1、BSI Standards PublicationBS EN ISO 18219:2015Leather Determination ofchlorinated hydrocarbons inleather Chromatographicmethod for short-chainchlorinated paraffins (SCCP)BS EN ISO 18219:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO18219:2015.The UK par
2、ticipation in its preparation was entrusted to TechnicalCommittee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. User
3、s are responsible for its correctapplication. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 78778 2ICS 59.140.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of th
4、eStandards Policy and Strategy Committee on 31 October 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 18219 October 2015 ICS 59.140.30 English Version Leather - Determination of chlorinated hydrocarbons in leath
5、er - Chromatographic method for short-chain chlorinated paraffins (SCCP) (ISO 18219:2015) Cuir - Dosage des hydrocarbures chlors dans le cuir - Mthode chromatographique pour les paraffines chlores chane courte (PCCC) (ISO 18219:2015) Leder - Bestimmung von chlorierten Kohlenwasserstoffen in Leder -
6、Chromatographische Verfahren fr kurzkettige Chlorparaffine (SCCP) (ISO 18219:2015) This European Standard was approved by CEN on 29 August 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
7、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
8、 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, Cypr
9、us, 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 andUnited King
10、dom. 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 of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 182
11、19:2015 EBS EN ISO 18219:2015EN ISO 18219:2015 (E) 3 European foreword This document (EN ISO 18219:2015) has been prepared by Technical Committee IULTCS “InternationalUnion of Leather Technologists and Chemists Societies“ in collaboration with the Technical CommitteeCEN/TC 289 “Leather” the secretar
12、iat of which is held by UNI. This European Standard shall be given the status of a national standard, either by publication of anidentical text or by endorsement, at the latest by April 2016, and conflicting national standards shall bewithdrawn at the latest by April 2016. Attention is drawn to the
13、possibility that some of the elements of this document may be the subject ofpatent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patentrights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of thefollowing countries
14、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, Por
15、tugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,Turkey and the United Kingdom. Endorsement notice The text of ISO 18219:2015 has been approved by CEN as EN ISO 18219:2015 without any modification. BS EN ISO 18219:2015ISO 18219:2015(E)IULTCS/IUC 30:2015(E)Foreword ivIntroduction v1 Sco
16、pe . 12 Normative references 13 Principle 14 Apparatus and materials 15 Chemicals . 26 Sampling 27 Sample preparation and analysis 27.1 Preparation of SCCP calibration solution (50 g/ml) with 59 % chlorination degree . 27.2 Extraction of leather . 27.3 Clean up . 37.4 GC-MS Determination . 38 Evalua
17、tion 39 Test report . 4Annex A (informative) Chromatographic analysis operating parameters 5 ISO 2015 All rights reserved iiiContents PageBS EN ISO 18219:2015ISO 18219:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
18、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, govern
19、mental 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 maintenan
20、ce 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
21、 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
22、/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 as
23、sessment, 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 18219 was prepared by the Chemical Test Commission of the International Union of Leather Technologists and Chemists Soci
24、eties (IUC Commission, IULTCS) in collaboration with the European Committee for Standardisation (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
25、 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 a
26、n international standardizing body for the preparation of test methods for leather.IULTCS/IUC 30:2015(E)iv ISO 2015 All rights reservedBS EN ISO 18219:2015ISO 18219:2015(E)IntroductionShort-chain chlorinated paraffins (SCCP) are classified as dangerous to the environment, since they are very toxic t
27、o aquatic organisms and may cause long-term adverse effects in the aquatic environment.In 2002, the European Directive 2002/45/EC restricted the sale and use of short-chain chlorinated paraffins (C10-C13) in product preparations for the fatliquoring of leather. Preparations containing concentrations
28、 equal or higher than 1 % of SCCP were forbidden. This Directive is included as part of the EU Regulation 1907/2006 (REACH). Within this EU Regulation, in October 2008, the short-chain chlorinated paraffins were added to the Candidate List of Substances of Very High Concern (SVHC).IULTCS/IUC 30:2015
29、(E) ISO 2015 All rights reserved vBS EN ISO 18219:2015BS EN ISO 18219:2015Leather Determination of chlorinated hydrocarbons in leather Chromatographic method for short-chain chlorinated paraffins (SCCP)1 ScopeThis International Standard specifies a chromatographic method to determine the amount of s
30、hort-chain chlorinated paraffins (SCCP) C10-C13in processed and unprocessed leathers.Annex A is for information only.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 t
31、he 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 4044, Leather Chemical tests Preparation of chemical test samples3 PrincipleT
32、he test sample is extracted using n-hexane at 60 C in an ultrasonic bath for 60 min. After SPE clean up, an aliquot is then analysed using a gas chromatograph fitted to a mass selective detector with chemical ionization (GC-ECNI-MS).Liquid chromatography system with single quad (LC-MS) or triple qua
33、d mass spectrometry (LC-MS/MS) can also be used if the user has demonstrated that the accuracy of measurement is equivalent to that of the GC-ECNI-MS method.4 Apparatus and materialsNormal laboratory apparatus and, in particular, the following.4.1 Analytical balance.4.2 Sealable vessel, with lid, 20
34、 ml, suitable for extraction with n-hexane.4.3 Ultrasonic bath, (temperature controlled).4.4 Pipette, 1 ml to 10 ml capacity.4.5 Volumetric flask, 2 ml.4.6 Solid phase extraction (SPE) system, with vacuum device and normal phase SPE cartridges, for example 500 mg/6 ml, e.g. Chromabond columns, Sorbe
35、nt: SiOH, 6 ml, 500 mg.4.7 PTFE membrane filter.INTERNATIONAL STANDARDISO 18219:2015(E)IULTCS/IUC 30:2015(E) ISO 2015 All rights reserved 1BS EN ISO 18219:2015ISO 18219:2015(E)4.8 Gas chromatograph and mass selective detector with chemical ionization (GC-ECNI-MS).5 ChemicalsIf not otherwise defined,
36、 analytical reagent grade chemicals shall be used.5.1 n-hexane, CAS1)No.: 110-54-3.5.2 Dichloromethane, CAS No: 75-09-2.5.3 Internal standard solution, 1,1,1,3,10,11-hexachloroundecane, CAS No: 601523-28-8, 1 000 g/ml.NOTE Other suitable internal standard can be used.5.4 Standard solutions, SCCP, C1
37、0-C13,with different chlorine content, each 100 g/ml:5.4.1 SCCP C10-C1355,5 % Cl, technical grade.5.4.2 SCCP C10-C1363 % Cl, technical grade.NOTE These SCCP calibration solutions are available commercially.5.5 Nitrogen gas.6 SamplingThe sampling shall be made according to ISO 2418. If a sampling acc
38、ording to ISO 2418 is not possible (e.g. in case of leather from finished products like shoes, clothing, etc.), the details of the sampling must be stated in the test report. Glue residuals must be mechanically removed from leather samples.The leather samples shall be ground or cut into smaller piec
39、es, not larger than 2 mm to 3 mm, according to ISO 4044.7 Sample preparation and analysis7.1 Preparation of SCCP calibration solution (50 g/ml) with 59 % chlorination degree533 l of SCCP C10-C1355,5 % Cl standard solution (5.4.1) and 467 l SCCP C10-C1363 % Cl standard solution (5.4.2) are transferre
40、d into a 2 ml volumetric flask (4.5). 20 l of internal standard solution (5.3) is added and the flask filled up to the volume with n-hexane (5.1).The calibration standard with 59 % chlorine content shall be used for the quantification of all samples, independent of their chlorination degree (if know
41、n).7.2 Extraction of leather0,5 g 0,001 g test leather sample is weighed with the analytical balance (4.1) into the sealable vessel (4.2). 9,9 ml n-hexane (5.1) and 100 l internal standard (5.3) are added and the vessel sealed and extracted at 60 C in an ultrasonic bath (4.3) for 60 min 2 min.1) Che
42、mical Abstracts Service.IULTCS/IUC 30:2015(E)2 ISO 2015 All rights reservedBS EN ISO 18219:2015ISO 18219:2015(E)7.3 Clean upThe SPE cartridges (4.6) are pre-treated with 2 ml n-hexane (5.1) per 100 mg sorbent. The cartridges shall not be dried during or after the pre-treating. The extraction solutio
43、n (7.2) is decanted through the cartridges and the eluate is collected in a new vessel. The cartridge is flushed into the vessel with 5 ml of a 50:50 (v/v) mixture from n-hexane (5.1) and dichloromethane (5.2). This solution is reduced to 1,0 ml under a gentle stream of nitrogen, filtered through a
44、PTFE membrane filter (4.7) and transferred to a GC-MS vial.7.4 GC-MS DeterminationThe solution is analysed using GC-ECNI-MS (4.8). An example of a suitable GC-ECNI-MS method is given in Annex A.8 EvaluationPeak areas from the four quantification masses of the standard are summed up and equated with
45、standard concentration. Peak areas of the samples are summed up too and the concentration is calculated with response of the standard.To check the linearity of the analytical system, a calibration standard as reference standard is analysed after each tenth sample and at the end of the sequence. The
46、deviation in reference to the calibration standard should be within 20 %, otherwise the analytical system has to be checked before retrying the analysis.Sample extract should always be diluted in the concentration range of the standard.The integration of the samples has only to be done in the retent
47、ion time window of the standard.The content of the short-chain chlorinated paraffins in leather is calculated according to Formula (1) as a mass fraction w in mg/kg:wAc VAmAAccSCCP SSCCP StdSCCP StdSStdSS=int.int.int.intt.Std(1)withASCCP-Ssum of the peak areas of SCCP in the sample;ASCCP-Stdsum of t
48、he peak areas of SCCP in the calibration standard;cSCCP-Stdconcentration of SCCP in the calibration standard g/ml;V final volume ml;mSmass of the sample g;Aint .Stdpeak area of internal standard in calibration standard;Aint .Speak area of internal standard in the sample;cint .Sconcentration of inter
49、nal standard in the sample g/ml;cint .Stdconcentration of internal standard in calibration standard g/ml.IULTCS/IUC 30:2015(E) ISO 2015 All rights reserved 3BS EN ISO 18219:2015ISO 18219:2015(E)9 Test reportThe test report shall include at least the following:a) a reference to this International Standard, i.e. ISO 18219;b) all details necessary for complete identification of the sample tested;c) extraction procedure used (7.2);d) amount of extracted SCCP (C10-C13) in mg/kg;e) any deviation by agreement o
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