1、BSI Standards PublicationBS EN ISO 16373-3:2014T e x t i l e s D y e s t u f f sPart 3: Method for determination of certain carcinogenic dyestuffs (method using triethylamine/methanol)BS EN ISO 16373-3:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 163
2、73-3:2014.The UK participation in its preparation was entrusted to Technical Committee TCI/80, Chemical testing of textiles.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
3、 contract. Users are responsible for its correct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 73784 8ICS 59.080.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under th
4、e authority of the Standards Policy and Strategy Committee on 30 June 2014.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16373-3 June 2014 ICS 59.080.01 English Version Textiles - Dyestuffs - Part 3: Method for dete
5、rmination of certain carcinogenic dyestuffs (method using triethylamine/methanol) (ISO 16373-3:2014) Textiles - Colorants - Partie 3: Mthode de dtermination de certains colorants cancrignes (mthode la trithylamine et au mthanol) (ISO 16373-3:2014) Textilien - Farbstoffe - Teil 3: Verfahren zur Besti
6、mmung von bestimmten karzinogenen Farbstoffen (Triethylamin/Methanol-Verfahren) (ISO 16373-3:2014) This European Standard was approved by CEN on 17 April 2014. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard t
7、he 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 Management Centre or to any CEN member. This European Standard exists in three official versions (English, Fre
8、nch, 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 status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria
9、, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav 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
10、 and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management 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
11、. No. EN ISO 16373-3:2014 EBS EN ISO 16373-3:2014BS EN ISO 16373-3:2014EN ISO 16373-3:2014 (E) 3 Foreword This document (EN ISO 16373-3:2014) has been prepared by Technical Committee ISO/TC 38 “Textiles” in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secreta
12、riat 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 December 2014, and conflicting national standards shall be withdrawn at the latest by December 2014. Attention is draw
13、n 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. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the followin
14、g countries are bound to implement this European Standard: 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, Malta, Netherlands, Norw
15、ay, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 16373-3:2014 has been approved by CEN as EN ISO 16373-3:2014 without any modification. BS EN ISO 16373-3:2014ISO 16373-3:2014(E) ISO 2014 All rights reserv
16、ed iiiContents PageForeword ivIntroduction v1 Scope . 12 Terms and definitions . 13 Principle 14 Safety precautions 24.1 General . 24.2 Handling 25 Apparatus . 26 Reagents 37 Test specimen sampling and preparation 37.1 General . 38 Procedure. 38.1 Extraction 38.2 Detection, identification and quanti
17、fication of carcinogenic dyestuffs 49 Test report . 4Annex A (informative) Chromatographic analysis . 5Annex B (informative) Round robin test results .22Bibliography .27BS EN ISO 16373-3:2014ISO 16373-3:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation
18、 of national 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.
19、International 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
20、 intended for its 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. ww
21、w.iso.org/directivesAttention 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 wi
22、ll be in the Introduction and/or on the ISO list of patent declarations received. www.iso.org/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 r
23、elated to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 38.ISO 16373 consists of the following parts, u
24、nder the general title Textiles Dyestuffs: Part 1: General principles of testing coloured textiles for dyestuff identification Part 2: General method for the determination of extractable dyestuffs including allergenic and carcinogenic dyestuffs (method using pyridine-water) Part 3: Method for determ
25、ination of certain carcinogenic dyestuffs (method using triethylamine/methanol)iv ISO 2014 All rights reservedBS EN ISO 16373-3:2014ISO 16373-3:2014(E)IntroductionDue to concerns of consumers over safety and hygiene, many countries have introduced regulations regarding carcinogenic dyestuffs in text
26、ile articles. To support international and national regulations the development of a test method is very important and this part of ISO 16373 does just that.The ISO 16373 series deal with dyestuffs used in textile for qualification and quantification. ISO 16373-11)includes the definition of the dyes
27、tuff, and classes the description of some procedures to identify qualitatively the dyestuff class used in textile material. The other parts of ISO 16373 are related to the quantification of some dyestuffs. In ISO 16373-2, the principle of the test method is based on extraction using pyridine-water s
28、olution, which has been found to be the most efficient solution to extract a large range of dyestuffs, including allergenic and carcinogenic dyestuffs. In this part of ISO 16373, the principle of the test method is based on extraction using triethylamine-methanol solution. This solution has been fou
29、nd to be efficient at extracting some dyestuffs in some cases.Additional information related to the recovery rate (to characterize the extraction efficiency) obtained from the application of ISO 16373-2 and this part of ISO 16373 is summarized in ISO 16373-1:, Annex B.It is important to note that th
30、ere are other test methods related to azo dyes, for which a reduction of the extracted azo dyes leads to the release of some aromatic amines to be detected and determined using chromatography.671) To be published. ISO 2014 All rights reserved vBS EN ISO 16373-3:2014BS EN ISO 16373-3:2014Textiles Dye
31、stuffs Part 3: Method for determination of certain carcinogenic dyestuffs (method using triethylamine/methanol)1 ScopeThis part of ISO 16373 specifies a method for the detection and quantitative determination of the presence of carcinogenic dyestuffs as listed in Table 1 in dyed, printed or coated t
32、extile products by chromatographic analysis of their extracts.2 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.2.1textilewoven fabric, knitted fabric, etc., formed by the interlocking of fibres and yarns having a certain cohesion and which is genera
33、lly intended for clothing or furniture applicationsNote 1 to entry: Textiles often include certain types of non-woven fabrics.2.2carcinogenic dyestuffsubstance yielding a dye that is a substance known to be or suspected of being a human carcinogen3 PrincipleThe dyestuff of a coloured test specimen i
34、s extracted by means of a solvent in an ultrasonic bath under specified conditions. The extract is analysed using either a high-performance liquid chromatography photodiode array detector (HPLC-DAD) or a high-performance liquid chromatography mass spectrometer (HPLC-MSD).The carcinogenic dyestuffs a
35、re listed in Table 1.Table 1 List of carcinogenic dyestuffsC.I. Generic name CAS numberC.I. Constitution numberC.I. Basic Red 9 569619 42500C.I. Disperse Orange 11 82280 60700C.I. Disperse Yellow 3 2832408 11855C.I. Acid Red 114 6459945 23635C.I. Acid Red 26 3761533 16150C.I. Direct Black 38 1937377
36、 30235C.I. Direct Red 28 573580 22120C.I. Disperse Blue 1 2475458 64500INTERNATIONAL STANDARD ISO 16373-3:2014(E) ISO 2014 All rights reserved 1BS EN ISO 16373-3:2014ISO 16373-3:2014(E)C.I. Generic name CAS numberC.I. Constitution numberC.I. Basic Violet 14 632995 42510C.I. Direct Blue 6 2602462 226
37、10C.I. Direct Brown 95 16071866 301454 Safety precautions4.1 GeneralWarning The dyestuffs targeted in this part of ISO 16373 are classified as substances known to be or suspected of being human carcinogens.4.2 HandlingIt is the users responsibility to ensure any handling and disposal of these substa
38、nces are in strict accordance with the appropriate national health and safety regulations.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 recommendati
39、ons.Good laboratory practice should be followed. Wear safety glasses in all laboratory areas and single-use dust respirator while handling the dyestuff powder.5 Apparatus5.1 Ultrasonic bath, capable of heating to and maintaining at (50 5) C and output power of 40 W, oscillating frequency, 42 kHz, or
40、 equivalent.5.2 Coil condenser, for chemical testing use.5.3 Vacuum rotary evaporator, capable of operating at water evaporation capacity of a maximum of 25 ml/min, or equivalent.5.4 Round bottom flask, of 200 ml in capacity.5.5 Pipettes, of 1 ml and 10 ml in capacity.5.6 Volumetric flask, of 10 ml,
41、 100 ml and 1 l in capacity.5.7 High-performance liquid chromatography (HPLC) system and diode array detector (DAD) or mass spectroscope (MSD).5.8 Test tube, of 100 ml in capacity, with a silicone plug.NOTE For details of the high-performance liquid chromatography equipment, see Annex A.5.9 Analytic
42、al balance, of 0,001 g in resolution.Table 1 (continued)2 ISO 2014 All rights reservedBS EN ISO 16373-3:2014ISO 16373-3:2014(E)6 ReagentsUnless otherwise specified, use only reagents of recognized analytical grade.6.1 Acetonitrile.6.2 Methanol.6.3 Hexane.6.4 0,25 % tri-ethylamine methanol solution,
43、2,5 ml triethylamine is dissolved in methanol and made up to 1 l.6.5 10 mmol/l ammonium acetate aqueous solution, 0,77 g ammonium acetate is dissolved in water and made up to 1 l.6.6 Carcinogenic dyestuffs. Use only carcinogenic dyestuffs of reagent grade of the highest purity available on the marke
44、t, or dyestuffs of which quantities of the dye are manufactured in controlled environments within Europe under the control of the EU creating standard dyestuffs.6.7 Standard solution of carcinogenic dyestuffs.An amount of each carcinogenic dyestuff is weighed accurately in the range of 1 mg to 10 mg
45、 and transferred quantitatively to a 10 ml volumetric flask, and then made up to volume with methanol (6.2) to prepare a standard solution in the range of 100 ug/ml to 1 000 ug/ml.The standard solution may be diluted properly and four solutions with known concentrations may be made to draw the calib
46、ration curve. As an example, the range of concentration of standard solutions for the calibration curve can be recommended to be from 1 g/ml to 100 g/ml.7 Test specimen sampling and preparation7.1 GeneralThe test specimen shall be selected based on the following criteria: parts of the textile articl
47、e; nature of the fibre component (fibre composition); colours.Prepare a test specimen of maximum 1,0 g (1,0 g) 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 g and record it as mE(see 8.2).8 Procedure8.1 Extract
48、ion8.1.1 CleansingIf required, remove oil, grease or other fatty matter from the surface of the test specimen by soaking it in 100 ml hexane (6.3) for 5 min in an ultrasonic bath (5.1) at ambient temperature. ISO 2014 All rights reserved 3BS EN ISO 16373-3:2014ISO 16373-3:2014(E)Remove and drain the
49、 test specimen.8.1.2 Extraction of dyestuffPlace 1,0 g of the test specimen in a 100 ml test tube. Add 100 ml of the 0,25 % tri-ethylamine methanol solution (6.4) and seal the test tube using a silicone plug. Heat the tube in an ultrasonic bath until a temperature of 50 C 2 C is reached and maintained this temperature for 3 h.8.1.3 Concentration of extract and preparation of analysis solutionTransfer the extract obtained according to 8.1.2 to a 200 ml round botto
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