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

This European Standard 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 with and without extraction.
Azo colorants accessible to reducing agent without extraction are those used to dye:
   cellulosic fibres (e.g. cotton, viscose);
   protein fibres (e.g. wool, silk);
   synthetic fibres (e.g. polyamide, acrylic).
Azo colorants accessible with extraction are those used to dye man-made fibres with disperse dyes. The following man-made fibres can be dyed with disperse dyes: polyester, polyamide, acetate, triacetate, acrylic and chlorofibre.
For certain commodities made of cellulose and/or protein fibres blended with man-made fibres it is necessary to extract the dye first.
The method is relevant for all coloured textiles, e.g. dyed, printed and coated textiles.

Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 1: Nachweis der Verwendung bestimmter Azofarbstoffe mit und ohne Extraktion der Faser

Dieser Teil der EN 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 mit und ohne vorheriger Extraktion reduziert werden können.
Azofarbstoffe, die ohne vorherige Extraktion reduziert werden können, sind diejenigen, die verwendet werden zum Färben von:
   Zellulosefasern (z. B. Baumwolle, Viskose);
   Eiweißfaserstoffen (z. B. Wolle, Seide);
   Synthesefasern (z. B. Polyamid, Acryl).
Azofarbstoffe, die mit vorheriger Extraktion verfügbar sind, sind diejenigen, die zum Färben von Chemiefasern mit Dispersionsfarbstoffen verwendet werden. Die folgenden Kunstfasern können mit Dispersionsfarbstoffen gefärbt werden: Polyester, Polyamid, Acetat, Triacetat, Acryl und Chlorfaser.
Bei bestimmten Waren, die aus Zellulose und/oder Eiweißfasern bestehen und mit Kunstfasern gemischt sind, ist es erforderlich, zuerst den Farbstoff zu extrahieren.
ANMERKUNG   Das Verfahren gilt für alle farbigen Textilien, z. B. gefärbte, bedruckte und beschichtete Textilien.

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

La présente partie de l’EN 14362 décrit un mode opératoire permettant de détecter l’utilisation de certains colorants azoïques qui ne peuvent pas être utilisés dans la fabrication ou le traitement de certains articles en fibres textiles et qui sont accessibles aux agents de réduction avec ou sans extraction.
Les colorants azoïques accessibles aux agents de réduction sans extraction sont ceux utilisés pour teindre :
   des fibres cellulosiques (par exemple, le coton, la viscose) ;
   des fibres protéiques (par exemple, la laine, la soie) ;
   des fibres synthétiques (par exemple, les polyamides, l’acrylique).
Les colorants azoïques accessibles avec extraction sont ceux utilisés pour teindre les fibres chimiques au moyen de colorants dispersés. Les fibres chimiques suivantes peuvent être teintes au moyen de colorants dispersés : polyester, polyamide, acétate, triacétate, acrylique et chlorofibre.
Il est nécessaire d’extraire en premier lieu le colorant pour certains articles constitués de fibres cellulosiques et/ou de fibres protéiques mélangées à des fibres chimiques.
NOTE   La méthode est adaptée à tous les textiles colorés, par exemple les textiles teints, imprimés et enduits.

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

Ta del standarda EN 14362 opisuje postopek za zaznavanje prisotnosti določenih azo barvil, ki se uporabljajo pri proizvodnji in obdelavi nekaterih izdelkov iz tekstilnih vlaken ter so reducentom dostopna z ekstrahiranjerm ali brez njega.
Azo barvila, reducentom dostopna brez ekstrahiranja, so tista barvila, ki se uporabljajo za barvanje:
 celuloznih vlaken (npr. bombaž, viskoza);
 proteinskih vlaken (npr. volna, svila);
 sintetičnih vlaken (npr. poliestrska, poliakrilonitrilna vlakna);
Azo barvila, reducentom dostopna z ekstrahiranjerm, so tista barvila, ki se uporabljajo za barvanje kemičnih vlaken z disperznimi barvili. Kemična vlakna, ki se lahko barvajo z disperznimi barvili so naslednja: poliestrska, poliamidna, acetatna, triacetatna in poliakrilonitrilna vlakna ter klorovlakna.
Pri nekaterih izdelkih iz mešanice celuloznih in/ali proteinskih vlaken ter kemičnih vlaken je najprej potrebna ekstrakcija barvila.
OPOMBA: Metoda je primerna za vse vrste barvanega tekstila, npr. barvan, tiskan in prevlečen tekstil.

General Information

Status
Withdrawn
Publication Date
07-Feb-2012
Withdrawal Date
07-Feb-2017
Current Stage
9960 - Withdrawal effective - Withdrawal
Completion Date
08-Feb-2017

RELATIONS

Buy Standard

Standard
EN 14362-1:2012
English language
29 pages
sale 10% off
Preview
sale 10% off
Preview

e-Library read for
1 day

Standards Content (sample)

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: Nachweis der Verwendung gewisser Azofarbstoffen bestimmbar durch reduzierende Substanzen, mit oder ohne

ExtraktionTextiles - Méthodes de détermination de certaines amines aromatiques dérivées de colorants azoïques - Partie 1: Détection de l'utilisation de certains colorants azoïques accessibles avec ou sans extractionTextiles - 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 fibres59.080.01Tekstilije na splošnoTextiles in generalICS:Ta slovenski standard je istoveten z:EN 14362-1:2012SIST EN 14362-1:2012en,fr,de01-maj-2012SIST EN 14362-1:2012SLOVENSKI

STANDARDSIST EN 14362-2:2003SIST EN 14362-2:2003/AC:2005SIST EN 14362-1:2003SIST EN 14362-1:2003/AC:20051DGRPHãþD

SIST EN 14362-1:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14362-1

February 2012 ICS 59.080.01 Supersedes EN 14362-1:2003, EN 14362-2:2003English Version

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

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

Textilien - Verfahren für die Bestimmung bestimmter aromatischer Amine aus Azofarbstoffen - Teil 1: Nachweis der Verwendung bestimmter Azofarbstoffe mit oder ohne Extraktion This European Standard was approved by CEN on 22 December 2011.

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 14362-1:2012: ESIST EN 14362-1:2012

EN 14362-1:2012 (E) 2 Contents Page Foreword ..............................................................................................................................................................41Scope ......................................................................................................................................................52Normative references ............................................................................................................................53General ....................................................................................................................................................54Principle ..................................................................................................................................................75Safety precautions .................................................................................................................................76Reagents .................................................................................................................................................77Apparatus ...............................................................................................................................................88Test specimen sampling and preparation ........................................................................................ 108.1General ................................................................................................................................................. 108.2Textile article ....................................................................................................................................... 108.3Fibre composition ............................................................................................................................... 108.4Case of the fibre blends ..................................................................................................................... 118.5Printed materials ................................................................................................................................. 118.6Colours ................................................................................................................................................ 118.6.1General ................................................................................................................................................. 118.6.2Case of colour gathering ................................................................................................................... 118.6.3Preparation of the three colour test specimen ................................................................................ 129Procedure ............................................................................................................................................ 129.1Colorant extraction for disperse dyes .............................................................................................. 129.1.1Extraction of disperse dyes with chlorobenzene ............................................................................ 129.1.2Textiles only dyed with disperse dyes ............................................................................................. 129.1.3Textiles dyed with disperse dyes and/or other dyes ...................................................................... 129.2Textiles dyed with dyes other than disperse dyes .......................................................................... 129.3Reductive cleavage ............................................................................................................................ 129.4Separation and concentration of the amines ................................................................................... 139.5Amine detection and quantification .................................................................................................. 139.6Check procedure................................................................................................................................. 139.6.1General ................................................................................................................................................. 139.6.2Calibration using internal standard (quantification performed by gas chromatography) .......... 139.6.3Calibration without internal standard ............................................................................................... 1410Evaluation ............................................................................................................................................ 1410.1General ................................................................................................................................................. 1410.2Calculation of amine in the sample................................................................................................... 1510.3Reliability of the method .................................................................................................................... 1511Test report ........................................................................................................................................... 15Annex A (informative)

Chromatographic analyses ..................................................................................... 16A.1Preliminary remark ............................................................................................................................. 16A.2Thin layer chromatography (TLC) ..................................................................................................... 16A.3High performance liquid chromatography (HPLC) .......................................................................... 17A.4Capillary gas chromatography/mass selective detector (GC/MS) ................................................. 18A.5Capillary electrophoresis (CE) .......................................................................................................... 18Annex B (informative)

Reliability of the method ......................................................................................... 20Annex C (informative)

Assessment guide-interpretation of analytical results ........................................ 22Annex D (informative)

Explanatory table of dyestuffs used in various textile materials ........................ 23SIST EN 14362-1:2012

EN 14362-1:2012 (E) 3 D.1General ................................................................................................................................................. 23D.2Criteria for printed materials .............................................................................................................. 24Annex E (informative)

Procedure for liquid/liquid-extraction without diatomaceous earth .................... 25E.1Preliminary remark .............................................................................................................................. 25E.2Additional reagents used.................................................................................................................... 25E.3Additional apparatus used ................................................................................................................. 26E.4Procedure ............................................................................................................................................. 26Annex F (normative)

Colorants - Methods for determination of certain aromatic amines ...................... 28F.1Scope .................................................................................................................................................... 28F.2Principle................................................................................................................................................ 28F.3Test specimen preparation ................................................................................................................. 28F.4Procedure ............................................................................................................................................. 28F.5Evaluation............................................................................................................................................. 28F.6Test report ............................................................................................................................................ 28Bibliography ...................................................................................................................................................... 29 SIST EN 14362-1:2012

EN 14362-1:2012 (E) 4 Foreword This document (EN 14362-1:2012) has been prepared by Technical Committee CEN/TC 248 “Textiles and textile 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 August 2012, and conflicting national standards shall be withdrawn at the latest by August 2012. 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. This document supersedes EN 14362-1:2003, EN 14362-2:2003. EN 14362 is composed of the following parts:  EN 14362-1, 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 14362-3, 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. The following is a list of technical changes since the last edition:  Part 2 of EN 14362 has been integrated into Part 1. This is mainly reflected in:  changes to Clause 4 "Principle";  insertion of a new Clause 8 "Test specimen sampling and preparation";  insertion of a new Subclause 9.1 "Colorant extraction for disperse dyes";  insertion of a new Subclause 9.2 "Textiles dyed with dyes other than disperse dyes";  addition of Annex D (informative) "Explanatory table of dyestuffs used in various textile materials".  Addition of Annex F (normative) "Colorants - Methods for determination of certain aromatic amines";  The calculation, previously Annex B (normative) has been moved to Subclause 9.6. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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 the United Kingdom. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 5 1 Scope This European Standard 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 with and without extraction. Azo colorants accessible to reducing agent without extraction are those used to dye:  cellulosic fibres (e.g. cotton, viscose);  protein fibres (e.g. wool, silk);  synthetic fibres (e.g. polyamide, acrylic). Azo colorants accessible with extraction are those used to dye man-made fibres with disperse dyes. The following man-made fibres can be dyed with disperse dyes: polyester, polyamide, acetate, triacetate, acrylic and chlorofibre. For certain commodities made of cellulose and/or protein fibres blended with man-made fibres it is necessary to extract the dye first. The method is relevant for all coloured textiles, e.g. dyed, printed and coated textiles. 2 Normative references The following referenced documents are indispensable for the application of this European Standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696:1995, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) 3 General Certain azo colorants may release, by reductive cleavage of azo group(s), one or more of the following aromatic amines, which are proscribed under Regulation (EC) No 1907/2006 of the European Parliament and of the Council of 18 December 2006 concerning the Registration, Evaluation, Authorisation and Restriction of Chemicals (REACH), establishing a European Chemicals Agency. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 6 Table 1 — Aromatic amines proscribed under Regulation REACH 1907/2006/Annex XVII No. CAS number Index number EC number Substances 1 92-67-1 612-072-00-6 202-177-1 biphenyl-4-ylamine

4-aminobiphenyl xenylamine 2 92-87-5 612-042-00-2 202-199-1 benzidine 3 95-69-2 612-196-00-0 202-441-6 4-chloro-o-toluidine 4 91-59-8 612-022-00-3 202-080-4 2-naphthylamine 5a 97-56-3 611-006-00-3 202-591-2 o-aminoazotoluene 4-amino-2',3-dimethylazobenzene 4-o-tolylazo-o-toluidine 6a 99-55-8 612-210-00-5 202-765-8 5-nitro-o-toluidine 2-amino-4-nitrotoluene 7 106-47-8 612-137-00-9 203-401-0 4-chloroaniline 8 615-05-4 612-200-00-0 210-406-1 4-methoxy-m-phenylenediamine 2,4-diaminoanisole 9 101-77-9 612-051-00-1 202-974-4 4,4'-methylenedianiline 4,4'-diaminodiphenylmethane 10 91-94-1 612-068-00-4 202-109-0 3,3'-dichlorobenzidine 3,3'-dichlorobiphenyl-4,4'-ylenediamine 11 119-90-4 612-036-00-X 204-355-4 3,3'-dimethoxybenzidine o-dianisidine 12 119-93-7 612-041-00-7 204-358-0 3,3'-dimethylbenzidine 4,4'-bi-o-toluidine 13 838-88-0 612-085-00-7 212-658-8 4,4'-methylenedi-o-toluidine 14 120-71-8 612-209-00-X 204-419-1 6-methoxy-m-toluidine p-cresidine 15 101-14-4 612-078-00-9 202-918-9 4,4'-methylene-bis-(2-chloro-aniline) 2,2'-dichloro-4.4’-methylene-dianiline 16 101-80-4 612-199-00-7 202-977-0 4,4'-oxydianiline 17 139-65-1 612-198-00-1 205-370-9 4,4'-thiodianiline 18 95-53-4 612-091-00-X 202-429-0 o-toluidine 2-aminotoluene 19 95-80-7 612-099-00-3 202-453-1 4-methyl-m-phenylenediamine 2,4-toluylendiamine 2,4-diaminotoluene 20 137-17-7 612-197-00-6 205-282-0 2,4,5-trimethylaniline 21 90-04-0 612-035-00-4 201-963-1 o-anisidine 2-methoxyaniline 22b 60-09-3 611-008-00-4 200-453-6 4-aminoazobenzene a 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). b Azo colorants that are able to form 4-aminoazobenzene, generate under the condition of this method aniline (CAS-number 62-53-3) and 1,4-phenylenediamine (CAS – number 106-50-3). Due to detection limits, only aniline may be detected. The presence of these colorants should be tested by EN 14362-3. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 7 4 Principle After selection of a coloured test specimen from the textile article, the test specimen is tested according to the method of colorant extraction for disperse dyes and/or the method of direct reduction for the other classes of dyes. The application of the combined methods or one of the two methods is based on the nature of the fibre(s) of the test specimen (composed of pure fibre or of fibre blends) and the colour treatment (dyeing or printing process). When relevant, if the test specimen is not discoloured during the application of one of the two methods, the other one is carried out. When the method of the colorant extraction for disperse dyes is carried out, the colorant is first extracted from the fibre in the headspace (see Figure 1) using chlorobenzene under reflux. The extract is concentrated and transferred to the reaction vessel with methanol for subsequent reduction with sodium dithionite in a citrate-buffered aqueous solution (pH = 6) at 70 °C. If the textile specimen is not completely discoloured after chlorobenzene extraction, the specimen is added to the reaction vessel with the methanolic solution of the dispersed dye for combined reduction. When the method for the other classes of the dyes is carried out, the test specimen is treated with sodium dithionite in a citrate-buffered aqueous solution (pH = 6) at 70 °C in a closed vessel. After the reduction, any amine released in the process is transferred to a t-butyl methyl ether phase by means of liquid-liquid extraction using diatomaceous earth columns. The t-butyl methyl ether extract is then concentrated, and the residue is taken up in a solvent appropriate for detection and determination of the amines using chromatography (see Annex A). A screening method, using liquid/liquid extraction without diatomaceous earth columns, is described in Annex E. If any amine is detected by one chromatographic method, then confirmation shall be made using one or more alternative methods. 5 Safety precautions 5.1 WARNING — The substances [amines] listed in Clause 3 are classified as substances known to be or suspected of being human carcinogens. 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 Chlorobenzene. 6.2 Acetonitrile. 6.3 Methanol. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 8 6.4 t-butyl methyl ether. 6.5 n-pentane. 6.6 Citrate/sodium hydroxide buffer solution, pH = 6, c = 0,06 mol/l1). 6.7 Aqueous sodium dithionite solution, ρ = 200 mg/ml2) freshly (daily) prepared. 6.8 Diatomaceous earth. 6.9 Amine 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. 6.10 Standard solutions. 6.10.1 Stock solution of amines with a concentration of equal to or greater than 300 µg of each amine per millilitre of an appropriate solvent.

NOTE Acetonitrile is an appropriate solvent for this stock solution, resulting in good stability of amines. 6.10.2 Calibration solution of amines for daily use.

Dilute from the stock solution 6.10.1 to a concentration of ρ = 15,0 µg of each amine per millilitre of an appropriate solvent. 6.10.3 Calibration solutions of amines for quantification, concentration range from 2 µg up to 50 µg of each amine per millilitre of an appropriate solvent. NOTE It is the responsibility of each lab to choose appropriate concentrations for the calibration. 6.10.4 Internal standards in solution (IS), ρ = 1,0 mg of IS/ml of the appropriate IS solvent.

In case of GC-MS analysis, use one of the following internal standards:  IS1: benzidine-d8, CAS No.: 92890-63-6;  IS2: naphthalene-d8, CAS No.: 1146-65-2;  IS3: 2,4,5-trichloroaniline, CAS No.: 636-30-6;  IS4: anthracene-d10, CAS No.: 1719-06-8. NOTE If the confirmation analysis for benzidine is done with DAD or TLC the use of IS1: benzidine-d8, CAS No.: 92890-63-6 is not feasible, because the peak cannot be separated from the none deuterated benzidine. 6.11 Sodium hydroxide aqueous solution, a mass fraction of 10 %. 6.12 Grade 3 water, complying with EN ISO 3696:1995. 7 Apparatus 7.1 Extraction apparatus, according to Figure 1, consisting of:

1) c is citrate concentration. 2) ρ is the mass concentration. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 9  coil condenser NS 29/32;  a hook, made from an inert material to hold the specimen in place so that the condensed solvent drips onto it;  100 ml round bottom flask NS 29/32;  heating source.

Figure 1 — Apparatus NOTE Similar apparatus may be used, if the same results are obtained. 7.2 Ultrasonic bath, controllable heating. 7.3 Reaction vessel (20 ml to 50 ml) of heat-resistant glass, with tight closure. 7.4 Heating source that generates (70 ± 2) °C. 7.5 Glass or polypropylene column, inside diameter 25 mm to 30 mm, length 130 mm to 150 mm, packed with 20 g of diatomaceous earth (6.8), fitted with glass fibre filter at the outlet.

The diatomaceous earth columns are either bought pre-packed and used as is, or 20 g of diatomaceous earth can be packed into a glass or polypropylene column of the dimensions given. 7.6 Vacuum rotary evaporator with vacuum control and water bath. NOTE Other kinds of evaporation apparatus may be used, e.g. a water bath with a controlled flow of nitrogen over the liquid. 7.7 Pipettes in required sizes or variables pipettes. 7.8 Chromatographic equipment selected from the following: 7.8.1 Thin layer chromatography (TLC) or high performance thin layer chromatography (HPTLC) equipment, including relevant detection. 7.8.2 High performance liquid chromatography (HPLC) with gradient elution and diode array detector (DAD) or mass selective detector (MS). 7.8.3 Gas chromatography (GC) with flame ionisation detector (FID) or mass selective detector (MS). 7.8.4 Capillary electrophoresis (CE) with diode array detector (DAD). NOTE A description of the chromatographic equipment is given in Annex A. SIST EN 14362-1:2012

EN 14362-1:2012 (E) 10 8 Test specimen sampling and preparation 8.1 General The test specimen shall be selected based on the following criteria:  Parts of the textile article;  Nature of the fibre components (fibre composition);  Printed materials;  Colours. Prepare the test specimen by cutting in order to obtain a total mass of 1 g. For specimens to be submitted to colorant extraction (9.1) cut into strips (if apparatus described in 7.1 is used) or cut into small pieces if other apparatus is used or for specimens to be submitted only to reductive cleavage (9.3). 8.2 Textile article If the textile article is a semi-manufactured product, such as yarns, fabrics, etc., cut out test specimens from it. If the textile article is composed of several parts of textile products, such as a garment, cut out test specimens from all the parts of the textile article that have direct and prolonged contact to skin or mouth, which can be:  principal fabric(s);  lining(s);  pocket fabric(s);  embroideries;  label(s) for textile article;  drawstring(s);  fastener(s);  false fur;  sewing threads. If the mass of some parts (e.g. labels, sewing threads, embroideries of small size) does not reach the mass (1 g) to be tested, gather identical parts when possible. If the total mass of material is below 0,5 g, this material is defined as a minor component. (See NOTE 2, Annex C.) Below 0,2 g of material the analysis is omitted. Embroideries shall be weighed with the ground fabric. 8.3 Fibre composition As the application of this standard is partly based on the extraction of colorants, identify the nature of the textile components so that the possible use of disperse dyestuffs can be determined. Table 2 summarizes the four cases: SIST EN 14362-1:2012

EN 14362-1:2012 (E) 11 Table 2 — Application of colorant extraction for disperse dyes (9.1) in relation to the fibre nature Nature of fibre Use of disperse dyestuffs Cases Colorant extraction for disperse dyes (9.1) necessary? Natural fibre No A No Man-made fibre No B No Undetermined C Yes Yes D Yes NOTE If a fibre is not dyed, the fibre shall not be tested.

Categories of dyestuffs used in either natural or man-made fibres are explained in Annex D. 8.4 Case of the fibre blends In the case when fibres of different types are mixed, refer to Table 3 in order to decide if application of the colorant extraction for disperse dyes (9.1) shall be applied. Table 3 — Application of colorant extraction for disperse dyes (9.1) in relation to the fibre blends Colorant extraction for disperse dyes (9.1) necessary? Other component of the blend A B C D Component of the blend A No No Yes Yes B No No Yes Yes C Yes Yes Yes Yes D Yes Yes Yes Yes NOTE

See Table 2 for meanings of A, B, C and D.

8.5 Printed materials If material is printed with pigments (Annex D) the method in 9.2 has to be used. 8.6 Colours 8.6.1 General All colours shall be tested. NOTE "White" is not considered as "colour" and therefore "white" parts do not have to be tested. 8.6.2 Case of colour gathering Up to three colours may be tested together. In order to gather three colours, the following rules shall be applied. The rules have been listed in order of preference:  Select the three colours from the same part of the textile article; SIST EN 14362-1:2012

EN 14362-1:2012 (E) 12  If the three colours do not come from the same part of the textile article, select these three colours from textile parts made of the same type of textile fibre;  If the three colours do not come from the same part of the textile article and do not come from the same type of textile fibre, select these three colours from textile parts on which the same procedure shall be applied. 8.6.3 Preparation of the three colour test specimen Each colour shall have approximately the same weight in order to obtain the total mass of 1 g. If the result of the combined test specimen is in the range between 5 mg/kg and 30 mg/kg of any of the named amines, separate testing is necessary as the result of testing a single colour test specimen may exceed 30 mg/kg. The quantification limits shall be documented for every amine by internal validation procedures. 9 Procedure 9.1 Colorant extraction for disperse dyes 9.1.1 Extraction of disperse dyes with chlorobenzene The textile specimen dyed with disperse dyes is kept in the extractor according to (7.1) 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 at a temperature of 45 °C to 60 °C to a small residual quantity. This residue is quantitatively transferred to the reaction vessel with two portions of 1 ml methanol using an ultrasonic bath to disperse the colorant. 9.1.2 Textiles only dyed with disperse dyes Remove the textile specimen from the extractor and discard it if it is completely made of fibres dyed with disperse dyes and/or becomes decolourised after extraction. 9.1.3 Textiles dyed with disperse dyes and/or other dyes Remove, from the extractor, the extracted textile specimen if it contains fibres

...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.