1、BSI Standards PublicationBS EN ISO 18218-2:2015Leather Determination ofethoxylated alkylphenolsPart 2: Indirect methodBS EN ISO 18218-2:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 18218-2:2015.The UK participation in its preparation was entrusted to
2、 Technical Committee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct applicati
3、on. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 78777 5 ICS 59.140.30 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committ
4、ee on 30 June 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 18218-2 June 2015 ICS 59.140.30 English Version Leather - Determination of ethoxylated alkylphenols - Part 2: Indirect method (ISO 18218-2:2015) Cuir
5、- Dtermination chimique des alkylphnols thoxyls - Partie 2: Mthode indirecte (ISO 18218-2:2015) Leder - Bestimmung von ethoxylierten Alkylphenolen - Teil 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 th
6、e 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 Managemen
7、t 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
8、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, N
9、etherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All
10、 rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 18218-2:2015 EBS EN ISO 18218-2:2015EN ISO 18218-2:2015 (E) 3 European foreword This document (EN ISO 18218-2:2015) has been prepared by Technical Committee CEN/TC 289 “Leather”,the secr
11、etariat of which is held by UNI, in collaboration with Technical Committee IULTCS “International Unionof Leather Technologists and Chemists Societies”. This European Standard shall be given the status of a national standard, either by publication of an identicaltext or by endorsement, at the latest
12、by December 2015, and conflicting national standards shall be withdrawnat the latest by December 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patentrights. CEN and/or CENELEC shall not be held responsible for identifying any or all such
13、 patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, CzechRepublic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedoni
14、a, 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
15、 EN ISO 18218-2:2015 without any modification. BS EN ISO 18218-2:2015ISO 18218-2:2015(E)IULTCS/IUC 28-2:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Apparatus and materials 25 Chemicals . 26 Sampling and sample preparation 36.1 Preparation of leather samples. 36.
16、1.1 Sampling and preparation of samples . 36.1.2 Sample extraction . 36.2 Preparation of leather process auxiliary samples 36.3 Blank determination 46.4 Determination of OP and NP . 46.5 Determination of OPEO and NPEO 46.6 Chromatographic analysis . 56.7 Evaluation 57 Calibration 57.1 Calibration fo
17、r OP and NP 57.2 Calibration for OPEO and NPEO . 58 Calculation 68.1 Calculation of OP and NP 68.2 Calculation of OPEO and NPEO . 69 Test report . 7Annex A (informative) Preparation of aluminium triiodide 8Annex B (informative) Example of HPLC chromatograms 9Annex C (informative) Example of GC-MS ch
18、romatograms 11Bibliography .13 ISO 2015 All rights reserved iiiContents PageBS EN ISO 18218-2:2015ISO 18218-2:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standa
19、rds 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 tak
20、e 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 par
21、ticular 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
22、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 w
23、ww.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 ISOs adherence to t
24、he WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 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
25、 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 profess
26、ional 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 o
27、f 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 methodIULTCS/IUC 28-2:2015(E)iv ISO 2015 All rights reservedBS EN ISO 18218-2:2015ISO 18218-2:2015(E)IntroductionNon
28、ylphenol 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 n
29、onylphenol 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
30、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:(C9alkyl chain, branched
31、or linear) Ph OCH2CH2nOH (with Ph = phenyl, n 1)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 a
32、lkyl 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 etho
33、xylate 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 alkylphe
34、nol. 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 alkylpheno
35、l. 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
36、 process auxiliaries.IULTCS/IUC 28-2:2015(E) ISO 2015 All rights reserved vBS EN ISO 18218-2:2015ISO 18218-2:2015(E)BS EN ISO 18218-2:2015Leather Determination of ethoxylated alkylphenols Part 2: Indirect method1 ScopeThis part of ISO 18218 is a method for determining alkylphenols (nonylphenol and o
37、ctylphenol) 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
38、 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 necessa
39、rily the same absolute result for the ethoxylated alkylphenol content in leather.2 Normative referencesThe 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 undate
40、d references, the latest edition of the referenced document (including any amendments) applies.ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling locationISO 3696:1987, Water for analytical laboratory use Specification and test methodsISO 4044, Leather Chemical tests Pre
41、paration of chemical test samples3 PrincipleLeather 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
42、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. T
43、he contents of NPEO and OPEO are then calculated by normalizing to NPEO9and OPEO10respectively. Examples of the four analytes used for the determination are shown in Table 1.Table 1 Analytes determinable by this methodAnalyte Empirical formula Abbreviation CASano.4-nonylphenol (mixture of isomers) C
44、9H19-C6H4-OH NP 848521534-tert-octylphenol C8H17-C6H4-OH OP 140669Nonylphenol ethoxylate C9H19-C6H4-(OC2H4)nOH (n9) NPEO99016459aCAS = Chemical Abstract Service.INTERNATIONAL STANDARDISO 18218-2:2015(E)IULTCS/IUC 28-2:2015(E) ISO 2015 All rights reserved 1BS EN ISO 18218-2:2015ISO 18218-2:2015(E)Ana
45、lyte Empirical formula Abbreviation CASano.Octyphenol ethoxylate C8H17-C6H4-(OC2H4)nOH (n10) OPEO109002931aCAS = Chemical Abstract Service.NOTE There are many CAS numbers for the nonylphenol ethoxylates and octylphenol ethoxylates. The CAS numbers in Table 1 are for the normalized structures used in
46、 the external calibration (see 7.2).4 Apparatus and materialsNormal laboratory apparatus and, in particular, the following:4.1 Analytical balance, weighing to an accuracy of 0,1 mg.4.2 Ultrasonic bath, (40 2) kHz, with thermostat capable of maintaining a temperature of (50 5) C.4.3 Separating funnel
47、s, 150 ml.4.4 Rotary evaporator, with thermostat and vacuum system.4.5 Membrane filter, polyamide, 0,45 m.4.6 HPLC, equipped with diode array detector (DAD) or fluorescence detector (FLD).4.7 GC, equipped with mass selective detector (MSD).4.8 Filter paper, fast, quantitative.5 ChemicalsUnless other
48、wise stated, analytical grade chemicals shall be used.5.1 Acetonitrile, for HPLC.5.2 n-Hexane.NOTE Iso-hexane can also be used.5.3 Aluminium triiodide, commercially available, or prepared according to Annex A.5.4 Sulfuric acid solution, 0,5 mol/L.5.5 Sodium thiosulfate solution, saturated at room te
49、mperature.5.6 Anhydrous magnesium sulfate (MgSO4), for analysis.5.7 Anhydrous sodium sulfate (Na2SO4), as desiccant for analysis. If not already an anhydrous powder, it can be treated at 800 C for 4 h, store dry.NOTE Other suitable desiccants can be used.5.8 Sodium chloride solution, saturated at room temperature.IULTCS/IUC 28-2:2015(E)Table 1 (continued)2 ISO 2015 All rights reservedBS EN ISO 18218-2:2015ISO 18218-2:2015(E)5.9 NP (in Table 1) solution, for calibration, 1 000 mg/L in n-hexane.5.10 OP (in Tab
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