Textiles - Method for the detection and determination of alkylphenol ethoxylates (APEO) - Part 2: Method using NPLC (ISO 18254-2:2018)

This document specifies the normal phase liquid chromatography (NPLC) separation method for the qualitative and quantitative analysis of extractable alkylphenol ethoxylates (APEO) in textiles and textile products.
This method provides several instrument options for the determination of alkylphenol ethoxylates (APEO) such as normal phase liquid chromatograph with mass spectrometer (NPLC/MS), normal phase liquid chromatograph with fluorescence detector (NPLC/FLD), normal phase liquid chromatograph with charged aerosol detector (NPLC/CAD) and normal phase liquid chromatograph with evaporative light scattering detector (NPLC/ELSD).

Textilien - Verfahren zum Nachweis und zur Bestimmung von Alkylphenolethoxylaten (APEO) - Teil 2: Verfahren unter Verwendung von NPLC (ISO 18254-2:2019)

Dieses Dokument legt das Normalphasenflüssigchromatographie Trennverfahren (NPLC) zur quantitativen und qualitativen Analyse extrahierbarer Alkylphenolethoxylate (APEO) in Textilien und textilähnlichen Produkten fest.
Dieses Verfahren bietet verschiedene Geräteoptionen zur Bestimmung von extrahierbaren Alkylphenol-ethoxylaten (APEO), z. B. Normalphasenflüssigchromatographie mit Massenspektrometer (NPLC/MS), Normalphasenflüssigchromatographie mit Fluoreszenzdetektor (NPLC/FLD), Normalphasenflüssig-chromatographie mit geladenem Aerosoldetektor (NPLC/CAD) und Normalphasenflüssigchroma¬tographie mit Verdampfungs Lichtstreudetektor (NPLC/ELSD).

Textiles - Méthode de détection et de détermination des alkylphénols éthoxylés (APEO) - Partie 2: Méthode utilisant la CLPN (ISO 18254-2:2018)

Le présent document spécifie la méthode de séparation par chromatographie liquide en phase normale (CLPN) pour l'analyse qualitative et quantitative des alkylphénols éthoxylés (APEO) extractibles dans les produits textiles et les produits connexes.
Cette méthode propose plusieurs options d'instruments pour la détermination des alkylphénols éthoxylés (APEO), notamment la chromatographie liquide en phase normale couplée à un spectromètre de masse (CLPN-MS), la chromatographie liquide en phase normale couplée à un détecteur de fluorescence (CLPN-FLD), la chromatographie liquide en phase normale couplée à un détecteur d'aérosols chargés (CLPN-CAD) et la chromatographie liquide en phase normale couplée à un détecteur évaporatif à diffusion de lumière (CLPN-DEDL).

Tekstilije - Metoda za odkrivanje in določevanje alkilfenoletoksilatov (APEO) - 2. del: Metoda z uporabo NPLC (ISO 18254-2:2018)

Ta dokument določa metodo ločevanja tekočinske kromatografije v običajni fazi (NPLC) za kvalitativno in kvantitativno analizo alkilfenoletoksilatov (APEO) v tekstilu in tekstilnih izdelkih, ki jih je mogoče ekstrahirati.
Ta metoda podaja več instrumentnih možnosti za določevanje alkilfenoletoksilatov (APEO), na primer tehniko tekočinske kromatografije z masno spektrometrijo v običajni fazi (NPLC/MS), tekočinske kromatografije s fluorescenčnim detektorjem v običajni fazi (NPLC/FLD), tekočinske kromatografije z detektorjem naelektrenih aerosolov v običajni fazi (NPLC/CAD) ter tekočinske kromatografije z izparilnim detektorjem razprševanja svetlobe v običajni fazi (NPLC/ELSD).

General Information

Status
Published
Publication Date
05-Feb-2019
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
06-Feb-2019
Completion Date
06-Feb-2019

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SLOVENSKI STANDARD
SIST EN ISO 18254-2:2019
01-april-2019

7HNVWLOLMH0HWRGD]DRGNULYDQMHLQGRORþHYDQMHDONLOIHQROHWRNVLODWRY $3(2 

GHO0HWRGD]XSRUDER13/& ,62

Textiles - Method for the detection and determination of alkylphenol ethoxylates (APEO)

- Part 2: Method using NPLC (ISO 18254-2:2018)
Textilien - Verfahren zum Nachweis und zur Bestimmung von Alkylphenolethoxylaten
(APEO) - Teil 2: Verfahren unter Verwendung von NPLC (ISO 18254-2:2018)

Textiles - Méthode de détection et de détermination des alkylphénols éthoxylés (APEO) -

Partie 2: Méthode utilisant la CLPN (ISO 18254-2:2018)
Ta slovenski standard je istoveten z: EN ISO 18254-2:2019
ICS:
59.080.01 Tekstilije na splošno Textiles in general
SIST EN ISO 18254-2:2019 en,fr,de

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

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SIST EN ISO 18254-2:2019
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SIST EN ISO 18254-2:2019
EN ISO 18254-2
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2019
EUROPÄISCHE NORM
ICS 59.080.01
English Version
Textiles - Method for the detection and determination of
alkylphenol ethoxylates (APEO) - Part 2: Method using
NPLC (ISO 18254-2:2018)

Textiles - Méthode de détection et de détermination Textilien - Verfahren zum Nachweis und zur

des alkylphénols éthoxylés (APEO) - Partie 2: Méthode Bestimmung von Alkylphenolethoxylaten (APEO) - Teil

utilisant la CLPN (ISO 18254-2:2018) 2: Verfahren unter Verwendung von NPLC (ISO 18254-

2:2018)
This European Standard was approved by CEN on 10 December 2018.

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: Rue de la Science 23, B-1040 Brussels

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 18254-2:2019 E

worldwide for CEN national Members.
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SIST EN ISO 18254-2:2019
EN ISO 18254-2:2019 (E)
Contents Page

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

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SIST EN ISO 18254-2:2019
EN ISO 18254-2:2019 (E)
European foreword

This document (EN ISO 18254-2:2019) 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 2019, and conflicting national standards shall

be withdrawn at the latest by August 2019.

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

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

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 18254-2:2018 has been approved by CEN as EN ISO 18254-2:2019 without any

modification.
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SIST EN ISO 18254-2:2019
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SIST EN ISO 18254-2:2019
INTERNATIONAL ISO
STANDARD 18254-2
First edition
2018-12
Textiles — Method for the detection
and determination of alkylphenol
ethoxylates (APEO) —
Part 2:
Method using NPLC
Textiles — Méthode de détection et de détermination des alkylphénols
éthoxylés (APEO) —
Partie 2: Méthode utilisant la CLPN
Reference number
ISO 18254-2:2018(E)
ISO 2018
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SIST EN ISO 18254-2:2019
ISO 18254-2:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018

All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved
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SIST EN ISO 18254-2:2019
ISO 18254-2:2018(E)
Contents Page

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

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

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

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

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Procedure..................................................................................................................................................................................................................... 3

7.1 Standard preparation ........................................................................................................................................................................ 3

7.2 Mobile phase for HPLC ..................................................................................................................................................................... 3

7.2.1 Methanol with 0,1 % formic acid and 0,01 % ammonium formate ..................................... 3

7.2.2 Acetonitrile with 0,1 % formic acid ................................................................................................................. 3

7.3 Sample preparation ............................................................................................................................................................................ 3

7.4 Sample extraction ................................................................................................................................................................................. 3

7.5 Sample analysis ...................................................................................................................................................................................... 4

8 Calculation and calibration ....................................................................................................................................................................... 4

8.1 Calculation of contribution percentage of each APEO congener in standard solution ............. 4

8.2 Calculation of concentration of each APEO congener in standard solution ....................................... 4

8.3 Calculation of concentration of each APEO congener in sample ................................................................. 4

8.4 Calculation of total concentration of all APEO congener in sample .......................................................... 5

8.5 Calibration curve ................................................................................................................................................................................... 5

9 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Examples of chromatographic condition ........................................................................................... 6

Annex B (informative) Examples of solid phase extraction (SPE) procedure for clean up .......................14

Annex C (informative) Results of the interlaboratory test..........................................................................................................15

Annex D (informative) Study of the contribution percentage (mole fraction) of APEO congeners ..16

Bibliography .............................................................................................................................................................................................................................18

© ISO 2018 – All rights reserved iii
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SIST EN ISO 18254-2:2019
ISO 18254-2:2018(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 (see 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 (see 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 of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso

.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 38, Textiles.
A list of all parts in the ISO 18254 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2018 – All rights reserved
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SIST EN ISO 18254-2:2019
ISO 18254-2:2018(E)
Introduction

This document specifies the normal phase liquid chromatography (NPLC) separation method for the

quantitative and qualitative analysis of extractable alkylphenol ethoxylates (APEO) in textile and

textile products. NPLC separation method enables alkylphenol ethoxylates to be analysed by high

performance liquid chromatograph (HPLC) with Mass Spectrometer (MS), fluorescence detector (FD),

charged aerosol detector (CAD) and evaporative light scattering detector (ELSD).

A study of the contribution percentage (mole fraction) of APEO congeners is presented in Annex D.

© ISO 2018 – All rights reserved v
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SIST EN ISO 18254-2:2019
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SIST EN ISO 18254-2:2019
INTERNATIONAL STANDARD ISO 18254-2:2018(E)
Textiles — Method for the detection and determination of
alkylphenol ethoxylates (APEO) —
Part 2:
Method using NPLC

WARNING — This document calls for the use of substances/procedures that may be injurious to

the health/environment if appropriate conditions are not observed. It refers only to technical

suitability and does not absolve the user from legal obligations relating to health and safety/

environment at any stage.
1 Scope

This document specifies the normal phase liquid chromatography (NPLC) separation method for the

qualitative and quantitative analysis of extractable alkylphenol ethoxylates (APEO) in textiles and

textile products.

This method provides several instrument options for the determination of alkylphenol ethoxylates

(APEO) such as normal phase liquid chromatograph with mass spectrometer (NPLC/MS), normal phase

liquid chromatograph with fluorescence detector (NPLC/FLD), normal phase liquid chromatograph

with charged aerosol detector (NPLC/CAD) and normal phase liquid chromatograph with evaporative

light scattering detector (NPLC/ELSD).
2 Normative references
There are no normative references in this document.
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Principle

The test specimen is cut into small pieces, transferred to a sample vial and treated with methanol

in ultrasonic water bath. The extract is filtered and collected. Subsequently, the collected extract is

analysed by NPLC/MS, NPLC/FLD, NPLC/CAD or NPLC/ELSD.
5 Reagents
Unless otherwise specified, analytical grade chemicals shall be used.
© ISO 2018 – All rights reserved 1
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SIST EN ISO 18254-2:2019
ISO 18254-2:2018(E)

5.1 Octylphenol ethoxylates (Triton® X-100), (OPEO) CAS No.9002-93-1, Sigma Aldrich® Part

No.T9284 (see NOTE in 5.2).

5.2 Nonylphenol ethoxylates (IGEPAL® CO-630), (NPEO) CAS No.68412-54-4, Sigma Aldrich® Part

No. 542334.

NOTE The mentioned brand names in 5.1 and 5.2 are given to improve the comparability of the test results

amongst laboratories. Using another batch or another supplier could lead to different results.

5.3 Methanol (HPLC grade).
5.4 Acetonitrile (HPLC grade).
5.5 Acetone (HPLC grade).
5.6 Ammonium formate (HPLC grade).
5.7 Formic acid (HPLC grade).
6 Apparatus
6.1 General

Clean all glassware by rinsing with acetone (5.5) prior to use. Avoid detergents when washing labware.

6.2 Apparatus and auxiliaries for preparing the sample
6.2.1 Standard laboratory equipment.

6.2.2 Analytical balance with resolution of 0,01 g (for test specimen preparation).

6.2.3 Analytical balance with resolution of 0,001 g (for standard preparation).
6.2.4 40 ml Glass vial with screw cap (for sample pre-treatment).
6.2.5 Ultrasonic water bath (to be set up at (70 ± 5) °C).
6.2.6 Disposable syringe and membrane filter (with 0,45 μm pore size or less).
6.2.7 Glass vial (with septum cap for HPLC).
6.2.8 Solid phase extraction (SPE) cartridge for clean up (optional).

The cartridge is packed with a minimum of 200 mg of sorbent (reverse phase or silica).

6.2.9 Solid
...

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