BS EN ISO 18218-1-2015 Leather Determination of ethoxylated alkylphenols Direct method《皮革 乙氧基烷基酚的测定 直接法》.pdf

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1、BSI Standards PublicationBS EN ISO 18218-1:2015Leather Determination ofethoxylated alkylphenolsPart 1: Direct methodBS EN ISO 18218-1:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 18218-1:2015.The UK participation in its preparation was entrusted to T

2、echnical 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 application

3、. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 78776 8 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 Committee

4、 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 18218-1 June 2015 ICS 59.140.30 English Version Leather - Determination of ethoxylated alkylphenols - Part 1: Direct method (ISO 18218-1:2015) Cuir - Dt

5、ermination chimique des alkylphnols thoxyls - Partie 1: Mthode directe (ISO 18218-1:2015) Leder - Bestimmung von ethoxylierten Alkylphenolen - Teil 1: Direktes Verfahren (ISO 18218-1:2015) This European Standard was approved by CEN on 28 February 2015. CEN members are bound to comply with the CEN/CE

6、NELEC 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

7、 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 o

8、fficial 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, Netherlan

9、ds, 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 rights

10、of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 18218-1:2015 EBS EN ISO 18218-1:2015EN ISO 18218-1:2015 (E) 3 European foreword This document (EN ISO 18218-1:2015) has been prepared by Technical Committee CEN/TC 289 “Leather”,the secretariat

11、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 by Decem

12、ber 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 patent

13、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 Macedonia, Franc

14、e, 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 18218-1:2015 has been approved by CEN as EN ISO

15、18218-1:2015 without any modification. BS EN ISO 18218-1:2015ISO 18218-1:2015(E)IULTCS/IUC 28-1:2015(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Apparatus and materials 15 Chemicals . 26 Sampling 27 Sample preparation and analysis 37.1 Extraction 37.2 Analysis 37.3 C

16、alibration 37.4 Calculation 38 Test report . 3Annex A (informative) Chromatographic analysis operating parameters 5Bibliography 7 ISO 2015 All rights reserved iiiContents PageBS EN ISO 18218-1:2015ISO 18218-1:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide fede

17、ration 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 commi

18、ttee. 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

19、 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

20、 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

21、 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

22、 and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 18218-1 was prepared by the Chemical Test Commission of the International Union

23、 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 cooperation between ISO and

24、 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 tes

25、ting 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 methodIULTCS/IUC

26、28-1:2015(E)iv ISO 2015 All rights reservedBS EN ISO 18218-1:2015ISO 18218-1:2015(E)IntroductionNonylphenol ethoxylate belongs to the non-ionic surfactants. The biodegradation of nonylphenol ethoxylate releases the persistent pollutant, the branched nonylphenol. Nonylphenol is a hormonal acting subs

27、tance that is toxic for waterborne organisms and many other organisms. For this reason the release of nonylphenol ethoxylate into the environment should be avoided.In 2003 the European Directive 2003/53/EC restricted the sale and use of nonylphenol and nonylphenol ethoxylate in product preparations

28、for industries with discharges to waste water. Preparations containing concentrations equal or higher than 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 n

29、onylphenol ethoxylate can be given, it is assigned the general structural formula:Calkylchain, branched or linear Ph -OCH CH -OHwit922n()hhPh=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 fol

30、lowing 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 individ

31、ual 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 prepar

32、ed for analysing leather samples.This part of ISO 18218 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

33、 nonylphenol ethoxylate and octylphenol ethoxylate.ISO 18218-2 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) equipme

34、nt. This method can also be used to indirectly determine the alkylphenol ethoxylate content in leather and process auxiliaries.IULTCS/IUC 28-1:2015(E) ISO 2015 All rights reserved vBS EN ISO 18218-1:2015BS EN ISO 18218-1:2015Leather Determination of ethoxylated alkylphenols Part 1: Direct method1 Sc

35、opeThis part of ISO 18218 is a method for determining ethoxylated alkylphenols (nonyphenol ethoxylate NPEOnwith 1 n 16 and octylphenol ethoxylate OPEOnwith 1 n 16) in leather. This direct method is especially suitable where a larger number of leather samples are to be checked for the presence of eth

36、oxylated alkylphenols.This method requires the use of high-performance liquid chromatography (HPLC) with triple quadrupole mass spectrometer (MSMS) to identify and quantify the ethoxylated alkylphenols.NOTE 1 In the leather industry, the most commonly used commercial ethoxylated alkylphenol is the N

37、PEO with an average of 9 EO. It has an optimum cloud point in water for the typical leather processing temperatures of 40 C to 55 C.NOTE 2 ISO 18218-1 and ISO 18218-2 use different solvents for the extraction of the ethoxylated alkylphenols from leather. Consequently, the two analytical methods are

38、expected to give similar trends but not necessarily 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 referen

39、ces, 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 locationISO 3696, Water for analytical laboratory use Specification and test m

40、ethodsISO 4044, Leather Chemical tests Preparation of chemical test samples3 PrincipleThe leather sample is extracted in methanol using an ultrasonic bath. Subsequently, an aliquot of the solution can, after filtering, be directly analysed without further cleaning of the sample using high-performanc

41、e liquid chromatography (HPLC) with a triple quadrupole mass spectrometer (MSMS).4 Apparatus and materialsNormal laboratory apparatus and, in particular, the following:4.1 Ultrasonic bath, with controllable heating capable of maintaining a temperature of (70 5) C.4.2 Glass container with a screw cap

42、 (22 ml has been found suitable).4.3 Polypropylene or polyethylene syringe, 2 ml.4.4 Syringe membrane filters, pore size 0,2 m, for use with syringe (4.3).INTERNATIONAL STANDARDISO 18218-1:2015(E)IULTCS/IUC 28-1:2015(E) ISO 2015 All rights reserved 1BS EN ISO 18218-1:2015ISO 18218-1:2015(E)4.5 Volum

43、etric flasks, 10 ml and 100 ml.4.6 Analytical balance, weighing to 1 mg.4.7 Pipettes, various sizes, 1 ml to 5 ml.4.8 Instrumental equipment, high-performance liquid chromatograph with gradient elution and triple quadrupole mass spectrometer (HPLC-MSMS).5 ChemicalsIf not otherwise defined, analytica

44、l reagent grade chemicals shall be used.5.1 Methanol.5.2 Nonylphenol ethoxylate, NPEOnwith n = 9 10, CAS No. 68412-54-4, Sigma-AldrichProduct No. T9284 (IGEPALCO-630)1), technical grade.NOTE The brand name is given to improve the comparability of test results amongst laboratories. The commercial non

45、ylphenol ethoxylate contains groups of ethoxylates of nonylphenol with linear and branched structures, so use of another reference can lead to different results. Only technical grade references are currently available from laboratory chemical suppliers.5.3 Octylphenol ethoxylate, OPEOnwith n = 9 10,

46、 CAS No. 9002-93-1, Sigma-AldrichProduct No. 542334 (Triton X-100)1), technical grade.NOTE The brand name is given to improve the comparability of test results amongst laboratories. The commercial octylphenol ethoxylate contains groups of ethoxylates of octylphenol with linear and branched structure

47、s, so use of another reference can lead to different results. Only technical grade references are currently available from laboratory chemical suppliers.5.4 Stock solution of nonylphenol ethoxylate and octylphenol ethoxylate, = 250 g/ml.25 mg of the respective alkylphenol ethoxylate (5.2 and 5.3) ar

48、e dissolved in different 100 ml volumetric flasks (4.5) with methanol (5.1) and filled up to the mark.5.5 Calibration solutions of nonylphenol ethoxylate and octylphenol ethoxylateFour calibration solutions of = 2,5 g/ml, = 5 g/ml and = 10 g/ml and = 50 g/ml for each alkylphenol ethoxylate are prepa

49、red using the respective stock solution (5.4).5.6 Formic acid.5.7 Water, deionised or distilled water, grade 3 according to ISO 3696.6 SamplingThe sampling shall be made according to ISO 2418. If a sampling according to ISO 2418 is not possible (e.g. in case of leather from finished products like shoes, clothing, etc.) the details of the sampling shall be given in the test report. Glue residuals shall be mechanically removed from leather samples.1) Sigma-AldrichProduct No. T9284 (IGEPALCO-630)