EN ISO 16373-2-2014 en Textiles - Dyestuffs - Part 2 General method for the determination of extractable dyestuffs including allergenic and carcinogenic dyestuffs (method using pyr.pdf

1、BSI Standards PublicationBS EN ISO 16373-2:2014Textiles DyestuffsPart 2: General method for thedetermination of extractable dyestuffsincluding allergenic and carcinogenicdyestuffs (method using pyridine-water)(ISO 16373-2:2014)BS EN ISO 16373-2:2014 BRITISH STANDARDNational forewordThis British Stan

2、dard is the UK implementation of EN ISO16373-2:2014.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to i

3、nclude all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 76070 9ICS 59.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This Br

4、itish Standard was published under the authority of theStandards Policy and Strategy Committee on 31 October 2014.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16373-2 June 2014 ICS 59.080.01 English Version Textiles - Dyestuffs - Part

5、2: General method for the determination of extractable dyestuffs including allergenic and carcinogenic dyestuffs (method using pyridine-water) (ISO 16373-2:2014) Textiles - Colorants - Partie 2: Mthode gnrale de dtermination des colorants extractibles, notamment les colorants allergnes et cancrignes

6、 (mthode utilisant un mlange pyridine/eau) (ISO 16373-2:2014) Textilien - Farbstoffe - Teil 2: Allgemeines Verfahren zur Bestimmung von extrahierbaren Farbstoffen einschlielich allergener und karzinogener Farbstoffe (Pyridin-Wasser-Verfahren) (ISO 16373-2:2014) This European Standard was approved by

7、 CEN on 3 June 2014. CEN members are bound to comply 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

8、 may be obtained on application to the CEN-CENELEC Management 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 notifi

9、ed to the CEN-CENELEC Management Centre has the same 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, Icel

10、and, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Manag

11、ement Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 16373-2:2014 EBS EN ISO 16373-2:2014EN ISO 16373-2:2014 (E) 3 Foreword This document (EN ISO 16373-2:2014) has been prepared b

12、y Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI, in collaboration with Technical Committee ISO/TC 38 “Textiles“. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsem

13、ent, at the latest by December 2014, and conflicting national standards shall be withdrawn at the latest by December 2014. 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 identi

14、fying any or all such patent rights. 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 Yugosl

15、av Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 16373-2:2014 ha

16、s been approved by CEN as EN ISO 16373-2:2014 without any modification. BS EN ISO 16373-2:2014ISO 16373-2:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Safety precautions 16 Reagents 27 Appar

17、atus . 27.1 Apparatus and auxiliaries for sample preparation 27.2 Chromatographic equipment (selected from the following). 28 Procedure. 38.1 Preparation of test specimen 38.2 Extraction 38.3 Detection and quantification of dyestuff 38.4 Calibration 39 Calculation and expression of the results 410 T

18、est report . 4Annex A (normative) List of carcinogenic dyestuffs . 5Annex B (normative) List of allergenic and other dyestuffs 6Annex C (normative) Calculation . 7Annex D (informative) Examples of chromatographic methods 8Annex E (informative) Reliability of the method 17Annex F (informative) Multip

19、le-extraction of several textile fibres with pyridine/water 18Bibliography .20BS EN ISO 16373-2:2014ISO 16373-2:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Stan

20、dards 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 t

21、ake 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 maintenance are described in the ISO/IEC Directives, Part 1. In p

22、articular 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. www.iso.org/directivesAttention is drawn to the possibility that some of the elements of this

23、 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 Introduction and/or on the ISO list of patent declarations received. www.iso.o

24、rg/patentsAny 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 meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO pri

25、nciples in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 16373-2 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 248, Textiles and textile products, in collaboration with ISO Technical Committee TC 38,

26、 Textiles, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).ISO 16373 consists of the following parts, under the general title Textiles Dyestuffs: Part 1: General principles of testing coloured textiles for dyestuff identification Part 2: General metho

27、d for the determination of extractable dyestuffs including allergenic and carcinogenic (method using pyridine-water) Part 3: Method for determination of carcinogenic extractable dyestuffs (method using triethylamine/methanol)iv ISO 2014 All rights reservedBS EN ISO 16373-2:2014ISO 16373-2:2014(E)Int

28、roductionThe ISO 16373 series deals with dyestuffs used in textile for qualification and quantification.ISO 16373-11)includes the definition of the dyestuff classes and the description of some procedures to identify qualitatively the dyestuff class used in textile material.The other parts of ISO 163

29、73 are related to the quantification of some dyestuffs.In this part of ISO 16373, the principle of the test method is based on the extraction using pyridine-water solution, which has been found to be the most efficient solution to extract a large range of dyestuffs, including allergenic and carcinog

30、enic dyestuffs.In ISO 16373-3, the principle of the test method is based on extraction using triethylamine/methanol solution. This solution has been found efficient to extract some dyestuffs in some cases.Additional information related to the recovery rate (to characterize the extraction efficiency)

31、 obtained from the application of ISO 16373-3 and this part of ISO 16373 will be summarized in ISO 16373-1.It is important to note that other test methods exist related to azo dyes, for which a reduction of those extracted azo dyes leads to the release of some aromatic amines, to be detected and det

32、ermined using chromatography.The percentage of recovery using the method of this part of ISO 16373 is shown in Annex F for the dyestuff classes (to be defined in ISO 16373-1) acid, basic, direct, disperse, solvent dyestuffs and “mordant dyestuffs” on different textile fibres.1) To be published. ISO

33、2014 All rights reserved vBS EN ISO 16373-2:2014BS EN ISO 16373-2:2014Textiles Dyestuffs Part 2: General method for the determination of extractable dyestuffs including allergenic and carcinogenic dyestuffs (method using pyridine-water)1 ScopeThis part of ISO 16373 specifies the analyses used to det

34、ect extractable dyestuffs in textile products, with the extraction performed for all kind of fibres and types of dyestuffs using pyridine/water (1:1). It lists (see Annexes A and B) the allergenic and carcinogenic dyestuffs which can be analysed using this method; the lists of dyestuffs are expandab

35、le.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any ame

36、ndments) appliesISO 3696, Water for analytical laboratory use Specification and test methods3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1allergenic dyestuffdyestuff which may cause an allergic skin reaction3.2carcinogenic dyestuffdyestuff whi

37、ch is classified as carcinogenic substanceNote 1 to entry: Harmonized classification according to the Globally harmonized system of classification and labelling of chemicals (GHS),2incorporated in EU Regulation 1272/2008 (CLP)3.4 PrincipleA coloured test specimen is selected from the textile article

38、 and extracted with pyridine/water at 100 C. The extract is analysed by liquid chromatography/diode array detection (LC/DAD) and/or by liquid chromatography/mass spectrometry (LC/MS).5 Safety precautionsWARNING The substances listed in Tables A.1, B.1 and B.2 are classified as substances known to be

39、 or suspected to be human allergens or carcinogens.Ensure that any handling and disposal of these substances is in strict accordance with the appropriate national health and safety regulations.INTERNATIONAL STANDARD ISO 16373-2:2014(E) ISO 2014 All rights reserved 1BS EN ISO 16373-2:2014ISO 16373-2:

40、2014(E)It is the users responsibility to use safe and proper techniques in handling materials in this test method. Consult manufacturers for specific details such as material safety data sheets and other recommendations.Good laboratory practice should be followed. Wear safety glasses in all laborato

41、ry areas and a single use dust respirator while handling powder dyestuffs.Attention is drawn to any national and local safety regulations.6 ReagentsUnless otherwise specified, analytical grade chemicals shall be used.6.1 Pyridine.6.2 Acetonitrile, chromatographic grade.6.3 Ammonium acetate.6.4 Tetra

42、butylammonium dihydrogen phosphate.6.5 Deionized water, grade 3 in accordance with ISO 3696.6.6 Pyridine/water (1:1), prepared by mixing 500 ml pyridine (6.1) and 500 ml water (6.5).Keep the solution in a brown glass bottle.6.7 Individual stock solutions, prepared in pyridine-water 1:1, of all refer

43、ence substances listed in Annexes A and BIt is recommended that reference substances (including those listed in Annexes A and B) of the highest purity grade available on the market be used. The given purity has to be considered for the calculation (see Clause 9).7 Apparatus7.1 Apparatus and auxiliar

44、ies for sample preparation7.1.1 Standard laboratory equipment.7.1.2 Analytical balance, resolution at 0,01 g.7.1.3 Glass vials (20 ml to 40 ml), with tight closure.7.1.4 Heating source that generates heat at a temperature of (100 2)C (thermal block or laboratory sand-bath, controllable).7.1.5 Autosa

45、mpler glass vials, with tight closure. 7.1.6 Thermo-sensing device, e.g. thermocouple, to measure at 100 C with a resolution of 0,1 C.7.2 Chromatographic equipment (selected from the following)7.2.1 Equipment for LC/DAD High performance liquid chromatograph (HPLC), DAD detector, separating column,2

46、ISO 2014 All rights reservedBS EN ISO 16373-2:2014ISO 16373-2:2014(E) guard column.7.2.2 Equipment for LC/MS High performance liquid chromatograph (HPLC), electrospray ion source, MS detector, separating column, guard column.8 Procedure8.1 Preparation of test specimenThe test specimen shall be selec

47、ted based on the following criteria: parts of the textile article; nature of the fibre component (fibre composition); colours.Prepare a test specimen of 1,0 g max. by cutting the laboratory sample up into small pieces no larger than 1 cm2. Determine the mass of the test specimen to the nearest 0,01

48、g and record it as mE(see 8.2).8.2 ExtractionAdd 7,5 ml of pyridine/water (1:1) (6.6) to the test specimen and close the vial tightly. Heat the vial in the heating source until the temperature of the solvent reaches (100 2) C, and hold this temperature for (35 5) min.Check the time taken for the tem

49、perature of the solvent to reach the required temperature using a glass vial (see 8.1) containing 7,5 ml of pyridine/water (1:1)(6.6) with a thermo-sensing element (7.1.6), which is plunged in the solvent and sealed with a septum.Allow the vial to cool down to 40 C or below before opening it.Transfer approximately 1 ml of (test) liquid from the vial to a smaller vial for further analysis.NOTE This step could be done with a syringe through the closed septum to minimize contact with pyridine.8.3 Detection and quanti