1、October 2014 Translation by DIN-Sprachendienst.English price group 13No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).IC
2、S 59.080.01; 87.060.10!%;s%“2248002www.din.deDDIN EN ISO 16373-2Textiles Dyestuffs Part 2: General method for the determination of extractable dyestuffsincluding allergenic and carcinogenic dyestuffs (method usingpyridine-water) (ISO 16373-2:2014);English version EN ISO 16373-2:2014,English translat
3、ion of DIN EN ISO 16373-2:2014-10Textilien Farbstoffe Teil 2: Allgemeines Verfahren zur Bestimmung von extrahierbaren Farbstoffeneinschlielich allergener und karzinogener Farbstoffe (Pyridin-Wasser-Verfahren)(ISO 16373-2:2014);Englische Fassung EN ISO 16373-2:2014,Englische bersetzung von DIN EN ISO
4、 16373-2:2014-10Textiles Colorants Partie 2: Mthode gnrale de dtermination des colorants extractibles, notamment lescolorants allergnes et cancrignes (mthode utilisant un mlange pyridine/eau)(ISO 16373-2:2014);Version anglaise EN ISO 16373-2:2014,Traduction anglaise de DIN EN ISO 16373-2:2014-10www.
5、beuth.deDocument comprises 26 pagesIn case of doubt, the German-language original shall be considered authoritative.09.14 DIN EN ISO 16373-2:2014-10 2 A comma is used as the decimal marker. National foreword This document (EN ISO 16373-2:2014) has been prepared by Technical Committee ISO/TC 38 “Text
6、iles” in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-1
7、2 AA Textilchemische Prfverfahren und Fasertrennung. EN 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 method for the determination of extractable dyestuffs inc
8、luding allergenic and carcinogenic (method using pyridine-water) Part 3: Method for determination of carcinogenic extractable dyestuffs (method using triethylamine/methanol) The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 3696 DIN ISO 3696
9、 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16373-2 June 2014 ICS 59.080.01 English Version Textiles - Dyestuffs - Part 2: General method for the determination
10、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 (mthode utilisant un mlange pyridine/ea
11、u) (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 CEN on 3 June 2014. CEN members are bou
12、nd 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 may be obtained on application to the C
13、EN-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 notified to the CEN-CENELEC Management Centre
14、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, Iceland, Ireland, Italy, Latvia, Lithuania,
15、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 Management Centre: Avenue Marnix 17, B-1000 B
16、russels 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 EContents PageForeword .3Introduction .41 Scope .52 Normative references 53 Terms and definitions .54 Principle 55 Safety precautions 56 Reagents 67 Appa
17、ratus .67.1 Apparatus and auxiliaries for sample preparation 67.2 Chromatographic equipment (selected from the following).68 Procedure.78.1 Preparation of test specimen 78.2 Extraction 78.3 Detection and quantification of dyestuff 78.4 Calibration 79 Calculation and expression of the results 810 Tes
18、t report .8Annex A (normative) List of carcinogenic dyestuffs .9Annex B (normative) List of allergenic and other dyestuffs 10Annex C (normative) Calculation 11Annex D (informative) Examples of chromatographic methods.12Annex E (informative) Reliability of the method . 21Annex F (informative) Multipl
19、e-extraction of several textile fibres with pyridine/water 22Bibliography 242DIN EN ISO 16373-2:2014-10 EN ISO 16373-2:2014 (E) This document (EN ISO 16373-2:2014) has been prepared by Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI, in collabor
20、ation 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 endorsement, at the latest by December 2014, and conflicting national standards shall be withdrawn at the latest by December
21、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 identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organi
22、zations of the following 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, M
23、alta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. The text of ISO 16373-2:2014 has been approved by CEN as EN ISO 16373-2:2014 without any modification. ForewordEndorsement notice 3DIN EN ISO 16373-2:2014-10 EN ISO 16
24、373-2:2014 (E) IntroductionThe 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 othe
25、r parts of ISO 16373 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 aller
26、genic and carcinogenic 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 extr
27、action efficiency) 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 b
28、e detected and determined 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
29、be published.4DIN EN ISO 16373-2:2014-10 EN ISO 16373-2:2014 (E) 1 ScopeThis part of ISO 16373 specifies the analyses used to detect 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 Annexe
30、s A and B) the allergenic and carcinogenic dyestuffs which can be analysed using this method; the lists of dyestuffs are expandable.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated ref
31、erences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) appliesISO 3696, Water for analytical laboratory use Specification and test methods3 Terms and definitionsFor the purposes of this document, the following terms a
32、nd definitions apply.3.1allergenic dyestuffdyestuff which may cause an allergic skin reaction3.2carcinogenic dyestuffdyestuff which is classified as carcinogenic substanceNote 1 to entry: Harmonized classification according to the Globally harmonized system of classification and labelling of chemica
33、ls (GHS),2incorporated in EU Regulation 1272/2008 (CLP)3.4 PrincipleA coloured test specimen is selected from the textile article 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 spectrome
34、try (LC/MS).5 Safety precautionsWARNING The substances listed in Tables A.1, B.1 and B.2 are classified as substances known to be 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 a
35、nd safety regulations.5method. Consult manufacturers recommendations.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 pr
36、actice should be followed. Wear safety glasses in all laboratory areas and a single use dust respirator while handling powder dyestuffs.Attention is drawn to any national and local safety regulations.DIN EN ISO 16373-2:2014-10 EN ISO 16373-2:2014 (E) 6 ReagentsUnless otherwise specified, analytical
37、grade chemicals shall be used.6.1 Pyridine.6.2 Acetonitrile, chromatographic grade.6.3 Ammonium acetate.6.4 Tetrabutylammonium 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
38、the solution in a brown glass bottle.6.7 Individual stock solutions, prepared in pyridine-water 1:1, of all reference 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 use
39、d. The given purity has to be considered for the calculation (see Clause 9).7 Apparatus7.1 Apparatus and auxiliaries 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 th
40、at generates heat at a temperature of (100 2)C (thermal block or laboratory sand-bath, controllable).7.1.5 Autosampler 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 foll
41、owing)7.2.1 Equipment for LC/DAD High performance liquid chromatograph (HPLC), DAD detector, separating column,6DIN EN ISO 16373-2:2014-10 EN ISO 16373-2:2014 (E) guard column.7.2.2 Equipment for LC/MS High performance liquid chromatograph (HPLC), electrospray ion source, MS detector, separating col
42、umn, guard column.8 Procedure8.1 Preparation of test specimenThe test specimen shall be selected 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 sm
43、all 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).8.2 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
44、 reaches (100 2) C, and hold this temperature for (35 5) min.Check the time taken for the temperature 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 an
45、d 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 Detectio
46、n and quantification of dyestuffDyestuff detection can be performed using the above-specified chromatographic techniques (7.2). If other analytical techniques are used it shall be reported.Dyestuff quantification is performed by means of HPLC/DAD/MS.NOTE Some dyes can be quantified with HPLC/DAD.8.4
47、 CalibrationFor the calibration, the mixed standards of the reference substances listed in Table A.1 (and respectively in Tables B.1 and B.2) are prepared in pyridine/water (1:1). The stock solutions are used to prepare mixed standards with concentrations levels of 1 mg/l, 5 mg/l, 10 mg/l and 20 mg/
48、l related to dyestuff content.7DIN EN ISO 16373-2:2014-10 EN ISO 16373-2:2014 (E) 9 Calculation and expression of the resultsAmounts of dyestuff are usually calculated by means of a software program. The calculation can be carried out manually as described in Annex C.Amounts of dyestuff are expressed in mg dyestuff per kg of textile (mg/kg).If the detected amount of a dye is over 100 mg/kg, it is certain that this dye is used such as one of those listed in Table A.1, B.1 or B.2.10 Test re
