EN ISO 17072-1-2011 en Leather - Chemical determination of metal content - Part 1 Extractable metals《皮革 化学测定金属含量 第1部分 可提取金属》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 17072-1:2011Leather Chemical determination of metal contentPart 1: Extractable metals (ISO 17072-1:2011)BS EN ISO 17072-1:2011 BRITISH STANDARDNational forewordThis Bri

2、tish Standard is the UK implementation of EN ISO 17072-1:2011.The UK participation 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 doe

3、s not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011 ISBN 978 0 580 66859 3 ICS 59.140.30 Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority

4、of theStandards Policy and Strategy Committee on 28 February 2011. Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17072-1 February 2011 ICS 59.140.30 English Version Leather - Chemical determination of metal content - Part 1: E

5、xtractable metals (ISO 17072-1:2011) Cuir - Dtermination chimique de la teneur en mtal - Partie 1: Mtaux extractibles (ISO 17072-1:2011) Leder - Chemische Bestimmung des Metallgehaltes - Teil 1: Extrahierbare Metalle (ISO 17072-1:2011) This European Standard was approved by CEN on 12 February 2011.

6、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 national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on a

7、pplication to the CEN-CENELEC Management 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

8、 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, N

9、etherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitat

10、ion in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17072-1:2011: EBS EN ISO 17072-1:2011 EN ISO 17072-1:2011 (E) 3 Foreword This document (EN ISO 17072-1:2011) has been prepared by Technical Committee CEN/TC 289 “Leather”, the secretariat of which is held b

11、y UNI, in collaboration with the International Union of Leather Technologists and Chemists Societies. 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 August 2011, and conflicting national standard

12、s shall be withdrawn at the latest by August 2011. 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/CENELEC Intern

13、al 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembo

14、urg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN ISO 17072-1:2011ISO 17072-1:2011(E) IULTCS/IUC 27-1:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Principle

15、.2 4 Reagents 2 5 Apparatus and materials 3 6 Sampling and sample preparation.3 7 Procedure.4 7.1 Preparation of acid artificial-perspiration solution in accordance with ISO 105-E04:2008, Clause 44 7.2 Extraction of leather sample 4 7.3 Digestion of the extracted solution .4 7.4 Analysis by ICP, AAS

16、 and SFA 4 7.4.1 ICP.4 7.4.2 AAS .5 7.4.3 Analysis by SFA technique 5 8 Calculation and expression of results 5 9 Test report6 Annex A (informative) Interlaboratory test results 7 Bibliography8 BS EN ISO 17072-1:2011ISO 17072-1:2011(E) IULTCS/IUC 27-1:2011(E) iv ISO 2011 All rights reservedForeword

17、ISO (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 body interested in a subject for which a technical

18、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 Electrotechnical Commission (IEC) on all matters of elect

19、rotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the

20、member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. 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 ident

21、ifying any or all such patent rights. ISO 17072-1 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with the Chemical Test Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, I

22、ULTCS), in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). This method is technically similar to the method in IUC 27-1. IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to further the advancement of leat

23、her 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 of test methods for leather. ISO 17072 consists of the foll

24、owing parts, under the general title Leather Chemical determination of metal content: Part 1: Extractable metals Part 2: Total metal content BS EN ISO 17072-1:2011INTERNATIONAL STANDARD ISO 17072-1:2011(E)IULTCS/IUC 27-1:2011(E) ISO 2011 All rights reserved 1Leather Chemical determination of metal c

25、ontent Part 1: Extractable metals 1 Scope This part of ISO 17072 specifies a method for the determination of extractable metals in leather using extraction with an acid artificial-perspiration solution and subsequent determination with inductively coupled plasma/optical emission spectrometry (ICP-OE

26、S), or inductively coupled plasma/atomic emission spectrometry (ICP/AES), or inductively coupled plasma/mass spectrometry (ICP/MS), or atomic absorption spectrometry (AAS) or spectrometry of atomic fluorescence (SFA). This method is especially suitable for determining the extractable chromium in chr

27、omium-tanned leathers. This method determines extractable metals in leather; it is not compound-specific or specific to the oxidation state of the metals. The method is also applicable for the determination of many extractable metals, including: Aluminium (Al) Antimony (Sb) Arsenic (As) Barium (Ba)

28、Cadmium (Cd) Calcium (Ca) Chromium (Cr) Cobalt (Co) Copper (Cu) Iron (Fe) Lead (Pb) Magnesium (Mg) Manganese (Mn) Mercury (Hg) Molybdenum (Mo) Nickel (Ni) Potassium (K) Selenium (Se) Tin (Sn) Titanium (Ti) Zinc (Zn) Zirconium (Zr) The quantification limit of extractable lead is 3 mg/kg (see Annex A)

29、. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 105-E04:2008, Textil

30、es Tests for colour fastness Part E04: Colour fastness to perspiration ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location ISO 3696:1987, Water for analytical laboratory use Specification and test methods BS EN ISO 17072-1:2011ISO 17072-1:2011(E) IULTCS/IUC 27-1:

31、2011(E) 2 ISO 2011 All rights reservedISO 4044, Leather Chemical tests Preparation of chemical test samples ISO 4684, Leather Chemical tests Determination of volatile matter ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-O

32、ES) ISO 15586, Water quality Determination of trace metals using atomic absorption spectrometry with graphite furnace ISO 17072-2:2011, Leather Chemical determination of metal content Part 2: Total metal content ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (

33、ICP-MS) Part 2: Determination of 62 elements ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry 3 Principle A sample of leather is ground and extracted at 37 C 2 C for 4 h 5 min in an acid artificial-perspiration solution. The extract solution is filtered

34、, acidified and analysed by ICP, or SFA or AAS. If necessary, digest a portion of filtrate solution in accordance with ISO 17072-2. The results are reported on the dry matter of the leather. If sampling in accordance with ISO 2418 is not possible (e.g. leathers are from finished products like shoes

35、or garments), details about the sampling shall be given together with the test report. 4 Reagents WARNING As concentrated acids are used, it is imperative to use all necessary personal protective equipment. 4.1 General Unless otherwise stated, only analytical grade chemicals shall be used. All solut

36、ions are aqueous solutions. 4.2 Nitric acid, 60 % to 70 % concentration (by mass). 4.3 L-histidine monohydrochloride monohydrate, C6H9O2N3 HClH2O. 4.4 Sodium chloride. 4.5 Sodium dihydrogen orthophosphate dihydrate, NaH2PO42H2O. 4.6 Sodium hydroxide, 0,1 mol/l. 4.7 Element stock solutions, of the va

37、rious metals with mass concentrations of 1 000 mg/l each. 4.8 Nitric acid, 0,1 mol/l. 4.9 Water, grade 3 in accordance with ISO 3696:1987. BS EN ISO 17072-1:2011ISO 17072-1:2011(E) IULTCS/IUC 27-1:2011(E) ISO 2011 All rights reserved 35 Apparatus and materials 5.1 General All glassware, the analytic

38、al devices and the materials, including filters, shall be suitable for analysis of trace metals. Use normal laboratory apparatus and, in particular, the following. 5.2 Laboratory oven, capable of maintaining 102 C 2 C. 5.3 Analytical balance, with an accuracy of 0,1 mg. 5.4 Laboratory balance, with

39、an accuracy of 0,01 g. 5.5 Membrane filters and holder, suitable for filtering aqueous solutions, with a pore size of 0,45 m. 5.6 Filter paper, fast, qualitative type. 5.7 Volumetric flasks, of various sizes (50 ml, 100 ml, 1 000 ml). 5.8 Wide-necked conical flasks, of approximately 250 ml capacity,

40、 with stoppers. 5.9 Volumetric conical flasks, of various sizes. 5.10 Water bath, thermostatically controlled to 37 C 2 C, fitted with a flask shaker or stirrer. 5.11 Inductively coupled plasma/optical emission spectrometer (ICP/OES) or atomic emission spectrometer (ICP/AES) (see ISO 11885), with a

41、hydride-generator module. The gases used shall be of analytical grade. 5.12 Flame or graphite-furnace atomic absorption spectrometer (AAS) (see ISO 15586), with a hydride-generator module and with a suitable hollow-cathode-lamp nitrous oxide burner head or high-solids nitrous oxide burner head. The

42、gases used shall be of analytical grade. 5.13 Inductively coupled plasma/mass spectrometer (ICP/MS) (see ISO 17294-2). The gases used shall be of analytical grade. 5.14 Spectrometer of atomic fluorescence (SFA), for mercury analysis. 6 Sampling and sample preparation 6.1 If the leather piece availab

43、le for testing is a whole hide or skin, then the test specimens shall be sampled in accordance with the standard procedures given in ISO 2418. If sampling in accordance with ISO 2418 is not possible (e.g. leathers are from finished products like shoes or garments), details about the sampling shall b

44、e given in the test report. 6.2 Grind the leather sample in accordance with ISO 4044. Test pieces that are wet (in excess of 30 % moisture) should be predried for at least 12 h, at a temperature not exceeding 50 C 2 C. The drying temperature should be selected while considering the influence of elev

45、ated temperature on the nature of the analyte. 6.3 Using the analytical balance (5.3), weigh accurately 2 g of the ground leather to the nearest 0,001 g and place in a wide-necked 250 ml conical flask (5.8). 6.4 Determine the volatile matter content in accordance with ISO 4684. The same sample of gr

46、ound leather can be used for the extraction in 7.2. BS EN ISO 17072-1:2011ISO 17072-1:2011(E) IULTCS/IUC 27-1:2011(E) 4 ISO 2011 All rights reserved7 Procedure 7.1 Preparation of acid artificial-perspiration solution in accordance with ISO 105-E04:2008, Clause 4 The solution shall be freshly prepare

47、d each day, containing, per litre: 0,5 g of L-histidine monohydrochloride monohydrate (4.3); 5 g of sodium chloride (4.4); 2,2 g of sodium dihydrogen orthophosphate dihydrate (4.5). The solution is brought to pH 5,5 (0,1) with 0,1 mol/l sodium hydroxide solution. 7.2 Extraction of leather sample To

48、the accurately weighed 2 g of ground leather sample (see 6.3) in the conical flask (5.8), add by pipette 100 ml of the acid artificial-perspiration solution (7.1) and, at 37 C 2 C, shake slowly in a water bath (5.10) for 4 h 5 min. Filter the extract with a filter paper (5.6), then filter with a mem

49、brane filter (5.5). For the direct measurement of the elements, take a suitable amount of extract for analysis and add 5 % (by volume) of nitric acid (4.2). Consider this addition in the dilution factor. To control the contaminants, it will be necessary to carry out a blank procedure. An aliquot of acid perspiration is placed in a sample container and treated as a sample, in all respects, including all analytical procedures. The above extraction conditions shall be followed