1、June 2011 Translation by DIN-Sprachendienst.English price group 10No 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 5
2、9.140.30!$qIQ“1783846www.din.deDDIN EN ISO 17072-1Leather Chemical determination of metal content Part 1: Extractable metals (ISO 17072-1:2011)English translation of DIN EN ISO 17072-1:2011-06Leder Chemische Bestimmung des Metallgehaltes Teil 1: Extrahierbare Metalle (ISO 17072-1:2011)Englische bers
3、etzung von DIN EN ISO 17072-1:2011-06Cuir Dtermination chimique de la teneur en mtal Partie 1: Mtaux extractibles (ISO 17072-1:2011)Traduction anglaise de DIN EN ISO 17072-1:2011-06www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.15
4、04.11 DIN EN ISO 17072-1:2011-05 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 r
5、esponsible 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 27-1 of IULTCS. DIN EN ISO 17072 consists of the
6、 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 105-E04 DIN EN ISO 105-E04 ISO 2418 DIN EN
7、 ISO 2418 ISO 3696 DIN ISO 3696 ISO 4044 DIN EN ISO 4044 ISO 4684 DIN EN ISO 4684 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 17072-2 DIN EN ISO 17072-2 ISO 17294-2 DIN EN ISO 17294-2 ISO 17852 DIN EN ISO 17852 2 DIN EN ISO 147072-1:2
8、011-05 National Annex NA (informative) Bibliography DIN EN ISO 105-E04, Textiles Tests for colour fastness Part E04: Colour fastness to perspiration DIN EN ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location DIN EN ISO 4044, Leather Chemical tests Preparation of
9、chemical test samples DIN EN ISO 4684, Leather Chemical tests Determination of volatile matter DIN EN ISO 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 usin
10、g atomic absorption spectrometry with graphite furnace DIN EN ISO 17072-2, Leather Chemical determination of metal content Part 2: Total metal content DIN EN ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elements DIN EN IS
11、O 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 (trueness and precision) of measurement methods and results Part 2: Basic method for the determinati
12、on 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 determination of the precision of a standard measurement method 3 DIN EN ISO 17072-1:2011-05 4 This page i
13、s intentionally blank EUROPEAN 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: Extractable metals (ISO 17072-1:2011) Cuir Dtermination chimique de la teneur en mtal Partie 1: Mtaux extractible
14、s (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. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
15、 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 CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official ver
16、sions (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 members are the national standards bodies of Austria
17、, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, 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 United Kingdom. EUROPEAN
18、 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 by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17072-1:2011: EContents Page
19、 Foreword 31 Scope4 2 Normative references4 3 Principle .5 4 Reagents 5 5 Apparatus and materials 6 6 Sampling and sample preparation.6 7 Procedure.7 7.1 Preparation of acid artificial-perspiration solution in accordance with ISO 105-E04:2008, Clause 47 7.2 Extraction of leather sample 7 7.3 Digesti
20、on of the extracted solution .7 7.4 Analysis by ICP, AAS and SFA 7 7.4.1 ICP.7 7.4.2 AAS .8 7.4.3 Analysis by SFA technique 8 8 Calculation and expression of results 8 9 Test report9 Annex A (informative) Interlaboratory test results 10 Bibliography11 2EN ISO 17072-1:2011 (E) DIN EN ISO 17072-1:2011
21、-05 Foreword This document (EN ISO 17072-1:2011) 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
22、a national standard, either by publication 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
23、patent rights. CEN and/or CENELEC 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,
24、 Croatia, Cyprus, Czech Republic, 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. 3EN ISO 17072-1:2011 (E
25、) DIN EN ISO 17072-1:2011-05 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-OES), o
26、r 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 chromium
27、-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) Cadmi
28、um (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). 2 N
29、ormative 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, Textiles Te
30、sts 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 ISO 4044, Leather Chemical tests Preparation of chemical test s
31、amples 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-OES) ISO 15586, Water quality Determination of trace metals using atomic absorption spectrometry with
32、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 (ICP-MS) Part 2: Determination of 62 elements ISO 17852, Water quality Determination of mercury Method
33、 using atomic fluorescence spectrometry 4EN ISO 17072-1:2011 (E) DIN EN ISO 17072-1:2011-05 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, acidified and analysed by ICP, or SFA or AAS. I
34、f 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 or garments), details about the sampling shall be
35、 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 aqueous solutions. 4.2 Nitric acid, 60 %
36、 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 various metals with mass concentrations of 1 000 mg
37、/l each. 4.8 Nitric acid, 0,1 mol/l. 4.9 Water, grade 3 in accordance with ISO 3696:1987. 5EN ISO 17072-1:2011 (E) DIN EN ISO 17072-1:2011-05 5 Apparatus and materials 5.1 General All glassware, the analytical devices and the materials, including filters, shall be suitable for analysis of trace meta
38、ls. 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 an accuracy of 0,01 g. 5.5 Membrane filters and holder, suitable for filtering aqueous soluti
39、ons, 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, with stoppers. 5.9 Volumetric conical flasks, of various sizes. 5.10 Water bath, thermostati
40、cally 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 hydride-generator module. The gases used shall be of analytical grade. 5.12 Flame or graphite
41、-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 gases used shall be of analytical grade. 5.13 Inductively coupled plasma/mass spectrometer (I
42、CP/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 available for testing is a whole hide or skin, then the test specimens shall be sampled in accordanc
43、e 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 be given in the test report. 6.2 Grind the leather sample in accordance with ISO 4044. Test pi
44、eces 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 elevated temperature on the nature of the analyte. 6.3 Using the analytical balance (5.3), weigh
45、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 ground leather can be used for the extraction in 7.2. 6EN ISO 17072-1:2011 (E) DIN EN ISO 17072
46、-1:2011-05 7 Procedure 7.1 Preparation of acid artificial-perspiration solution in accordance with ISO 105-E04:2008, Clause 4 The solution shall be freshly prepared 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 sodiu
47、m 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 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-pe
48、rspiration 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 membrane 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
