1、October 2014 Translation by DIN-Sprachendienst.English price group 15No 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!%;r“2247998www.din.deDDIN EN ISO 16373-3Textiles Dyestuffs Part 3: Method for determination of certain carcinogenic dyestuffs(method using triethylamine/methanol) (ISO 16373-3:2014);English version EN ISO 16373-3:2014,English translation of DIN EN ISO 16373-3:2014-10Textilien
3、Farbstoffe Teil 3: Verfahren zur Bestimmung von bestimmten karzinogenen Farbstoffen(Triethylamin/Methanol-Verfahren) (ISO 16373-3:2014);Englische Fassung EN ISO 16373-3:2014,Englische bersetzung von DIN EN ISO 16373-3:2014-10Textiles Colorants Partie 3: Mthode de dtermination de certains colorants c
4、ancrignes (mthode latrithylamine et au mthanol) (ISO 16373-3:2014);Version anglaise EN ISO 16373-3:2014,Traduction anglaise de DIN EN ISO 16373-3:2014-10www.beuth.deDocument comprises 33 pagesIn case of doubt, the German-language original shall be considered authoritative.09.14 DIN EN ISO 16373-3:20
5、14-10 2 A comma is used as the decimal marker. National 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” (Secretariat: BSI, United Kingdom). The responsible
6、German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-12 AA Textilchemische Prfverfahren und Fasertrennung. EN ISO 16373 consists of the following parts, under the general title Textiles Dyestuffs:
7、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 (method using pyridine-water) Part 3: Method for determination of carcinogenic extractable dyestuffs (method
8、 using triethylamine/methanol) The DIN Standards corresponding to the International Standard referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 4787 DIN EN ISO 4787 ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliography DIN EN ISO 4787, Laboratory glassware Volume
9、tric instruments Methods for testing of capacity and for use DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproduci
10、bility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16373-3 June 2014 ICS 59.080.01 English Version Textiles - Dyestuffs - Part 3: Method for determination of certain carcinogenic dyestuffs (method using triethylamine/methanol) (ISO 16373-3:2014) Textiles
11、 - 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 Bestimmung von bestimmten karzinogenen Farbstoffen (Triethylamin/Methanol-Verfahren) (ISO 16373-3:2014) This Europ
12、ean 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 the status of a national standard without any alteration. Up-to-date lists and bibliographical references conc
13、erning 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, French, German). A version in any other language made by translation under the responsibility of a CEN member in
14、to 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, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France,
15、Germany, Greece, Hungary, Iceland, 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 KOMITE
16、E 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. No. EN ISO 16373-3:2014 EContents PageForeword .3Introduction .41 Scope .52 Terms and definitions .53 Princ
17、iple 54 Safety precautions . 64.1 General .64.2 Handling65 Apparatus .66 Reagents 77 Test specimen sampling and preparation 77.1 General .78 Procedure.78.1 Extraction . 78.2 Detection, identification and quantification of carcinogenic dyestuffs . 89 Test report 8Annex A (informative) Chromatographic
18、 analysis 9Annex B (informative) Round robin test results 26Bibliography .312DIN EN ISO 16373-3:2014-10 EN ISO 16373-3:2014 (E) 3This 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 textil
19、e 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 December 2014, and conflicting national standards shall be withdrawn at the latest by December
20、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
21、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
22、alta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement noticeThe text of ISO 16373-3:2014 has been approved by CEN as EN ISO 16373-3:2014 without any modification. Foreword DIN EN ISO 16373-3:2014-10 EN ISO 163
23、73-3:2014 (E) IntroductionDue to concerns of consumers over safety and hygiene, many countries have introduced regulations regarding carcinogenic dyestuffs in textile articles. To support international and national regulations the development of a test method is very important and this part of ISO 1
24、6373 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 dyestuff, and classes the description of some procedures to identify qualitatively the dyestuff class used in textile material. The other par
25、ts 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 solution, which has been found to be the most efficient solution to extract a large range of dyestuffs, including allergenic and carcinoge
26、nic 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 found to be efficient at extracting some dyestuffs in some cases.Additional information related to the recovery rate (to characterize the ex
27、traction 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 there are other test methods related to azo dyes, for which a reduction of the extracted azo dyes leads to the release of some aromatic ami
28、nes to be detected and determined using chromatography.671) To be published.4DIN EN ISO 16373-3:2014-10 EN ISO 16373-3:2014 (E) 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, pr
29、inted or coated textile 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 an
30、d which is generally 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 coloure
31、d test specimen is 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 carcino
32、genic dyestuffs are 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
33、 Black 38 1937377 30235C.I. Direct Red 28 573580 22120C.I. Disperse Blue 1 2475458 645005C.I. Basic Violet 14 632995 42510C.I. Direct Blue 6 2602462 22610C.I. Direct Brown 95 16071866 30145DIN EN ISO 16373-3:2014-10 EN ISO 16373-3:2014 (E) 4 Safety precautions4.1 GeneralWarning The dyestuffs targete
34、d 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 substances are in strict accordance with the appropriate national health and safety regulations.It is t
35、he 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 laboratory areas and
36、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 equivalent.5.2 Coil condenser, for chemical testing use.5.3 Vacuum rotary evaporator, capable of
37、 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, 100 ml and 1 l in capacity.5.7 High-performance liquid chromatography (HPLC) system and diode ar
38、ray 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 Analytical balance, of 0,001 g in resolution.6DIN EN ISO 16373-3:2014-10 EN ISO 16373-3:2014 (E) 6 Reagen
39、tsUnless 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, 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 aceta
40、te 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 market, or dyestuffs of which quantities of the dye are manufactured in controlled environments within Europe under the control of the EU cr
41、eating 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 and transferred quantitatively to a 10 ml volumetric flask, and then made up to volume with methanol (6.2) to prepare a standard solut
42、ion 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 calibration curve. As an example, the range of concentration of standard solutions for the calibration curve can be recommended to be from 1
43、 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 article; nature of the fibre component (fibre composition); colours.Prepare a test specimen of maximum 1,0 g (1,0 g) by cutting the laborator
44、y 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 Extraction8.1.1 CleansingIf required, remove oil, grease or other fatty matter from the surface of the test specimen by soaking it in 100 ml h
45、exane (6.3) for 5 min in an ultrasonic bath (5.1) at ambient temperature.7DIN EN ISO 16373-3:2014-10 EN ISO 16373-3:2014 (E) Remove and drain the 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 solutio
46、n (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
47、 round bottom flask (5.4) and place it in a vacuum rotary evaporator (5.3) in the water bath at 40 C 2 C until all the liquid has evaporated.Dissolve the residue in 1 ml of methanol. Filter the solution through a 0,45 m PTFE filter. If the resultant measurement is higher than the calibrated range of
48、 the chromatograph, dilute the solution further with methanol.8.2 Detection, identification and quantification of carcinogenic dyestuffsDetection of carcinogenic dyestuffs is performed by the chromatographic analysis using the apparatus described in 5.7. When the carcinogenic dyestuffs are identified by comparing with peaks of reference carcinogenic dyestuffs, quantification is performed using a calibration curve, which is draw
