SIST EN ISO 18218-2:2015

Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2015)

This standard specifies a method for the determination of ethoxylated alkylphenols  by an indirect method

Leder - Chemische Bestimmung von ethoxylierten Alkylphenolen - Teil 2: Indirektes Verfahren (ISO 18218-2:2015)

Diese Norm 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 der Alkylphenolethoxylat wird durch Spaltung von Alkylphenolethoxylat und die Messung des freigesetzten Alkylphenols durchgeführt.
Die Anhänge A, B und C sind informativ.

Cuir - Détermination chimique des alkylphénols éthoxylés - Partie 2: Méthode indirecte (ISO 18218-2:2015)

ISO 18218-2:2015 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 la présente partie de l'ISO 18218 impliquent l'utilisation de solvants différents pour l'extraction des alkylphénols éthoxylés du cuir. Par conséquent, on peut s'attendre à ce que les résultats obtenus en suivant l'une des deux méthodes analytiques soient comparables à ceux obtenus en suivant la seconde méthode, 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 18218-2:2015)

Ta standard določa metodo za določevanje etoksilatnih alkilfenolov s posredno metodo.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 01-Mar-2015
• Publication Date: 26-Jul-2015
• Withdrawal Date: 12-Aug-2019
• ICS: 59.140.30 - Leather and furs
• Technical Committee: IUSN - Leather
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 08-Aug-2019
• Due Date: 31-Aug-2019
• Completion Date: 13-Aug-2019
• Ref Project: EN ISO 18218-2:2015 - Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2015)

Relations

• Replaced By: SIST EN ISO 18218-2:2019 - Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2019)
• Effective Date: 01-Sep-2019
• Replaced By: SIST EN ISO 18218-2:2019 - Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2019)
• Effective Date: 08-Jun-2022

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 18218-2:2015
01-september-2015
8VQMH'RORþHYDQMHHWRNVLODWQLKDONLOIHQRORYGHO3RVUHGQDPHWRGD,62

Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218
-2:2015)
Leder - Chemische Bestimmung von ethoxylierten Alkylphenolen - Teil 2: Indirektes
Verfahren (ISO 18218-2:2015)
Cuir - Détermination chimique des alkylphénols éthoxylés - Partie 2: Méthode indirecte
(ISO 18218-2:2015)
Ta slovenski standard je istoveten z: EN ISO 18218-2:2015
ICS:
59.140.30 Usnje in krzno Leather and furs
SIST EN ISO 18218-2:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 18218-2:2015

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SIST EN ISO 18218-2:2015

EUROPEAN STANDARD
EN ISO 18218-2

NORME EUROPÉENNE

EUROPÄISCHE NORM
June 2015
ICS 59.140.30
English Version
Leather - Determination of ethoxylated alkylphenols - Part 2:
Indirect method (ISO 18218-2:2015)
Cuir - Détermination chimique des alkylphénols éthoxylés - Leder - Bestimmung von ethoxylierten Alkylphenolen - Teil
Partie 2: Méthode indirecte (ISO 18218-2:2015) 2: Indirektes Verfahren (ISO 18218-2:2015)
This European Standard was approved by CEN on 28 February 2015.

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, 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
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 18218-2:2015 E
worldwide for CEN national Members.

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SIST EN ISO 18218-2:2015
EN ISO 18218-2:2015 (E)
Contents Page
European foreword .3

2

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SIST EN ISO 18218-2:2015
EN ISO 18218-2:2015 (E)
European foreword
This document (EN ISO 18218-2:2015) has been prepared by Technical Committee CEN/TC 289 “Leather”,
the secretariat of which is held by UNI, in collaboration with Technical Committee IULTCS “International Union
of Leather Technologists and Chemists Societies”.
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 December 2015, and conflicting national standards shall be withdrawn
at the latest by December 2015.
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.
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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 18218-2:2015 has been approved by CEN as EN ISO 18218-2:2015 without any modification.

3

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SIST EN ISO 18218-2:2015

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SIST EN ISO 18218-2:2015
INTERNATIONAL ISO
STANDARD 18218-2
IULTCS/IUC 28-2
First edition
2015-06-15
Leather — Determination of
ethoxylated alkylphenols —
Part 2:
Indirect method
Cuir — Détermination chimique des alkylphénols éthoxylés —
Partie 2: Méthode indirecte
Reference numbers
ISO 18218-2:2015(E)
IULTCS/IUC 28-2:2015(E)
©
ISO 2015

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015(E)
IULTCS/IUC 28-2:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, Published in Switzerland
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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2015 – All rights reserved

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015(E)
IULTCS/IUC 28-2:2015(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Apparatus and materials. 2
5 Chemicals . 2
6 Sampling and sample preparation . 3
6.1 Preparation of leather samples. 3
6.1.1 Sampling and preparation of samples . 3
6.1.2 Sample extraction . 3
6.2 Preparation of leather process auxiliary samples . 3
6.3 Blank determination . 4
6.4 Determination of OP and NP . 4
6.5 Determination of OPEO and NPEO . 4
6.6 Chromatographic analysis . 5
6.7 Evaluation . 5
7 Calibration . 5
7.1 Calibration for OP and NP . 5
7.2 Calibration for OPEO and NPEO . 5
8 Calculation . 6
8.1 Calculation of OP and NP . 6
8.2 Calculation of OPEO and NPEO . 6
9 Test report . 7
Annex A (informative) Preparation of aluminium triiodide . 8
Annex B (informative) Example of HPLC chromatograms . 9
Annex C (informative) Example of GC-MS chromatograms .11
Bibliography .13
© ISO 2015 – All rights reserved iii

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015(E)
IULTCS/IUC 28-2:2015(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 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
ISO 18218-2 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.
ISO 18218 consists of the following parts, under the general title Leather — Determination of ethoxylated
alkylphenols:
— Part 1: Direct method
— Part 2: Indirect method
iv © ISO 2015 – All rights reserved

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015(E)
IULTCS/IUC 28-2:2015(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 has to 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 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 analysing 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 part of ISO 18218 is 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 2015 – All rights reserved v

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SIST EN ISO 18218-2:2015

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015(E)
INTERNATIONAL STANDARD
IULTCS/IUC 28-2:2015(E)
Leather — Determination of ethoxylated alkylphenols —
Part 2:
Indirect method
1 Scope
This part of ISO 18218 is 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 part of ISO 18218 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, 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 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 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 NPEO and
9
OPEO respectively. Examples of the four analytes used for the determination are shown in Table 1.
10
Table 1 — Analytes determinable by this method
a
Analyte Empirical formula Abbreviation CAS no.
4-nonylphenol (mixture of isomers) C H -C H -OH NP 84852–15–3
9 19 6 4
4-tert-octylphenol C H -C H -OH OP 140–66–9
8 17 6 4
Nonylphenol ethoxylate C H -C H -(OC H ) OH (n≈9) NPEO 9016–45–9
9 19 6 4 2 4 n 9
a
CAS = Chemical Abstract Service.
© ISO 2015 – All rights reserved 1

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SIST EN ISO 18218-2:2015
ISO 18218-2:2015
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