EN ISO 17072-2-2011 en Leather - Chemical determination of metal content - Part 2 Total metal content《皮革 金属含量的化学测定 总金属含量》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 17072-2:2011Leather Chemical determination of metal contentPart 2: Total metal content (ISO 17072-2:2011)BS EN ISO 17072-2:2011 BRITISH STANDARDNational forewordThis Br

2、itish Standard is the UK implementation of EN ISO 17072-2:2011.The UK participation in its preparation was entrusted to Technical 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

3、does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. BSI 2011 ISBN 978 0 580 66860 9 ICS 59.140.30 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the auth

4、ority of the Standards Policy and Strategy Committee on 31 March 2011.Amendments issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17072-2 February 2011 ICS 59.140.30 English Version Leather - Chemical determination of metal content - Part 2

5、: Total metal content (ISO 17072-2:2011) Cuir - Dtermination chimique de la teneur en mtal - Partie 2: Teneur totale en mtaux (ISO 17072-2:2011) Leder - Chemische Bestimmung des Metallgehaltes - Teil 2: Gesamtmetallgehalt (ISO 17072-2:2011) This European Standard was approved by CEN on 12 February 2

6、011. 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

7、 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 version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CE

8、NELEC 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, Mal

9、ta, Netherlands, 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 expl

10、oitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17072-2:2011: EBS EN ISO 17072-2:2011 EN ISO 17072-2:2011 (E) 3 Foreword This document (EN ISO 17072-2:2011) has been prepared by Technical Committee CEN/TC 289 “Leather”, the secretariat of which is h

11、eld by 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 sta

12、ndards 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 I

13、nternal 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, Lu

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

15、iple .2 4 Reagents 2 5 Apparatus and materials 2 6 Sampling and sample preparation.3 7 Instrumental procedure 4 7.1 Analysis by ICP, AAS and SFA 4 7.1.1 ICP.4 7.1.2 AAS .4 7.2 Analysis by hydride technique 5 7.3 Analysis by SFA technique 5 8 Calculation and expression of results 5 9 Test report5 Ann

16、ex A (informative) Interlaboratory test results 6 Bibliography7 BS EN ISO 17072-2:2011ISO 17072-2:2011(E) IULTCS/IUC 27-2:2011(E) iv ISO 2011 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies

17、). 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, governmental and no

18、n-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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Par

19、t 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting

20、 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 identifying any or all such patent rights. ISO 17072-2 was prepared by the European Committee for Standardization (CEN) Technical Commi

21、ttee CEN/TC 289, Leather, in collaboration with the Chemical Test Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, IULTCS), in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). This method is technical

22、ly similar to the method in IUC 27-2. 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 sam

23、pling 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 following parts, under the general title Leather Chemical determination of metal content: Part 1: Extractable metals Part 2: Total met

24、al content BS EN ISO 17072-2:2011INTERNATIONAL STANDARD ISO 17072-2:2011(E)IULTCS/IUC 27-2:2011(E) ISO 2011 All rights reserved 1Leather Chemical determination of metal content Part 2: Total metal content 1 Scope This part of ISO 17072 specifies a method for the determination of the total metal cont

25、ent in leather using digestion of the leather and subsequent determination with inductively coupled plasma/optical emission spectrometry (ICP/OES), or inductively coupled plasma/mass spectrometry (ICP/MS), or atomic absorption spectrometry (AAS) or spectrometry of atomic fluorescence (SFA). This met

26、hod determines the total metal content in leather; it is not compound-specific or specific to the oxidation state of the metals. The method is applicable for determining the following metals: Aluminium (Al) Copper (Cu) Potassium (K) Antimony (Sb) Iron (Fe) Selenium (Se) Arsenic (As) Lead (Pb) Silico

27、n (Si) Barium (Ba) Magnesium (Mg) Sodium (Na) Cadmium (Cd) Manganese (Mn) Tin (Sn) Calcium (Ca) Mercury (Hg) Titanium (Ti) Chromium (Cr) (except chromium-tanned leathers) Molybdenum (Mo) Zinc (Zn) Cobalt (Co) Nickel (Ni) Zirconium (Zr) The quantification limit of total lead is 8 mg/kg (see Annex A).

28、 This part of ISO 17072 is not applicable to chromium-tanned leathers. In this case, ISO 5398-1, or ISO 5398-2, or ISO 5398-3, or ISO 5398-4 are used. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edit

29、ion 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 location ISO 3696:1987, Water for analytical laboratory use Specification and test methods BS E

30、N ISO 17072-2:2011ISO 17072-2:2011(E) IULTCS/IUC 27-2:2011(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 inductive

31、ly coupled plasma optical emission spectrometry (ICP-OES) ISO 15586, Water quality Determination of trace metals using atomic absorption spectrometry with graphite furnace ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elem

32、ents ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry EN 14602, Footwear Test methods for the assessment of ecological criteria 3 Principle Digestion of the sample of ground leather (see ISO 4044) is carried out using a ternary acid mixture or microwave

33、 digestion until complete mineralization is achieved. The residue is redissolved with water and analysed by AAS or ICP. 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 or garments)

34、, 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 solutions are aqu

35、eous solutions. 4.2 Nitric acid, 60 % to 70 % concentration (by mass). 4.3 Sulfuric acid (H2SO4), 98 % concentration (by mass). 4.4 Perchloric acid, 60 % to 70 % concentration (by mass). 4.5 Element stock solutions, of the various metals with mass concentrations of 1 000 mg/l each. 4.6 Hydrochloric

36、acid (HCl), 37 %. 4.7 Water, grade 3 in accordance with ISO 3696:1987. 5 Apparatus and materials 5.1 General All glassware, the analytical devices and the materials, including filters, shall be suitable for analysis of trace metals. BS EN ISO 17072-2:2011ISO 17072-2:2011(E) IULTCS/IUC 27-2:2011(E) I

37、SO 2011 All rights reserved 3Use 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 Heating apparatus for Kjeldahl flasks, equipped with fume extraction. 5.5 Long-necked Kjeldah

38、l digestion flask, 1 l volume, with reflux condenser. 5.6 Membrane filters and holders, suitable for filtering aqueous solutions, with a pore size of 0,45 m. 5.7 Vacuum filter system for membrane filters. 5.8 Magnetic stirrer. 5.9 Glass boiling beads. 5.10 Inductively coupled plasma/optical emission

39、 spectrometer (ICP/OES) (see ISO 11885), with hydride-generator module. The gases used shall be of analytical grade. 5.11 Flame or graphite-furnace atomic absorption spectrometer (AAS) (see ISO 15586), with hydride-generator module and with a suitable hollow-cathode-lamp nitrous oxide burner head or

40、 high-solids nitrous oxide burner head. The gases used shall be of analytical grade. 5.12 Inductively coupled plasma/mass spectrometer (ICP/MS) (see ISO 17294-2). The gases used shall be of analytical grade. 5.13 Spectrometer of atomic fluorescence (SFA), for mercury analysis. 6 Sampling and sample

41、preparation 6.1 If the leather piece available 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 g

42、arments), details about the sampling shall be 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 sele

43、cted while considering the influence of elevated temperature on the nature of the analyte. 6.3 Determine the dry matter content in accordance with ISO 4684. The same sample of ground leather can be used for the digestion in 6.5. 6.4 Using the analytical balance (5.3), weigh accurately 1 g of the gro

44、und leather to the nearest 0,001 g and place in a long-necked Kjeldahl digestion flask (5.5). 6.5 Prepare the sample using the digestion method for the determination of Al, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Na, Ni, Pb, Si, Sn, Ti, Zn, Zr, As, Se, Sb, Hg. If using acid digestion (6.5.1) for

45、Pb detection, the digestion procedure shall be carried out separately, replacing H2SO4with HCl. 6.5.1 Acid digestion WARNING It is imperative that the leather sample is not in direct contact with perchloric acid because of the possible explosive reaction. BS EN ISO 17072-2:2011ISO 17072-2:2011(E) IU

46、LTCS/IUC 27-2:2011(E) 4 ISO 2011 All rights reservedPlace the ground leather sample in the Kjeldahl flask (5.5), add, using a measuring cylinder, 10 ml to 20 ml of a ternary mixture of nitric acid (4.2), sulfuric acid (4.3) and perchloric acid (4.4) in a ratio of 3:1:1, and a few glass boiling beads

47、 (5.9). Place a funnel or splash bulb in the neck of the flask and heat to boiling on a wire gauze over a moderate flame. Leave to react on the heating apparatus (5.4) until digestion is complete and the red vapours of nitrogen dioxide have disappeared. In the event of incomplete digestion, allow th

48、e flask to cool, add a further 10 ml to 20 ml of the ternary mixture and repeat the procedure. Allow to cool, redissolve with 30 ml of distilled water, filter if necessary, then transfer the filtrate to a 100 ml volumetric flask. With 30 ml of distilled water, thoroughly wash the flask used for dige

49、stion and the filter, transfer the water to the volumetric flask, and make up to volume. To control the contaminants, it will be necessary to carry out a blank procedure. An aliquot of the mixture of acids is placed in a sample container and treated as a sample in all respects, including all analytical procedures. 6.5.2 Microwave digestion The sample for analysis can also be prepared through application of microwave-assisted digestion (MAD). If this is used, then a suitable procedure such as that describ