1、BSI Standards PublicationBS EN ISO 19070:2016Leather Chemicaldetermination of N-methyl-2-pyrrolidone (NMP) in leatherBS EN ISO 19070:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 19070:2016.The UK participation in its preparation was entrusted to Tech
2、nical 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. T
3、he British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 83034 1 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 on
4、 30 April 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 19070 April 2016 ICS 59.140.30 English Version Leather - Chemical determination of N-methyl-2-pyrrolidone (NMP) in leather (ISO 19070:2016) Cuir - Dtermin
5、ation de la teneur en N-mthyl-2-pyrrolidone (NMP) dans le cuir (ISO 19070:2016) Leder - Chemische Bestimmung von N-methyl-2-pyrrolidon (NMP) in Leder (ISO 19070:2016) This European Standard was approved by CEN on 13 February 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulat
6、ions 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.
7、 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
8、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, Po
9、rtugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any
10、form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 19070:2016 EBS EN ISO 19070:2016EN ISO 19070:2016 (E) 3 European foreword This document (EN ISO 19070:2016) has been prepared by Technical Committee IULTCS “International Union of Leather Technologists and Chemists So
11、cieties“ 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 October 2016, and conflicting natio
12、nal standards shall be withdrawn at the latest by October 2016. 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-C
13、ENELEC 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,
14、 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 19070:2016 has been approved by CEN as EN ISO 19070:2016 without any modif
15、ication. BS EN ISO 19070:2016ISO 19070:2016(E)IULTCS/IUC 34:2016(E)Foreword ivIntroduction v1 Scope . 12 Normative references 13 Principle 14 Reagents 15 Apparatus . 16 Procedure. 26.1 Preparation of standard solutions . 26.1.1 NMP stock solution (1 000 g/ml) . 26.1.2 NMP Calibration solution . 26.2
16、 Sample preparation 26.3 Extraction procedure . 27 Chromatographic determination 28 Quantification 39 Performance of the method 310 Test report . 3Annex A (informative) Chromatographic analysis . 4 ISO 2016 All rights reserved iiiContents PageBS EN ISO 19070:2016ISO 19070:2016(E)ForewordISO (the Int
17、ernational 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 ha
18、s 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
19、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 acc
20、ordance 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. Detai
21、ls 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 end
22、orsement.For an explanation on the meaning of ISO specific terms 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 19070 was prepa
23、red by the Chemical Testing 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 accor
24、dance with the Agreement on technical cooperation 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
25、 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.IULTCS/IUC 34:2016(E)iv ISO 2016 All rights reservedBS EN ISO 19070:2016ISO 19070:2016(E)IntroductionUnder the
26、 REACH regulation in the European Union (EU Regulation 1907/2006), N-methyl-2-pyrrolidone has been included in the candidate list of substances of very high concern (SVHC) and its use is restricted.Accordingly, a new method is given for the determination of N-methyl-2-pyrrolidone in leather.IULTCS/I
27、UC 34:2016(E) ISO 2016 All rights reserved vBS EN ISO 19070:2016BS EN ISO 19070:2016Leather Chemical determination of N-methyl-2-pyrrolidone (NMP) in leather1 ScopeThis International Standard specifies a method to determine the amount of N-methyl-2-pyrrolidone (NMP) in leather and leather components
28、.This method may also be used for the determination of N-ethyl-2-pyrrolidone (NEP) 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 applie
29、s. 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 PrincipleThe test sample is extra
30、cted using acetone at 50 C in an ultrasonic bath for 1 h. An aliquot is then analysed using a gas chromatograph with a mass selective detector (GC-MS).4 ReagentsAll reagents shall be analytical grade.4.1 Acetone, CAS1)No. 67-64-1.4.2 N-methyl-2-pyrrolidone, at least 99,5 %, CAS No. 872-50-4.5 Appara
31、tusUsual laboratory equipment and, in particular, the following.5.1 Analytical balance, capable of reading to 0,000 1 g.5.2 Sealable jar, approximately 20 ml, with lid (suitable for carrying out an acetone extraction at 50 C).5.3 Ultrasonic bath (temperature controlled).5.4 Micro-pipettes, 50 l and
32、100 l.5.5 Pipettes, 0,5 ml to 5 ml capacity.5.6 Volumetric flasks, 100 ml.1) CAS = Chemical Abstracts ServiceINTERNATIONAL STANDARDISO 19070:2016(E)IULTCS/IUC 34:2016(E) ISO 2016 All rights reserved 1BS EN ISO 19070:2016ISO 19070:2016(E)5.7 Gas chromatograph, with mass selective detector (GC-MS).5.8
33、 PTFE-membrane filter, pore size 0,45 m.5.9 Sample vials, PTFE seal.6 Procedure6.1 Preparation of standard solutions6.1.1 NMP stock solution (1 000 g/ml)Weigh accurately 0,1 g of N-methyl-2-pyrrolidone using the analytical balance (5.1), into a 100 ml volumetric flask (5.6) and fill up to the mark w
34、ith acetone (4.1).6.1.2 NMP Calibration solutionFour calibration solutions are used to establish the calibration curve. They are all prepared in 100 ml volumetric flasks, as specified in Table 1.Table 1 Preparation of calibration solutionsCalibration solution Volume of the NMP stock solution (6.1.1)
35、Concentration of NMP in the calibration solution1 0,1 ml 1 g/ml2 0,5 ml 5 g/ml3 1 ml 10 g/ml4 5 ml 50 g/mlFilled up to the mark with acetone6.2 Sample preparationTake a representative sample from the leather or leather component. When possible sample according to ISO 2418.The leather specimen shall
36、be cut into pieces in accordance with ISO 4044. The dimensions of the pieces shall not be larger than 2 mm to 3 mm. Do not condition the sample.6.3 Extraction procedureWeigh accurately approximately 1 g of the leather pieces with the analytical balance (5.1) and place them into the sealable jar (5.2
37、). Add 10 ml of acetone and extract the leather at (50 2) C in an ultrasonic bath for (1,0 0,1) h.After cooling to room temperature, filter the solution through a PTFE membrane filter (5.8) and transfer to a vial (5.9), and seal with a PTFE cap. This solution is now ready for instrumental analysis,
38、which shall be performed within 24 h.If there is to be any delay in analysing the prepared sample then it may be stored at (4 2) C for up to 24 h.7 Chromatographic determinationThe detection of the N-methyl-2-pyrrolidone may be performed using the GC-MS chromatographic technique given in Annex A.IUL
39、TCS/IUC 34:2016(E)2 ISO 2016 All rights reservedBS EN ISO 19070:2016ISO 19070:2016(E)If the amount of NMP in the sample is above the highest calibration point, a dilution step is necessary, which has to be considered in the calculation in Clause 8.8 QuantificationThe content of N-methyl-2-pyrrolidon
40、e is calculated as a mass fraction, w, in mg/kg, according to Formula (1):wAC VAm=NMP-SNMP-StdNMP-StdS(1)whereANMP-Sis the peak area of NMP in the sample;ANMP-Stdis the peak area of NMP in the calibration standard;CNMP-Stdis the concentration of NMP in the calibration standard, in g/ml;V is the fina
41、l volume of sample, in ml, (V = 10 ml according to 6.3);mSis the mass of the sample as received, in g.9 Performance of the methodThe quantification limit shall be sufficient to ensure the analysis complies with any specification or legislative framework requirements, for example less than 1 000 mg/k
42、g for N-methyl-2-pyrrolidone in the leather. The typical limit of quantification for this method is 5 mg/kg.10 Test reportThe test report shall include at least the following:a) a reference to this International Standard, i.e. ISO 19070;b) the date of the test;c) all details necessary for complete i
43、dentification of the sample tested;d) the amount of N-methyl-2-pyrrolidone determined in the leather sample, in mg/kg;e) the limit of detection for this method;f) any deviation from the analytical procedure specified in this International Standard.IULTCS/IUC 34:2016(E) ISO 2016 All rights reserved 3
44、BS EN ISO 19070:2016ISO 19070:2016(E)Annex A (informative) Chromatographic analysisA.1 Preliminary remarkAs the instrumental equipment (5.7) of the laboratories may vary, no generally applicable instructions can be provided for chromatographic analyses. The following procedures have been tested and
45、used.A.2 Gas chromatography with mass selective detector (GC-MS)Column: 5 % phenyl 95 % dimethylpolysiloxane, 30 m 0,25 mm 0,25 mCarrier gas: helium; flow 1,2 ml/minInjection system: splitlessInjector temperature: 250 CInjection volume: 1 lTemperature programme: 60 C at 4 min, 15 C/min to 140 C and
46、30 C/min to 300 C for 1 minTransfer line temperature: 300 CSource Temperature: 230 CQuadrupole Temperature: 150 CMS-Detection (SIM/SCAN Mode): SCAN: m/z 60110; SIM: m/z 99IULTCS/IUC 34:2016(E)4 ISO 2016 All rights reservedBS EN ISO 19070:2016This page deliberately left blankThis page deliberately le
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