Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2019)

This document specifies a method for determining alkylphenols (nonylphenol and octylphenol) and alkylphenol ethoxylates (nonylphenol ethoxylate and octylphenol ethoxylate) in leather and process auxiliaries. The analysis is based on high-performance liquid chromatography (HPLC) or gas chromatography-mass spectrometry (GC-MS).
The analysis of the alkylphenol ethoxylate is made by cleaving the alkylphenol ethoxylate and measuring the released alkylphenol.
NOTE ISO 18218-1 and this document use different solvents for the extraction of the ethoxylated alkylphenols from leather. Consequently, the two analytical methods are expected to give similar trends but not necessarily the same absolute result for the ethoxylated alkylphenol content in leather.

Leder - Bestimmung von ethoxylierten Alkylphenolen - Teil 2: Indirektes Verfahren (ISO 18218-2:2019)

Dieses Dokument legt ein Verfahren zur Bestimmung von Alkylphenol (Nonylphenol und Octylphenol) und Alkylphenolethoxylat (Nonylphenolethoxylat und Octylphenolethoxylat) in Leder und Prozesshilfsstoffen fest. Die Analyse basiert auf Hochleistungsflüssigkeitschromatographie (HPLC) oder Gaschromatographie-Massenspektrometrie (GC MS).
Die Analyse des Alkylphenolethoxylats wird durch Spaltung von Alkylphenolethoxylat und die Messung des freigesetzten Alkylphenols durchgeführt.
ANMERKUNG   ISO 18218 1 und dieses Dokument verwenden verschiedene Lösemittel zur Extraktion der ethoxylierten Alkylphenole aus Leder. Für die beiden analytischen Verfahren wird erwartet, dass sie für den Gehalt ethoxylierter Alkylphenole in Leder konsequenterweise ähnliche Tendenzen jedoch nicht zwangsläufig das absolut identische Ergebnis liefern.

Cuir - Détermination des alkylphénols éthoxylés - Partie 2: Méthode indirecte (ISO 18218-2:2019)

Le présent document spécifie une méthode de détermination des alkylphénols (le nonylphénol et l'octylphénol) et des éthoxylates d'alkylphénol (l'éthoxylate de nonylphénol et l'éthoxylate d'octylphénol) dans le cuir et les produits auxiliaires de traitement. Cette analyse est effectuée par chromatographie en phase liquide à haute performance (CLHP) ou par chromatographie en phase gazeuse couplée à la spectrométrie de masse (CG-SM).
L'éthoxylate d'alkylphénol est clivé et l'alkylphénol ainsi formé est dosé.
NOTE L'ISO 18218-1 et le présent document impliquent l'utilisation de solvants différents pour l'extraction des alkylphénols éthoxylés du cuir. Par conséquent, il est attendu que les deux méthodes analytiques donnent des résultats comparables, mais non nécessairement identiques, pour ce qui concerne la teneur en alkylphénols éthoxylés dans le cuir.

Usnje - Določevanje etoksilatnih alkilfenolov - 2. del: Posredna metoda (ISO 18218-2:2019)

Ta dokument določa metodo za določevanje alkilfenolov (nonilfenol in oktilfenol) ter alkilfenoletoksilatov (nonilfenol etoksilatov in oktilfenol etoksilatov) v usnju ter pomožnih sredstvih za predelavo. Analiza temelji na tekočinski kromatografiji visoke ločljivosti (HPLC) ali plinski kromatografiji/masni spektrometriji (GC-MS).
Analiza alkilfenoletoksilata se opravi s cepitvijo alkilfenoletoksilata in merjenjem sproščenega alkilfenola.
OPOMBA: Standard ISO 18218-1 in ta dokument uporabljata različni topili za ekstrakcijo alkilfenoletoksilatov iz usnja. Posledično je za pričakovati, da bosta analizni metodi pokazali podobne trende, ne pa nujno tudi enakega absolutnega rezultata pri vsebnosti alkilfenoletoksilata v usnju.

General Information

Status
Published
Publication Date
09-Jul-2019
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
10-Jul-2019
Completion Date
10-Jul-2019

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SLOVENSKI STANDARD
SIST EN ISO 18218-2:2019
01-september-2019
Nadomešča:
SIST EN ISO 18218-2:2015

Usnje - Določevanje etoksilatnih alkilfenolov - 2. del: Posredna metoda (ISO 18218-

2:2019)

Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218

-2:2019)

Leder - Bestimmung von ethoxylierten Alkylphenolen - Teil 2: Indirektes Verfahren (ISO

18218-2:2019)

Cuir - Détermination des alkylphénols éthoxylés - Partie 2: Méthode indirecte (ISO 18218

-2:2019)
Ta slovenski standard je istoveten z: EN ISO 18218-2:2019
ICS:
59.140.30 Usnje in krzno Leather and furs
SIST EN ISO 18218-2:2019 en,fr,de

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

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SIST EN ISO 18218-2:2019
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SIST EN ISO 18218-2:2019
EN ISO 18218-2
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2019
EUROPÄISCHE NORM
ICS 59.140.30 Supersedes EN ISO 18218-2:2015
English Version
Leather - Determination of ethoxylated alkylphenols - Part
2: Indirect method (ISO 18218-2:2019)

Cuir - Détermination des alkylphénols éthoxylés - Leder - Bestimmung von ethoxylierten Alkylphenolen -

Partie 2: Méthode indirecte (ISO 18218-2:2019) Teil 2: Indirektes Verfahren (ISO 18218-2:2019)

This European Standard was approved by CEN on 10 June 2019.

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, Republic of North Macedonia, 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 18218-2:2019 E

worldwide for CEN national Members.
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SIST EN ISO 18218-2:2019
EN ISO 18218-2:2019 (E)
Contents Page

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

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SIST EN ISO 18218-2:2019
EN ISO 18218-2:2019 (E)
European foreword

This document (EN ISO 18218-2:2019) has been prepared by Technical Committee IULTCS

"International Union of Leather Technologists and Chemists Societies" in collaboration with Technical

Committee CEN/TC 289 “Leather” the secretariat of which is held by UNI.

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 January 2020, and conflicting national standards shall

be withdrawn at the latest by January 2020.

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.

This document supersedes EN ISO 18218-2:2015.

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, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 18218-2:2019 has been approved by CEN as EN ISO 18218-2:2019 without any

modification.
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SIST EN ISO 18218-2:2019
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SIST EN ISO 18218-2:2019
INTERNATIONAL ISO
STANDARD 18218-2
IULTCS/IUC 28-2
Second edition
2019-06
Leather — Determination of
ethoxylated alkylphenols —
Part 2:
Indirect method
Cuir — Détermination des alkylphénols éthoxylés —
Partie 2: Méthode indirecte
Reference numbers
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(E)
ISO 2019
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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 2019 – All rights reserved
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(E)
Contents Page

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

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

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

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

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

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

5 Apparatus and materials.............................................................................................................................................................................. 2

6 Chemicals ..................................................................................................................................................................................................................... 2

7 Sampling and sample preparation .................................................................................................................................................... 3

7.1 Preparation of leather samples................................................................................................................................................. 3

7.1.1 Sampling and preparation of samples ........................................................................................................... 3

7.1.2 Sample extraction ........................................................................................................................................................... 3

7.2 Preparation of leather process auxiliary samples .................................................................................................... 4

7.3 Blank determination .......................................................................................................................................................................... 4

7.4 Determination of OP and NP ....................................................................................................................................................... 4

7.5 Determination of OPEO and NPEO ........................................................................................................................................ 4

7.6 Chromatographic analysis ............................................................................................................................................................. 5

7.7 Evaluation .................................................................................................................................................................................................... 5

8 Calibration .................................................................................................................................................................................................................. 5

8.1 Calibration for OP and NP .............................................................................................................................................................. 5

8.2 Calibration for OPEO and NPEO ............................................................................................................................................... 5

9 Calculation .................................................................................................................................................................................................................. 6

9.1 Calculation of OP and NP ................................................................................................................................................................ 6

9.2 Calculation of OPEO and NPEO ................................................................................................................................................. 6

10 Test report ................................................................................................................................................................................................................... 7

Annex A (normative) Preparation of aluminium triiodide ........................................................................................................... 8

Annex B (informative) Example of HPLC chromatograms .............................................................................................................. 9

Annex C (informative) Example of GC-MS chromatograms ........................................................................................................11

Bibliography .............................................................................................................................................................................................................................14

© ISO 2019 – All rights reserved iii
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(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 the Chemical Test Commission of the International Union of Leather

Technologists and Chemists Societies (IUC Commission, IULTCS) in collaboration with the European

Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of

which is held by UNI, in accordance with the agreement on technical co-operation between ISO and CEN

(Vienna Agreement).

IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to

further the advancement of leather science and technology. IULTCS has three Commissions, which

are responsible for establishing international methods for the sampling and testing of leather. ISO

recognizes IULTCS as an international standardizing body for the preparation of test methods for

leather.

This second edition cancels and replaces the first edition (ISO 18218-2:2015), which has been

technically revised as follows:
— 6.14 and 6.15 have been added;
— 7.4, 7.5 and 7.6 have been technically revised;
— 8.1 has been revised by including a reference to 6.14.
A list of all parts in the ISO 18218 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 2019 – All rights reserved
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(E)
Introduction

Nonylphenol ethoxylate belongs to the non-ionic surfactants. The biodegradation of nonylphenol

ethoxylate releases the persistent pollutant branched nonylphenol. Nonylphenol is a hormonal acting

substance that is toxic for waterborne organisms and many other organisms. For this reason, the

release of nonylphenol ethoxylate into the environment shall be avoided.

In 2003, the European Directive 2003/53/EC restricted the sale and use of nonylphenol and nonylphenol

ethoxylate in product preparations for industries with discharges to waste water. Preparations

containing concentrations equal to or higher than 0,1 % of nonylphenol ethoxylate or nonylphenol were

forbidden. This directive is included as part of the EU Regulation 1907/2006 (REACH).

No detailed composition of the chemical substance nonylphenol ethoxylate can be given; it is assigned

the general structural formula:

(C alkyl chain, branched or linear) − Ph − [OCH CH ] − OH (with Ph = phenyl, n ≥ 1)

9 2 2 n

To cover the group of ethoxylates of 4-nonylphenol, branched and linear, the European Chemical Agency

(ECHA) has assigned the substance the following definition:

‘4-nonylphenol, branched and linear, ethoxylated [substances with a linear and/or branched alkyl

chain with a carbon number of 9 covalently bound in position 4 to phenol, ethoxylated covering UVCB

and well-defined substances, polymers, and homologues, which include any of the individual isomers

and/or combinations thereof].’

In the leather industry, nonylphenol ethoxylate and octylphenol ethoxylate surfactants have been used.

However, the water insoluble substances nonylphenol and octylphenol have not been used. For this

reason, two different analytical procedures have been prepared for analysing leather samples.

ISO 18218-1 is a method that directly determines the ethoxylated alkylphenol. It is an efficient

procedure for the analysis of a larger number of leather samples. This procedure requires HPLC with

triple quadrupole mass spectrometer (MSMS) to identify the nonylphenol ethoxylate and octylphenol

ethoxylate.

This document specifies a procedure for analysing the alkylphenol. The ethoxylated alkylphenol is

cleaved to form the alkylphenol, which is identified using high-performance liquid chromatography

(HPLC) or gas chromatography-mass spectrometry (GC-MS) equipment. This method can also be used

to indirectly determine the alkylphenol ethoxylate content in leather and process auxiliaries.

© ISO 2019 – All rights reserved v
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SIST EN ISO 18218-2:2019
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
INTERNATIONAL STANDARD
IULTCS/IUC 28-2:2019(E)
Leather — Determination of ethoxylated alkylphenols —
Part 2:
Indirect method
1 Scope

This document specifies a method for determining alkylphenols (nonylphenol and octylphenol)

and alkylphenol ethoxylates (nonylphenol ethoxylate and octylphenol ethoxylate) in leather and

process auxiliaries. The analysis is based on high-performance liquid chromatography (HPLC) or gas

chromatography-mass spectrometry (GC-MS).

The analysis of the alkylphenol ethoxylate is made by cleaving the alkylphenol ethoxylate and

measuring the released alkylphenol.

NOTE ISO 18218-1 and this document use different solvents for the extraction of the ethoxylated

alkylphenols from leather. Consequently, the two analytical methods are expected to give similar trends but not

necessarily the same absolute result for the ethoxylated alkylphenol content in leather.

2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 2418, Leather — Chemical, physical and mechanical and fastness tests — Sampling location

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

ISO 4044, Leather — Chemical tests — Preparation of chemical test samples
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

Leather samples are extracted with acetonitrile using an ultrasonic bath and the nonylphenol (NP)

and/or octylphenol (OP) in the extract is quantitatively determined by HPLC or GC-MS.

The leather process auxiliaries are dissolved in acetonitrile and the NP and/or OP in the solution is

quantitatively determined by HPLC or GC-MS.

The nonylphenol ethoxylate (NPEO) and octylphenol ethoxylate (OPEO) in the extract or solution are

first converted into NP and OP, using aluminium triiodide as cleavage agent, and the NP and OP are

determined by HPLC or GC-MS. The contents of NPEO and OPEO are then calculated by normalizing to

© ISO 2019 – All rights reserved 1
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SIST EN ISO 18218-2:2019
ISO 18218-2:2019(E)
IULTCS/IUC 28-2:2019(E)

NPEO and OPEO , respectively. Examples of the four analytes used for the determination are shown

9 10
in Table 1.
Table 1
...

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