analyses 8Annex B (informative) Calculation.14Annex C (informative) Reliability of the method 15Annex D (informative) Assessment guide Interpretation of analytical results .16 ISO 2

21、017 All rights reserved iiiContents PageBS EN ISO 14362-3:2017ISO 14362-3:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through

22、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 part in the work. ISO collaborates

23、 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 maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval crite

24、ria 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).Attention is drawn to the possibility that some of the elements of this document may be the subject

25、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 Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade

26、name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (W

27、TO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .htmlThis document was prepared by the European Committee Standardization (CEN) Technical Committee CEN/TC 248, Textiles and textile products, in collaboration with ISO Technical Committee TC

28、38, Textiles, in accordance with the agreement on technical cooperation between ISO and CEN (Vienna Agreement).This first edition of ISO 14362-3 cancels and replaces ISO 24362-3:2014, which has been technically revised.The following is a list of the major technical changes between this edition and I

29、SO 24362-3:2014: addition of a new Clause 3 and renumbered; changes to 7.1 to clarify the preparation and use of sodium dithionite solution; changes to Clause 9 “Procedure” to improve the method, including using xylene as substitute for chlorobenzene (reasons: lower toxicity and lower adverse enviro

30、nmental effect of xylene).A list of all parts in the ISO 14362 series can be found on the ISO website.iv ISO 2017 All rights reservedBS EN ISO 14362-3:2017INTERNATIONAL STANDARD ISO 14362-3:2017(E)Textiles Methods for determination of certain aromatic amines derived from azo colorants Part 3: Detect

31、ion of the use of certain azo colorants, which may release 4-aminoazobenzene1 ScopeAzo colorants that are able to form 4-aminoazobenzene, generate under the conditions of ISO 14362-1, the amines aniline and 1,4-phenylenediamine. The presence of these 4-aminoazobenzene colorants cannot be reliably as

32、certained without additional information (e.g. the chemical structure of the colorant used) or without a special procedure.This document is supplementary to ISO 14362-1 and describes a special procedure to detect the use, in commodities, of certain azo colorants, which may release 4-aminoazobenzene,

33、 and that are accessible to reducing agent without extraction, particularly concerning textiles made of cellulose and protein fibres (e.g. cotton, viscose, wool, silk), and accessible by extracting the fibres (e.g. polyester or imitation leather).For certain fibre blends, in 9.3 and 9.4 (with and wi

34、thout extraction) may need to be applied.The procedure also detects 4-aminoazobenzene (Solvent Yellow 1), which is already available as free amine in commodities without reducing pre-treatment.The use of certain azo colorants, which may release, by reductive cleavage of their azo group(s), one or mo

35、re of the other aromatic amines listed in the Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorization and Restriction of Chemicals (REACH) as regards Annex XVII, except 4-aminoazobenzene, cannot be determined quantitatively with this

36、method.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 references, the latest edition of the referenced document (inc

37、luding any amendments) applies.ISO 3696, Water for analytical laboratory use Specification and test methodsISO 14362-1:2017, Textiles Methods for determination of certain aromatic amines derived from azo colorants Part 1: Detection of the use of certain azo colorants accessible with and without extr

38、acting the fibres3 Terms and definitionNo terms and definitions are listed in this document. ISO 2017 All rights reserved 1BS EN ISO 14362-3:2017ISO 14362-3:2017(E)ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at h t

39、t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp4 GeneralCertain azo colorants may release, by reductive cleavage of azo group(s), 4-aminoazobenzene.Table 1 4-aminoazobenzeneaNo. CAS number Index number EC number Substance22 60093 611008004 2004

40、536 4-aminoazobenzeneaProscribed aromatic amine under Regulation (EC) No 1907/2006 of the European Parliament and of the Council of 18 December 2006 concerning the Registration, Evaluation, Authorization and Restriction of Chemicals (REACH), establishing a European Chemicals Agency.5 PrincipleAfter

41、selection of a coloured test specimen from the textile article, the test specimen is tested according to the method of the colorant extraction for disperse dyes and/or the method of the direct reduction for the other classes of colorants (pigments and/or dyes) (see ISO 14362-1).The textile sample or

42、 the residue of the sample extraction is treated with sodium dithionite in an alkaline solution at 40 C in a closed vessel. 4-aminoazobenzene, which is released in the process, is transferred to a t-butyl methyl ether phase by means of liquid-liquid extraction. An aliquot of the t-butyl methyl ether

43、 phase is used for analysis. The detection and determination of 4-aminoazobenzene can be performed using chromatography (see Annex A).If 4-aminoazobenzene is detected by one chromatographic method, then confirmation shall be made using one or more alternative methods.6 Safety precautionsWARNING 4-am

44、inoazobenzene is classified as a substance known to be or suspected to be human carcinogen.Any handling and disposal of these substances shall be in strict accordance with the appropriate national health and safety regulations.It is the users responsibility to use safe and proper techniques in handl

45、ing materials in this test method. Consult manufacturers for specific details, such as material safety data sheets and other recommendations.7 ReagentsUnless otherwise specified, analytical grade chemicals shall be used.7.1 Aqueous sodium dithionite solution, = 200 mg/ml freshly prepared: rest the s

46、olution in a closed vessel for (55 1) min, transfer it into an open glass beaker, rest for 5 min (0 min, + 5 min) and then use within 10 min.7.2 Sodium hydroxide aqueous solution, = 2 %.1)1) = a mass fraction of 2%.2 ISO 2017 All rights reservedBS EN ISO 14362-3:2017ISO 14362-3:2017(E)7.3 Methanol.7

47、.4 Xylene (mixture of isomers) CAS No 1330-20-7.7.5 t-butyl methyl ether.7.6 Sodium chloride.7.7 4-aminoazobenzene, highest available defined purity standard.7.8 Internal standards for gas chromatography (IS), e.g. in the case of GC-MS analysis, one of the following internal standards can be used: I

48、S1: naphthalene-d8, CAS No.: 1146-65-2; IS2: 2,4,5-trichloroaniline, CAS No.: 636-30-6; IS3: anthracene-d10, CAS No.: 1719-06-8.7.9 Standard solutions.7.9.1 Internal standard solution, IS in t-butyl methyl ether, = 10,0 g/ml.7.9.2 4-aminoazobenzene calibration solution for checking the experimental

49、procedure and preparation of calibration solutions4-aminoazobenzene in methanol, = 500 g/ml.7.10 Grade 3 water, complying with ISO 3696.8 Apparatus8.1 Extraction apparatus, according to Figure 1, consisting of coil condenser NS 29/32, a hook made from an inert material to hold the specimen in place so that the condensed solvent drips onto the specimen, 100 ml round bottom flask NS 29/32, and heating source.Figure 1 Apparatus ISO 2017 All rights reserved 3BS EN ISO 14362-3:2017ISO 14362-3