EN 14362-3:2012
(Main)Textiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3: Detection of the use of certain azo colorants, which may release 4-aminoazobenzene
Textiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3: Detection of the use of certain azo colorants, which may release 4-aminoazobenzene
Azo colorants that are able to form 4-aminoazobenzene, generate under the conditions of EN 14362-1 the
amines aniline and 1,4-phenylenediamine. The presence of these 4-aminoazobenzene colorants cannot be
reliably ascertained without additional information (e.g. the chemical structure of the colorant used) or without
a special procedure.
This part of EN 14362 is supplementary to Part 1 and describes a special procedure to detect the use of
certain azo colorants in commodities, which may release 4-aminoazobenzene,
- accessible to reducing agent without extraction, particularly concerning textiles made of cellulose and
protein fibres (e.g. cotton, viscose, wool, silk);
- accessible by extracting the fibres (e.g. polyester or imitation leather).
For certain fibre blends both parts of this standard (without or with extraction) may need to be applied.
The procedure detects as well 4-aminoazobenzene (Solvent Yellow 1) which is already available as free
amine in commodities without reducing pre-treatment.
The use of certain azo colorants, which may release by reductive cleavage of their azo group(s) one or more
of the other aromatic amines listed in the Regulation (EC) No 1907/2006 of the European Parliament and of
the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) as regards
Annex XVII, except 4-aminoazobenzene, cannot be determined quantitatively with this method.
Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 3: Nachweis der Verwendung gewisser Azofarbstoffe, die 4-Aminoazobenzol freisetzen können
Azofarbstoffe, die 4 Aminoazobenzol bilden können, erzeugen unter den Bedingungen von EN 14362 1 die Amine Anilin und 1,4 Phenylendiamin. Die Anwesenheit dieser 4 Aminoazobenzol Farbstoffe kann ohne zusätzliche Angaben (z. B. die chemische Struktur des verwendeten Farbstoffs) oder ohne ein spezielles Verfahren nicht zuverlässig bestimmt werden.
Dieser Teil der EN 14362 ergänzt den Teil 1 und beschreibt ein spezielles Verfahren zum Verwendungs-nachweis bestimmter Azofarbstoffe in Bedarfsgegenständen, die 4 Aminoazobenzol freisetzen können,
- die ohne vorherige Extraktion reduziert werden können, insbesondere bei Textilien aus Zellulosefasern und Eiweißfasern (z. B. Baumwolle, Viskose, Wolle, Seide);
- die durch Extraktion der Fasern verfügbar sind (z. B. Polyester oder Kunstleder).
Bei bestimmten Fasermischungen kann es erforderlich sein, beide Teile dieser Norm (ohne oder mit Extraktion) anzuwenden.
Die Methode erfasst auch 4-Aminoazobenzol (Solvent Yellow 1), welches bereits ohne reduktive Vorbehandlung im Erzeugnis als freies Amin vorliegen kann.
Mit Ausnahme von 4 Aminoazobenzol kann die Verwendung bestimmter Azofarbstoffe, die durch reduktive Spaltung ihrer Azogruppe(n) ein oder mehrere weitere aromatische Amine freisetzen und in Anhang XVII der Verordnung (EG) Nr. 1907/2006 des Europäischen Parlaments und des Rates vom 18. Dezember 2006 zur Registrierung, Bewertung, Zulassung und Beschränkung chemischer Stoffe (REACH) aufgeführt sind, mit dem vorliegenden Verfahren quantitativ nicht bestimmt werden.
Textiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoïques - Partie 3: Détection de l’utilisation de certains colorants azoïques susceptibles de libérer du 4-aminoazobenzène
Les colorants azoïques capables de former du 4-aminoazobenzène génèrent, dans les conditions de l’EN 14362-1, des amines dont l’aniline et la 1,4-phénylènediamine. La présence de ces colorants à base de 4-aminoazobenzène ne peut être déterminée de façon fiable sans information supplémentaire (par exemple sur la structure chimique du colorant utilisé) ou sans mode opératoire spécifique.
La présente partie de l’EN 14362 est un supplément à la Partie 1 et décrit un mode opératoire spécifique permettant de détecter l'utilisation de certains colorants azoïques dans des articles pouvant libérer du 4-aminoazobenzène,
- accessibles aux agents de réduction sans extraction, en particulier dans le cas des textiles fabriqués à partir de fibres de cellulose et de fibres animales (par exemple, le coton, la viscose, la laine, la soie) ;
- accessibles par extraction des fibres (par exemple le polyester ou le simili cuir).
Pour certains mélanges de fibres, il peut être nécessaire d’appliquer les deux parties de la présente norme (avec et sans extraction).
Ce mode opératoire détecte également le 4-aminoazobenzène utilisé en tant que colorant (Solvent Yellow 1) qui est déjà disponible dans des articles sous la forme de l’amine libre, sans dégradation par traitement de réduction.
L’utilisation de certains colorants azoïques, qui peuvent libérer par clivage réducteur de leur(s) groupe(s) azoïque(s) une ou plusieurs des autres amines aromatiques répertoriées dans le Règlement CE n° 1907/2006 du Parlement européen et du Conseil concernant l'enregistrement, l'évaluation et l'autorisation des substances chimiques, ainsi que les restrictions applicables à ces substances (REACH) conformément à l’Annexe XVII, exception faite du 4-aminoazobenzène, ne peut pas être déterminée quantitativement avec cette méthode.
Tekstilije - Metode za določevanje nekaterih aromatskih aminov, izvirajočih iz azo barvil - 3. del: Zaznavanje prisotnosti določenih azo barvil, ki lahko sproščajo 4-aminoazobenzen
Iz azo barvil, ki lahko tvorijo 4-aminoazobenzen, pod pogoji iz standarda prEN 14362-1 nastaneta amina anilin in 1,4-fenilenediamin. Prisotnosti teh barvil iz 4-aminoazobenzena ni mogoče zanesljivo ugotoviti brez dodatnih informacij (npr. kemijske strukture uporabljenega barvila) ali posebnega postopka. Ta del standarda EN 14362 dopolnjuje 1. del in opisuje poseben postopek za zaznavanje prisotnosti določenih azo barvil, ki lahko sproščajo 4-aminoazobenzen in so reducentom dostopna brez ekstrahiranja, pri izdelkih, zlasti tekstilijah iz celuloznih in proteinskih vlaken (npr. bombaž, viskoza, volna, svila) ter takih, ki so dostopna z ekstrakcijo vlaken (npr. poliester ali umetno usnje). Za nekatere mešanice vlaken (z ekstrakcijo ali brez) bo morda treba uporabiti oba dela tega standarda. Postopek omogoča tudi zaznavanje 4-aminoazobenzena (Solvent Yellow 1 – topilo rumena 1), ki je v izdelkih že razpoložljiv kot prosti amin brez predhodne obdelave z redukcijo. Kvantitativno določevanje uporabe določenih azo barvil, ki lahko z redukcijsko cepitvijo njihovih azo skupin sproščajo enega ali več drugih aromatskih aminov iz Priloge XVII k Uredbi (ES) št. 1907/2006 Evropskega parlamenta in Sveta o registraciji, evalvaciji, avtorizaciji in omejevanju kemikalij (REACH), razen 4-aminoazobenzena, s to metodo ni mogoče.
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.DPLQRD]REHQ]HQTextilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 3: Nachweis der Verwendung gewisser Azofarbstoffe die 4-Aminoazobenzol freisetzen könnenTextiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoïques - Partie 3: Détection de l’utilisation de certains colorants azoïques susceptibles de libérer du 4-aminoazobenzèneTextiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3: Detection of the use of certain azo colorants which may release 4-aminoazobenzene59.080.01Tekstilije na splošnoTextiles in generalICS:Ta slovenski standard je istoveten z:EN 14362-3:2012SIST EN 14362-3:2012en,fr,de01-september-2012SIST EN 14362-3:2012SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14362-3
June 2012 ICS 59.080.01 English Version
Textiles - Methods for determination of certain aromatic amines derived from azo colorants - Part 3: Detection of the use of certain azo colorants, which may release 4-aminoazobenzene
Textiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoïques - Partie 3: Détection de l'utilisation de certains colorants azoïques susceptibles de libérer du 4-aminoazobenzène
Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 3: Nachweis der Verwendung gewisser Azofarbstoffe, die 4-Aminoazobenzol freisetzen können This European Standard was approved by CEN on 24 May 2012.
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 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, 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 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, France, 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
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 14362-3:2012: ESIST EN 14362-3:2012
Chromatographic analyses . 11Annex B (normative)
Calculation . 16Annex C (informative)
Reliability of the method . 18Annex D (informative)
Assessment guide - Interpretation of analytical results . 20 SIST EN 14362-3:2012
accessible to reducing agent without extraction, particularly concerning textiles made of cellulose and protein fibres (e.g. cotton, viscose, wool, silk); accessible by extracting the fibres (e.g. polyester or imitation leather). For certain fibre blends both parts of this standard (without or with extraction) may need to be applied.
The procedure detects as well 4-aminoazobenzene (Solvent Yellow 1) which is already available as free amine in commodities without reducing pre-treatment. The use of certain azo colorants, which may release by reductive cleavage of their azo group(s) one or more of the other aromatic amines listed in the Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) as regards Annex XVII, except 4-aminoazobenzene, cannot be determined quantitatively with this method. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 14362-1:2012, Textiles — Methods for determination of certain aromatic amines derived from azo colorants — Part 1: Detection of the use of certain azo colorants accessible with and without extracting the fibres EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) 3 General Certain azo colorants may release, by reductive cleavage of azo group(s), 4-aminoazobenzene, which is proscribed under Regulation (EC) No 1907/2006 of the European Parliament and of the Council on the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH) as regards Annex XVII. Table 1 — 4-aminoazobenzene proscribed under Regulation REACH 1907/2006/Annex XVII No. CAS number Index number EC number Substance 22 60-09-3 611-008-00-4 200-453-6 4-aminoazobenzene
5 Safety precautions 5.1
WARNING — 4-aminoazobenzene is classified as a substance known to be or suspected to be human carcinogen.
Any handling and disposal of these substances shall be in strict accordance with the appropriate national health and safety regulations. 5.2 It 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. 5.3 Good laboratory practice should be followed. Wear safety glasses in all laboratory areas and a single-use dust respirator while handling powder colorants. 5.4 Users should comply with any national and local safety regulations. 6 Reagents Unless otherwise specified, analytical grade chemicals shall be used.
6.1
aqueous sodium dithionite solution, ρ = 200 mg/ml1), freshly prepared, to use immediately after resting for one hour in a closed vessel 6.2 sodium hydroxide aqueous solution, ω = 2 %2) 6.3 n-pentane 6.4 methanol
6.5 chlorobenzene 6.6 t-butyl methyl ether 6.7 sodium chloride
1) ρ = mass concentration 2) ω = mass portion (% by weight) SIST EN 14362-3:2012
Figure 1 — Apparatus NOTE Similar apparatus can be used, if the same results are obtained. 7.3 heating source that generates a temperature of (40 ± 2) °C SIST EN 14362-3:2012
7.7 ultrasonic bath, at least ultrasonic power RMS 160 Watt, with controllable heating 7.8 horizontal shaker with sufficient frequency of 5 s-1, path length 2 cm to 5 cm 7.9 instrumental equipment 7.9.1 gas chromatography (GC) with mass selective detector (MS) 7.9.2 high performance liquid chromatography (HPLC) with gradient elution and diode array detector (DAD) or mass selective detector (MS) 7.9.3 thin layer chromatography (TLC) or high performance thin layer chromatography (HPTLC) equipment, including relevant detection
7.9.4 capillary electrophoresis (CE) with DAD NOTE A description of the equipment is given in Annex A. 8 Procedure 8.1 General Apply this standard to the test specimen that gave a positive result for aniline and 1,4-phenylenediamine or only aniline using EN 14362-1. Choose 8.3 or 8.4 depending of the sample composition. 8.2 Preparation of test specimens In the case of fabrics with multicoloured patterns, the various colours have to be taken into account separately as far as possible. For commodities consisting of various textile qualities, specimens of the various qualities (in terms of fibre and/or colour) shall be analyzed separately. Prepare the test specimen by cutting in order to obtain a total mass of 1 g. For specimens to be submitted to colorant extraction (8.3) cut into strips (if apparatus described in 7.2 is used) or cut into small pieces if other apparatus is used or for specimens to be submitted only to reductive cleavage (8.4). 8.3 Colorant extraction for disperse dyes 8.3.1 Extraction if disperse dyes with chlorobenzene The textile specimen dyed with disperse dyes (see Annex D from EN 14362-1:2012) is kept in the extractor (7.2) for 30 min above 25 ml boiling chlorobenzene. The chlorobenzene extract is allowed to cool down to room temperature before detaching it from the extractor. Concentrate the chlorobenzene extract in the evaporation apparatus (7.5) at a temperature of 45 °C to 60 °C to a small residual quantity. This residue is quantitatively transferred to the reaction vessel with 7 ml methanol (6.4) in total, using an ultrasonic bath to disperse the colorant.
NOTE 1 It is recommended to carry out the transfer in multiple steps; e. g. to add 4 ml of methanol and to dissolve the residue from the glass flask using an ultrasonic bath, then to transfer the suspension quantitatively into the reaction vessel using a pipette, subsequently to rinse three times with 1 ml of methanol and to transfer the solution quantitatively. SIST EN 14362-3:2012
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