SIST EN 14362-2:2003

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 2: Verwendungsnachweis bestimmter Azofarbstoffe durch Extraktion der FasernTextiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoiques - Partie 2: Détection de l'utilisation de certains colorants azoiques accessibles par l'extraction des fibresTextiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 2: Detection of the use of certain azo colorants accessible by extracting the fibres59.080.01Tekstilije na splošnoTextiles in generalICS:Ta slovenski standard je istoveten z:EN 14362-2:2003SIST EN 14362-2:2003en01-december-2003SIST EN 14362-2:2003SLOVENSKI
STANDARD



SIST EN 14362-2:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14362-2October 2003ICS 59.080.30English versionTextiles - Methods for determination of certain aromatic aminesderived from azo colorants - Part 2: Detection of the use ofcertain azo colorants accessible by extracting the fibresTextiles - Méthodes de détermination de certaines aminesaromatiques dérivées de colorants azoïques - Partie 2:Détection de l'utilisation de certains colorants azoïquesaccessibles par l'extraction des fibresTextilien - Verfahren für die Bestimmung bestimmteraromatischer Amine aus Azofarbstoffen - Teil 2:Verwendungsnachweis bestimmter Azofarbstoffe durchExtraktion der FasernThis European Standard was approved by CEN on 1 September 2003.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14362-2:2003 ESIST EN 14362-2:2003



EN 14362-2:2003 (E)2ContentspageForeword.31Scope.42Normative references.43General.44Principle.55Safety precautions.66Reagents.67Apparatus.78Procedure.88.1Preparation of test specimens.88.2Extraction.88.3Reductive cleavage.88.4Separation and concentration of the amines.88.5Amine detection and quantification.99Evaluation.99.1Calculation.99.2Reliability of the method.910Test report.9Annex A (informative)
Chromatographic analyses.10A.1Preliminary remark.10A.2Thin layer chromatography (TLC).10A.3High performance liquid chromatography (HPLC).11A.4Capillary gas chromatography (GC).11A.5Capillary electrophoresis (CE).12A.6Check of the analytical system.12Annex B (normative)
Calculation.14Annex C (informative)
Reliability of the method.15Annex D (informative)
Assessment guide-interpretation of analytical results.16Annex E (informative) Apparatus - Extractor according to Baumgarte.17SIST EN 14362-2:2003



EN 14362-2:2003 (E)3ForewordThis document (EN 14362-2:2003) has been prepared by Technical Committee CEN/TC 248 “Textiles and textileproducts”, 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 orby endorsement, at the latest by April 2004, and conflicting national standards shall be withdrawn at the latest byApril 2004.Annexes A, C, D and E are informative.
Annex B is normative.This European Standard calls for the use of substances and/or procedures that may be injurious to healthif appropriate precautions are not observed. It refers only to technical suitability and does not absolve theuser from legal obligations relating to health and safety at any stage.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 14362-2:2003



EN 14362-2:2003 (E)41 ScopeThis part of EN 14362 describes a procedure to detect the use of certain azo colorants that may not be used in themanufacture or treatment of certain commodities made of synthetic fibres dyed with extractable dyes.For the direct test method, see EN 14362-1 Detection of the use of certain azo colorants accessible withoutextraction.For certain fibre blends both parts of this standard may need to be applied.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references subsequent amendments to, or revisions of, any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)ISO 4787, Laboratory glassware — Volumetric glassware – Methods for use and testing of capacity3 GeneralCertain azo colorants may release, by reductive cleavage of azo group(s), one or more of the following aromaticamines, which are proscribed under Directive 2002/61/EC.Table 1 – Aromatic amines proscribed under Directive 2002/61/EC.No.CAS numberIndexnumberEC numberSubstances192-67-1612-072-00-6202-177-1biphenyl-4-ylamin4-aminobiphenylxenylamine292-87-5612-042-00-2202-199-1benzidine395-69-2202-441-64-chloro-o-toluidine491-59-8612-022-00-3202-080-42-naphthylamine5*97-56-3611-006-00-3202-591-2o-aminoazotoluene4-amino-2',3-dimethylazobenzene4-o-tolylazo-o-toluidine6*99-55-8202-765-85-nitro-o-toluidine7106-47-8612-137-00-9203-401-04-chloroaniline8615-05-4210-406-14-methoxy-m-phenylenediamineSIST EN 14362-2:2003



EN 14362-2:2003 (E)59101-77-9612-051-00-1202-974-44,4'-methylenedianiline4,4'-diaminodiphenylmethane1091-94-1612-068-00-4202-109-03,3'-dichlorobenzidine3,3'-dichlorobiphenyl-4,4'-ylenediamine11119-90-4612-036-00-X204-355-43,3'-dimethoxybenzidineo-dianisidine12119-93-7612-041-00-7204-358-03,3'-dimethylbenzidine4,4'-bi-o-toluidine13838-88-0612-085-00-7212-658-84,4'-methylenedi-o-toluidine14120-71-8204-419-16-methoxy-m-toluidinep-cresidine15101-14-4612-078-00-9202-918-94,4'-methylene-bis-(2-chloro-aniline)2,2'-dichloro-4.4’-methylene-dianiline16101-80-4202-977-04,4'-oxydianiline17139-65-1205-370-94,4'-thiodianiline1895-53-4612-091-00-X202-429-0o-toluidine2-aminotoluene1995-80-7612-099-00-3202-453-14-methyl-m-phenylenediamine20137-17-7205-282-02,4,5-trimethylaniline2190-04-0612-035-00-4201-963-1o-anisidine2-methoxyaniline22**60-09-3611-008-00-4200-453-64-aminoazobenzene*The CAS-numbers 97-56-3 (No. 5) and 99-55-8 (No. 6) are
further reduced to CAS-numbers 95-53-4 (No.18) and 95-80-7 (No. 19).** Azo colorants that are able to form 4-aminoazobenzene, generate under the condition of this methodaniline and 1,4-phenylenediamine. The presence of these colorants cannot be reliably ascertained withoutadditional information, e.g. the chemical structure of the colorant used.4 PrincipleThe colorant is extracted (see Figure 1) from the fibre in the headspace using appropriate solvents under reflux, forexample for polyester fibres use chlorobenzene. The extract is concentrated, transferred with methanol, taken up inaqueous citrate-buffer solution and treated in an ultrasonic bath for dispersion of the colorant.The amines formed by adding sodium dithionite are transferred to a t-butyl methyl ether phase by means of liquid-liquid extraction using diatomaceous earth columns. The extract is concentrated, and the residue is taken up inmethanol or a solvent appropriate for detection and determination of the amines using chromatography.If the amines are detected by one chromatographic method, then confirmation shall be made using one or morealternative methods.SIST EN 14362-2:2003



EN 14362-2:2003 (E)65 Safety precautions5.1GeneralWARNING The substances [amines] listed in Table 1 are classified as substances known to be orsuspected to be human carcinogens.Any handling and disposal of these substances shall be in strict accordance with the appropriate nationalhealth and safety regulations.5.2It is the user’s 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.5.3Good laboratory practice should be followed. Wear safety glasses in all laboratory areas and a single-usedust respirator while handling powder colorants.5.4Users should comply with any national and local safety regulations.6 Reagents6.1GeneralUnless otherwise specified, analytical grade chemicals have to be used.6.2chlorobenzene6.3methanol6.4ethyl acetate6.5t-butyl methyl ether6.6citrate/sodium hydroxide buffer solution, pH = 6, c = 0,06 mol/ml1)6.7aqueous sodium dithionite solution,
= 200 mg/m, l2) freshly (daily) prepared6.8diatomaceous earth6.9amine substances - amines 1 to 4, 7 to 21 (as specified in Table 1), and aniline and 1,4-phenylenediamine -all of highest available defined purity standard6.10standard solutions6.10.1calibration solution of amines (see
6.9)
= 15,0 g of each amine per millilitre of an appropriatesolvent6.10.2an appropriate mixture of internal standards in solution,
= 10,0 g of each IS/ml of the appropriate ISsolventNOTE IS1: naphthalene-d8, CAS No.: 1146-65-2
IS2: 2,4,5-trichloroaniline, CAS No.: 636-30-6
IS3: 4-aminoquinaldine, CAS No.: 6628-04-2
1)c is citrate concentration.2) is the mass concentrationSIST EN 14362-2:2003



EN 14362-2:2003 (E)7
IS4: anthracene-d10, CAS No.: 1719-06-8.6.10.3solution of amine (see 6.9) for checking the experimental procedure,
= 30,0 g of each amine permillilitre methanol6.11grade 3 water, complying with EN ISO 3696.7 Apparatus7.1extraction apparatus, according to Figure 1, consisting ofcoil condenser NS 29/32a hook, made from an inert material to hold the specimen in place so that the condensed solvent drips onto
the specimens100 ml round bottom flask NS 29/32heating sourceFigure 1 — ApparatusNOTESimilar apparatus can be used, if the same results are obtained. (See annex E.)7.2ultrasonic bath, controllable heating7.3reaction vessel (20 ml to 50 ml) of heat-resistant glass, with tight closure7.4heating source that generates (70
2) C7.5glass or polypropylene column, inside diameter 25 mm to 30 mm, length 140 mm to 150 mm, packed wit
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