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 (ISO 14362-1:2017)

ISO 14362-1:2017 describes a method 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 colour with pigments or to dye
- cellulosic fibres (e.g. cotton, viscose),
- protein fibres (e.g. wool, silk), and
- 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.
The method is relevant for all coloured textiles, e.g. dyed, printed and coated textiles.

Textilien - Verfahren für die Bestimmung gewisser aromatischer Amine aus Azofarbstoffen - Teil 1: Nachweis der Verwendung gewisser Azofarbstoffe mit und ohne Extraktion der Fasern (ISO 14362-1:2017)

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 (ISO 14362-1:2017)

ISO 14362-1:2017 spécifie une méthode 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 accessibles aux agents réducteurs avec ou sans extraction.
Les colorants azoïques accessibles aux agents réducteurs sans extraction sont ceux utilisés pour colorer avec des pigments ou pour teindre:
- des fibres cellulosiques (par exemple le coton, la viscose);
- des fibres animales (par exemple la laine, la soie); et
- des fibres synthétiques (par exemple le polyamide, 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.
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 (ISO 24362-1:2017)

Ta del standarda ISO 24362 opisuje postopek za zaznavanje prisotnosti določenih azo barvil,
ki jih ni dovoljeno uporabljati pri proizvodnji ali obdelavi nekaterih izdelkov iz tekstilnih vlaken in ki so
dostopna reducentom z ekstrahiranjem 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. poliamidna, akrilna 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, akrilna, modakrilna in aramidna vlakna ter klorovlakna.
Pri nekaterih izdelkih iz mešanice celuloznih in/ali proteinskih vlaken ter kemičnih vlaken je najprej potrebna ekstrakcija barvila.
Metoda je primerna za vse vrste barvanega tekstila, npr. barvan, tiskan in prevlečen tekstil.

General Information

Status
Published
Publication Date
07-Feb-2017
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
08-Feb-2017
Completion Date
08-Feb-2017

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SLOVENSKI STANDARD
SIST EN ISO 14362-1:2017
01-april-2017
1DGRPHãþD
SIST EN 14362-1:2012

7HNVWLOLMH0HWRGH]DGRORþHYDQMHQHNDWHULKDURPDWVNLKDPLQRYL]YLUDMRþLKL]D]R

EDUYLOGHO=D]QDYDQMHSULVRWQRVWLGRORþHQLKD]REDUYLOGRVWRSQLK]
HNVWUDKLUDQMHPYODNHQLQEUH]QMHJD ,62
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 (ISO 24362-1:2017)
Textilien - Verfahren für die Bestimmung gewisser aromatischer Amine aus

Azofarbstoffen - Teil 1: Nachweis der Verwendung gewisser Azofarbstoffe mit und ohne

Extraktion der Fasern (ISO 24362-1:2017)
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 (ISO 24362-1:2017)
Ta slovenski standard je istoveten z: EN ISO 14362-1:2017
ICS:
59.080.01 Tekstilije na splošno Textiles in general
SIST EN ISO 14362-1:2017 sl,en,fr

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 14362-1:2017
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SIST EN ISO 14362-1:2017
EN ISO 14362-1
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2017
EUROPÄISCHE NORM
ICS 59.060.01 Supersedes EN 14362-1:2012
English 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 (ISO 14362-1:2017)

Textiles - Méthodes de détermination de certaines Textilien - Verfahren für die Bestimmung gewisser

amines aromatiques dérivées de colorants azoïques - aromatischer Amine aus Azofarbstoffen - Teil 1:

Partie 1: Détection de l'utilisation de certains colorants Nachweis der Verwendung gewisser Azofarbstoffe mit

azoïques accessibles avec ou sans extraction (ISO und ohne Extraktion der Fasern (ISO 14362-1:2017)

14362-1:2017)
This European Standard was approved by CEN on 21 December 2016.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14362-1:2017 E

worldwide for CEN national Members.
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SIST EN ISO 14362-1:2017
EN ISO 14362-1:2017 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 14362-1:2017
EN ISO 14362-1:2017 (E)
European foreword

This document (EN ISO 14362-1:2017) has been prepared by Technical Committee ISO/TC 38

"Textiles" in collaboration with 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 2017, and conflicting national standards shall

be withdrawn at the latest by August 2017.

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 14362-1:2012.

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, Former Yugoslav Republic of Macedonia,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,

Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
Endorsement notice

The text of ISO 14362-1:2017 has been approved by CEN as EN ISO 14362-1:2017 without any

modification.
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SIST EN ISO 14362-1:2017
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SIST EN ISO 14362-1:2017
INTERNATIONAL ISO
STANDARD 24362-1
First edition
2014-02-01
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 colorants azoïques
accessibles avec ou sans extraction
Reference number
ISO 24362-1:2014(E)
ISO 2014
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 General ............................................................................................................................................................................................................................ 1

4 Principle ........................................................................................................................................................................................................................ 3

5 Safety precautions .............................................................................................................................................................................................. 3

6 Reagents ........................................................................................................................................................................................................................ 3

7 Apparatus ..................................................................................................................................................................................................................... 5

8 Test specimen sampling and preparation .................................................................................................................................. 6

8.1 General ........................................................................................................................................................................................................... 6

8.2 Textile article ............................................................................................................................................................................................ 6

8.3 Fibre composition ................................................................................................................................................................................ 7

8.4 Case of the fibre blends.................................................................................................................................................................... 7

8.5 Printed materials .................................................................................................................................................................................. 7

8.6 Colours ........................................................................................................................................................................................................... 7

9 Procedure..................................................................................................................................................................................................................... 8

9.1 Colorant extraction for disperse dyes ................................................................................................................................. 8

9.2 Textiles dyed with dyes other than disperse dyes .................................................................................................... 8

9.3 Reductive cleavage ............................................................................................................................................................................... 8

9.4 Separation and concentration of the amines ................................................................................................................ 9

9.5 Amine detection and quantification ..................................................................................................................................... 9

9.6 Check procedure .................................................................................................................................................................................... 9

10 Evaluation .................................................................................................................................................................................................................11

10.1 General ........................................................................................................................................................................................................11

10.2 Calculation of amine in the sample ....................................................................................................................................11

10.3 Reliability of the method .............................................................................................................................................................11

11 Test report ................................................................................................................................................................................................................11

Annex A (informative) Chromatographic analyses .............................................................................................................................12

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

Annex C (informative) Assessment guide — Interpretation of analytical results ..............................................17

Annex D (informative) Explanatory table of dyestuffs used in various textile materials ...........................19

Annex E (informative) Procedure for liquid-liquid-extraction without diatomaceous earth................21

Annex F (normative) Colorants-Methods for determination of certain aromatic amines ........................24

Bibliography .............................................................................................................................................................................................................................25

© ISO 2014 – All rights reserved iii
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directives

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any

patent rights identified during the development of the document will be in the Introduction and/or on

the ISO list of patent declarations received. www.iso.org/patents

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 38, Textiles.

ISO 24362 consists of the following parts, under the general title 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

— Part 3: Detection of the use of certain azo colorants, which may release 4-aminoazobenzene

iv © ISO 2014 – All rights reserved
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
Introduction

This part of ISO 24362 is based on EN 14362-1:2012 which has been prepared by Technical Committee

CEN/TC 248 “Textiles and textile products”, the secretariat of which is held by BSI.

© ISO 2014 – All rights reserved v
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SIST EN ISO 14362-1:2017
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SIST EN ISO 14362-1:2017
INTERNATIONAL STANDARD ISO 24362-1:2014(E)
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
1 Scope

This part of ISO 24362 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 a reducing agent with and without extraction.

Azo colorants accessible to a 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, modacrylic, aramid 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 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.

ISO 3696:1987, Water for analytical laboratory use — Specification and test methods

3 General

Certain azo colorants may release, by reductive cleavage of azo group(s), one or more of the following

aromatic amines.
© ISO 2014 – All rights reserved 1
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
Table 1 — Aromatic amines subjected
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
5 97–56–3 611–006–00–3 202–591–2 o-aminoazotoluene
4-amino-2’,3-dimethylazobenzene
4-o-tolylazo-o-toluidine
6 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
22 60–09–3 611–008–00–4 200–453–6 4-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 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 ISO 24362-3..
2 © ISO 2014 – All rights reserved
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
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

WARNING — The substances [amines] listed in Clause 3 are classified as substances known to be

or suspected of being human carcinogens.

5.1 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.

WARNING — This is a toxic chemical. To handle chlorobenzene, special care is required to prevent

skin contact swallowing and aspiration.
© ISO 2014 – All rights reserved 3
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
6.2 Acetonitrile.
6.3 Methanol.
6.4 t-butyl methyl ether.
6.5 n-pentane.
6.6 Citrate/sodium hydroxide buffer solution, pH = 6, c = 0,06 mol/l .
6.7 Aqueous sodium dithionite solution, ρ = 200 mg/ml freshly (daily) prepared.
6.8 Diatomaceous earth.

6.9 Amine substances, amines 1 to 21 (as specified in Table 1), and aniline and 1,4-phenylenediamine,

all of the 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 ISO 3696:1987.
1) c is citrate concentration.
2) ρ is the mass concentration.
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
7 Apparatus
7.1 Extraction apparatus, according to Figure 1, consisting of:
— 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, capable of ultrasonic power 160 Watt RMS, with controllable heating equipment.

7.3 Reaction vessel (20 ml to 50 ml) of heat-resistant glass, with tight closure.

7.4 Heating source, capable of maintaining the temperature at (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 a 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 variable 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) equipment, with gradient elution and

diode array detector (DAD) or mass selective detector (MS).

7.8.3 Gas chromatography (GC) equipment,with flame ionization detector (FID) or mass selective

detector (MS).
© ISO 2014 – All rights reserved 5
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
7.8.4 Capillary electrophoresis (CE) equipment,with diode array detector (DAD).
NOTE A description of the chromatographic equipment is given in Annex A.
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.

NOTE If there are omitted portions of sampling because of less than 0,2 g, record the details in the test

report.
Embroideries shall be weighed with the ground fabric.
6 © ISO 2014 – All rights reserved
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SIST EN ISO 14362-1:2017
ISO 24362-1:2014(E)
8.3 Fibre composition

As the application of this part of ISO 24362 is partly based on the extraction of colorants, identify the

nature of the textile
...

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