Textiles - Methods for the determination of certain aromatic amines derived from azo colorants - Part 1: Detection of the use of certain azo colorants accessible without extraction

This part of prEN 14362 describes a procedure to detect the use of certain azo colorants that may not be used in the manufacture or treatment of certain commodities made of textile fibres and that are accessible to reducing agent without extraction, particularly textiles made of cellulose and protein fibres (e.g. cotton, viscose, wool, silk).
For the extraction test method see prEN 14362-2 Detection of the use of certain azo colorants accessible by extracting the fibres
For certain fibre blends both parts of this standard may need to be applied.

Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 1: Verwendungsnachweis bestimmter Azofarbstoffe ohne vorherige Extraktion

Dieser Teil der prEN 14362 legt ein Verfahren zum Verwendungsnachweis bestimmter Azofarbstoffe fest, die bei der Herstellung oder Behandlung bestimmter Waren aus Textilfasern nicht verwendet werden dürfen und die ohne vorherige Extraktion reduziert werden können, insbesondere Textilien aus Zellulose und Eiweißfasern (z. B. Baumwolle, Viscose, Wolle, Seide).
Hinsichtlich des Extraktionsprüfverfahrens wird auf prEN 14362-2 Verwendungsnachweis bestimmter Azofarb-stoffe durch Extraktion der Fasern verwiesen.
Bei bestimmten Fasermischungen kann es erforderlich sein, beide Teile dieser Norm anzuwenden.

Textiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoiques - Partie 1: Détection de l'utilisation de certains colorants azoiques accessibles sans extraction

La présente partie du prEN 14362 décrit un mode opératoire permettant de détecter l'utilisation de certains colorants azoiques qui ne peuvent etre utilisés dans la fabrication ou le traitement de certains articles en fibres textiles et qui sont accessibles aux agents de réduction sans extraction, en particulier les textiles fabriqués a partir de fibres de cellulose et de fibres protéiques (par exemple coton, viscose, laine, soie).
Pour la méthode d'essai d'extraction, voir le prEN 14362-2 « Détection de l'utilisation de certains colorants azoiques accessibles par extraction des fibres ».
Pour certains mélanges de matieres filables, il peut etre nécessaire d'appliquer les deux parties de la présente norme.

Tekstilije - Metode za določevanje nekaterih aromatskih aminov, izvirajočih iz azo barvil - 1. del: Zaznavanje prisotnosti določenih azo barvil, dostopnih brez ekstrahiranja vlaken

General Information

Status
Withdrawn
Publication Date
30-Nov-2003
Withdrawal Date
21-Mar-2012
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
22-Mar-2012
Due Date
14-Apr-2012
Completion Date
22-Mar-2012

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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 1: Verwendungsnachweis bestimmter Azofarbstoffe ohne vorherige ExtraktionTextiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoiques - Partie 1: Détection de l'utilisation de certains colorants azoiques accessibles sans extractionTextiles - Methods for the determination of certain aromatic amines derived from azo colorants - Part 1: Detection of the use of certain azo colorants accessible without extraction59.080.01Tekstilije na splošnoTextiles in generalICS:Ta slovenski standard je istoveten z:EN 14362-1:2003SIST EN 14362-1:2003en01-december-2003SIST EN 14362-1:2003SLOVENSKI

STANDARD
SIST EN 14362-1:2003

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14362-1October 2003ICS 59.080.30English versionTextiles - Methods for the determination of certain aromaticamines derived from azo colorants - Part 1: Detection of the useof certain azo colorants accessible without extractionTextiles - Méthodes de détermination de certaines aminesaromatiques dérivées de colorants azoïques - Partie 1:Détection de l'utilisation de certains colorants azoïquesaccessibles sans extractionTextilien - Verfahren für die Bestimmung bestimmteraromatischer Amine aus Azofarbstoffen - Teil 1:Verwendungsnachweis bestimmter Azofarbstoffe ohnevorherige ExtraktionThis 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 14362-1:2003 ESIST EN 14362-1:2003

EN 14362-1:2003 (E)2ContentsPageForeword.............................................................................................................................................................31Scope.....................................................................................................................................................42Normative references...........................................................................................................................43General...................................................................................................................................................44Principle.................................................................................................................................................55Safety precautions................................................................................................................................66Reagents................................................................................................................................................67Apparatus..............................................................................................................................................78Procedure..............................................................................................................................................79Evaluation..............................................................................................................................................910Test report.............................................................................................................................................9Annex A (informative)

Chromatographic analyses.......................................................................................10Annex B (normative)

Calculation....................................................................................................................15Annex C (informative)

Reliability of the method...........................................................................................16Annex D (informative)

Assessment guide - Interpretation of analytical results........................................17SIST EN 14362-1:2003

EN 14362-1:2003 (E)3ForewordThis document (EN 14362-1:2003) has been prepared by Technical Committee CEN/TC 248 “Textiles andtextile 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 identicaltext or by endorsement, at the latest by April 2004, and conflicting national standards shall be withdrawn at thelatest by April 2004.Annexes A, C and D are informative.

Annex B is normative.This European Standard calls for the use of substances and/or procedures that may be injurious tohealth if appropriate precautions are not observed. It refers only to technical suitability and does notabsolve the user 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 14362-1:2003

EN 14362-1:2003 (E)41 ScopeThis part of EN 14362 describes a procedure to detect the use of certain azo colorants that may not be usedin the manufacture or treatment of certain commodities made of textile fibres and that are accessible toreducing agent without extraction, particularly textiles made of cellulose and protein fibres (e.g. cotton,viscose, wool, silk).For the extraction test method see EN 14362-2 Detection of the use of certain azo colorants accessible byextracting the fibres.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.These normative references are cited at the appropriate places in the text and the publications are listedhereafter. For dated references subsequent amendments to, or revisions of, any of these publications apply tothis European Standard only when incorporated in it by amendment or revision. For undated references thelatest edition of the publication 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 followingaromatic amines, which are proscribed under Directive 2002/61/EC.Table 1 – Aromatic amines proscribed under Directive 2002/61/EC.No.CASnumberIndexnumberEC numberSubstances192-67-1612-072-00-6202-177-1biphenyl-4-ylamine4-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-toluidineSIST EN 14362-1:2003

EN 14362-1:2003 (E)57106-47-8612-137-00-9203-401-04-chloroaniline8615-05-4210-406-14-methoxy-m-phenylenediamine9101-77-9612-051-00-1202-974-44,4'-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 textile sample is treated with sodium dithionite in a citrate-buffered aqueous solution (pH = 6) at 70 °C ina closed vessel. The amines released in the process are transferred to a t-butyl methyl ether phase by meansof liquid-liquid extraction using diatomaceous earth columns. The t-butyl methyl ether extract is thenconcentrated and the residue is taken up in either methanol or another solvent appropriate for the detectionand determination of amines using chromatography.SIST EN 14362-1:2003

EN 14362-1:2003 (E)6If the amines are detected by one chromatographic method, then confirmation shall be made using one ormore alternative methods.5 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 appropriatenational health 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-use dust 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.6.2methanol6.3ethyl acetate6.4t-butyl methyl ether6.5citrate/sodium hydroxide buffer solution, pH = 6, c = 0,06 mol/l1) 6.6aqueous sodium dithionite solution,

= 200 mg/ml2), freshly (daily) prepared6.7diatomaceous earth

6.8amine 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 standard.6.9standard solutions6.9.1calibration solution of amines (see 6.7)

= 15,0 g of each amine per millilitre of an appropriatesolvent
1)c is citrate concentration2)
is mass concentrationSIST EN 14362-1:2003

EN 14362-1:2003 (E)76.9.2an appropriate mixture of internal standards in solution,

= 10,0 g of each IS/ml of theappropriate IS solventNOTEIS1: naphthalene-d8, CAS No.: 1146-65-2IS2: 2,4,5-trichloroaniline, CAS No.: 636-30-6IS3: 4-aminoquinaldine, CAS No.: 6628-04-2IS4: anthracene-d10, CAS No.: 1719-06-86.9.3solution of amine (see 6.8) for checking the experimental procedure,

= 30,0 g of each amine permillilitre methanol6.10grade 3 water, complying with EN ISO 3696.7 Apparatus7.1reaction vessel (20 ml to 50 ml) of heat-resistant glass, with tight closure7.2heating source that generates (70

2) C7.3glass or polypropylene column, inside diameter 25 to 30 mm, length 140 to 150 mm, packed with 20g of diatomaceous earth (6.7), fitted with glass fibre filter at the outlet. The diatomaceous earth columns areeither bought pre-packed and used as is, or 20 g of diatomaceous earth can be packed into a glass orpolypropylene column of the dimensions given.7.4vacuum rotary evaporator with water bath7.5pipettes 10 ml, 5 ml, 2 ml, 1 ml of class 1 complying with ISO 47877.6chromatographic equipment selected from the following:7.6.1thin layer chromatography (TLC) or high performance thin layer chromatography (HPTLC)equipment, including relevant detection7.6.2high performance liquid chromatography (HPLC) with gradient elution and diode array detector(DAD) or mass selective detector (MSD)7.6.3gas chromatography (GC) with flame ionisation detector (FID) or mass selective detec

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