1、English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 59.140.30!%XL?“2534128www.din.deDIN EN ISO 190
2、70Leather Chemical determination of N-methyl-2-pyrrolidone (NMP) in leather (ISO 19070:2016);English version EN ISO 19070:2016,English translation of DIN EN ISO 19070:2016-07Leder Chemische Bestimmung von N-methyl-2-pyrrolidon (NMP) in Leder (ISO 19070:2016);Englische Fassung EN ISO 19070:2016,Engli
3、sche bersetzung von DIN EN ISO 19070:2016-07Cuir Dtermination de la teneur en N-mthyl-2-pyrrolidone (NMP) dans le cuir (ISO 19070:2016);Version anglaise EN ISO 19070:2016,Traduction anglaise de DIN EN ISO 19070:2016-07www.beuth.deDocument comprises 11 pagesDTranslation by DIN-Sprachendienst.In case
4、of doubt, the German-language original shall be considered authoritative.July 201607.16DIN EN ISO 19070:2016-07 2 A comma is used as the decimal marker. National foreword This document (EN ISO 19070:2016) has been prepared by Technical Committee IULTCS “International Union of Leather Technologists a
5、nd Chemists Societies” in collaboration with Technical Committee CEN/TC 289 “Leather” (Secretariat: UNI, Italy). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-52 AA Chemische Prf
6、verfahren fr Leder. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 2418 DIN EN ISO 2418 ISO 4044 DIN EN ISO 4044 National Annex NA (informative) Bibliography DIN EN ISO 2418, Leather Chemical, physical and mechanical and fastness tests
7、 Sampling location DIN EN ISO 4044, Leather Chemical tests Preparation of chemical test samples EUROPEAN 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 Dter
8、mination 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 Regula
9、tions 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
10、. 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
11、 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, P
12、ortugal, 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 2016 CEN All rights of exploitation in an
13、y form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 19070:2016 E EN ISO 19070:2016 (E) Contents Page 2European foreword . 3 Foreword 4 Introduction 5 1 Scope 6 2 Normative references 6 3 Principle . 6 4 Reagents . 6 5 Apparatus . 6 6 Procedure. 7 6.1 Preparation of s
14、tandard solutions 7 6.1.1 NMP stock solution (1 000 g/ml) 7 6.1.2 NMP Calibration solution . 7 6.2 Sample preparation 7 6.3 Extraction procedure . 7 7 Chromatographic determination 7 8 Quantification . 8 9 Performance of the method . 8 10 Test report . 8 Annex A (informative) Chromatographic analysi
15、s . 9 A.1 Preliminary remark . 9 A.2 Gas chromatography with mass selective detector (GC-MS) . 9 DIN EN ISO 19070:2016-07 EN ISO 19070:2016 (E) European foreword This document (EN ISO 19070:2016) has been prepared by Technical Committee IULTCS “International Union of Leather Technologists and Chemis
16、ts Societies” 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
17、national 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
18、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, Hun
19、gary, 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
20、modification. 3DIN EN ISO 19070:2016-07 ForewordISO (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 bod
21、y 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 Electrote
22、chnical 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
23、 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 resp
24、onsible 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
25、 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 the WTO principles in the Technical Barriers to Trade (TBT) see the following
26、URL: Foreword - Supplementary informationISO 19070 was prepared 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
27、, Leather, the secretariat of which is held by UNI, in accordance 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 tec
28、hnology. 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.EN ISO 19070:2016 (E) 4DIN EN ISO 19070:2016-07 In
29、troductionUnder the 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
30、in leather.EN ISO 19070:2016 (E) 5DIN EN ISO 19070:2016-07 1 ScopeThis International Standard specifies a method to determine the amount of N-methyl-2-pyrrolidone (NMP) in leather and leather components.This method may also be used for the determination of N-ethyl-2-pyrrolidone (NEP) in leather.2 No
31、rmative 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 undated references, the latest edition of the referenced document (including any amendments
32、) 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 extracted using acetone at 50 C in an ultrasonic bath for 1 h. An aliquot is then analysed using a gas
33、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 ApparatusUsual laboratory equipment and, in particular, the following.5.1 Analytical balance, capable of
34、 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 100 l.5.5 Pipettes, 0,5 ml to 5 ml capacity.5.6 Volumetric flasks, 100 ml.1) CAS = Chemical Abstra
35、cts ServiceEN ISO 19070:2016 (E) 6DIN EN ISO 19070:2016-07 5.7 Gas chromatograph, with mass selective detector (GC-MS).5.8 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
36、 N-methyl-2-pyrrolidone using the analytical balance (5.1), into a 100 ml volumetric flask (5.6) and fill up to the mark with 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 spec
37、ified in Table 1.Table 1 Preparation of calibration solutionsCalibration solution Volume of the NMP stock solution (6.1.1)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 represent
38、ative sample from the leather or leather component. When possible sample according to ISO 2418.The leather specimen shall 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 accu
39、rately approximately 1 g of the leather pieces with the analytical balance (5.1) and place them into the sealable jar (5.2). 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 f
40、ilter (5.8) and transfer to a vial (5.9), and seal with a PTFE cap. This solution is now ready for instrumental analysis, 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 determinationT
41、he detection of the N-methyl-2-pyrrolidone may be performed using the GC-MS chromatographic technique given in Annex A.EN ISO 19070:2016 (E) 7DIN EN ISO 19070:2016-07 If the amount of NMP in the sample is above the highest calibration point, a dilution step is necessary, which has to be considered i
42、n the calculation in Clause 8.8 QuantificationThe content of N-methyl-2-pyrrolidone 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
43、-Stdis the concentration of NMP in the calibration standard, in g/ml;V is the final 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 spe
44、cification or legislative framework requirements, for example less than 1 000 mg/kg 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 Standa
45、rd, i.e. ISO 19070;b) the date of the test;c) all details necessary for complete identification 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 i
46、n this International Standard.EN ISO 19070:2016 (E) 8DIN EN ISO 19070:2016-07 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 f
47、ollowing procedures have been tested and 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 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 99EN ISO 19070:2016 (E) 9DIN EN ISO 19070:2016-07
