DIN EN ISO 17072-2-2011 Leather - Chemical determination of metal content - Part 2 Total metal content (ISO 17072-2 2011) German version EN ISO 17072-2 2011《皮革 金属含量的化学测定 第2部分 总金属含量.pdf

1、June 2011 Translation by DIN-Sprachendienst.English price group 9No 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

2、.140.30!$qIP“1783845www.din.deDDIN EN ISO 17072-2Leather Chemical determination of metal content Part 2: Total metal content (ISO 17072-2:2011)English translation of DIN EN ISO 17072-2:2011-06Leder Chemische Bestimmung des Metallgehaltes Teil 2: Gesamtmetallgehalt (ISO 17072-2:2011)Englische bersetz

3、ung von DIN EN ISO 17072-2:2011-06Cuir Dtermination chimique de la teneur en mtal Partie 2: Teneur totale en mtaux (ISO 17072-2:2011)Traduction anglaise de DIN EN ISO 17072-2:2011-06www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.1

4、404.11 DIN EN ISO 17072-2:2011-05 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 289 “Leather” (Secretariat: UNI, Italy) in collaboration with IULTCS, the International Union of Leather Technologists and Chemists Societies. The

5、responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-52 AA Chemische Prfverfahren fr Leder. This document is based on the method specified in IUC 27-2 of IULTCS. DIN EN ISO 17072 consists of th

6、e following parts, under the general title Leather Chemical determination of metal content: Part 1: Extractable metals Part 2: Total metal content The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 2418 DIN EN ISO 2418 ISO 3696 DIN ISO 369

7、6 ISO 4044 DIN EN ISO 4044 ISO 4684, DIN EN ISO 4684 ISO 5398-1 DIN EN ISO 5398-1 ISO 5398-2 DIN EN ISO 5398-2 ISO 5398-3 DIN EN ISO 5398-3 ISO 5398-4 DIN EN ISO 5398-4 ISO 5725-2 DIN ISO 5725-2 ISO 5725-5 DIN ISO 5725-5 ISO 11885 DIN EN ISO 11885 ISO 15586 DIN EN ISO 15586 ISO 17294-2 DIN EN ISO 17

8、294-2 ISO 17852 DIN EN ISO 17852 2 DIN EN ISO 17072-2:2011-05 National Annex NA (informative) Bibliography DIN EN ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location DIN EN ISO 4044, Leather Chemical tests Preparation of chemical test samples DIN EN ISO 4684, Lea

9、ther Chemical tests Determination of volatile matter DIN EN ISO 5398-1, Leather Chemical determination of chromic oxide content Part 1: Quantification by titration DIN EN ISO 5398-2, Leather Chemical determination of chromic oxide content Part 2: Quantification by colorimetric determination DIN EN I

10、SO 5398-3, Leather Chemical determination of chromic oxide content Part 3: Quantification by atomic absorption spectrometry DIN EN ISO 5398-4, Leather Chemical determination of chromic oxide content Part 4: Quantification by inductively coupled plasma optical emission spectrometer (ICP-OES) DIN EN I

11、SO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) DIN EN ISO 15586, Water quality Determination of trace elements using atomic absorption spectrometry with graphite furnace DIN EN ISO 17294-2, Water quality Application of

12、 inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elements DIN EN ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-2, Accuracy

13、 (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the deter

14、mination of the precision of a standard measurement method 3 DIN EN ISO 17072-2:2011-05 4 This page is intentionally blank EUROPEAN 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: Total metal

15、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 2011. CEN members are b

16、ound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard 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

17、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 Management Centre

18、 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, Netherlands, Norway

19、, 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 exploitation in any form and

20、 by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17072-2:2011: EContents Page Foreword 31 Scope4 2 Normative references4 3 Principle .5 4 Reagents 5 5 Apparatus and materials 5 6 Sampling and sample preparation.6 7 Instrumental procedure 7 7.1 Analysis by ICP, AAS and SFA 7

21、 7.1.1 ICP.7 7.1.2 AAS .7 7.2 Analysis by hydride technique 7 7.3 Analysis by SFA technique 7 8 Calculation and expression of results 8 9 Test report8 Annex A (informative) Interlaboratory test results 9 Bibliography10 EN ISO 17072-2:2011 (E) DIN EN ISO 17072-2:2011-05 2Foreword This document (EN IS

22、O 17072-2:2011) has been prepared by Technical Committee CEN/TC 289 “Leather”, the secretariat of which is held 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 pu

23、blication of an identical text or by endorsement, at the latest by August 2011, and conflicting national standards 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

24、 shall not be held responsible for identifying any or all such patent rights. According to the 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,

25、 Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. EN ISO 17072-2:2011 (E) DIN EN ISO 17072-2:2011-05 31 Sc

26、ope This part of ISO 17072 specifies a method for the determination of the total metal content 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

27、atomic absorption spectrometry (AAS) or spectrometry of atomic fluorescence (SFA). This method 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) Co

28、pper (Cu) Potassium (K) Antimony (Sb) Iron (Fe) Selenium (Se) Arsenic (As) Lead (Pb) Silicon (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)

29、Nickel (Ni) Zirconium (Zr) The quantification limit of total lead is 8 mg/kg (see Annex A). 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

30、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 2418, Leather Chemical, physical and mechanical and fastness tests Sampling loca

31、tion ISO 3696:1987, Water for analytical laboratory use Specification and test methods ISO 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 co

32、upled 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 elements

33、ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry EN 14602, Footwear Test methods for the assessment of ecological criteria EN ISO 17072-2:2011 (E) DIN EN ISO 17072-2:2011-05 43 Principle Digestion of the sample of ground leather (see ISO 4044) is carrie

34、d out using a ternary acid mixture or microwave 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

35、 from finished products like shoes 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

36、 chemicals shall be used. All solutions are aqueous 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 conce

37、ntrations of 1 000 mg/l each. 4.6 Hydrochloric 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. Use normal laborator

38、y 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 Kjeldahl digestion flask, 1 l volume, with reflux conden

39、ser. 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. EN ISO 17072-2:2011 (E) DIN EN ISO 17072-2:2011-05 55.10 Inductively coupled plasma/optical emiss

40、ion 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

41、 or 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 samp

42、le 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 o

43、r garments), 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 s

44、elected 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

45、ground 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) f

46、or 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. Place the ground leather sample in the Kj

47、eldahl 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 (5.9). Place a funnel or splash bulb in the neck of the flask and heat to boiling on a wire

48、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 the 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 volumet