1、BRITISH STANDARDBS EN ISO 5398-4:2007Leather Chemical determination of chromic oxide content Part 4: Quantification by inductively coupled plasma-optical emission spectrometer (ICP-OES)The European Standard EN ISO 5398-4:2007 has the status of a British StandardICS 59.140.30g49g50g3g38g50g51g60g44g4
2、9g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 5398-4:2007This British Standard was published under the authority of the Standards Policy and Strategy Committee o
3、n 31 December 2007 BSI 2007ISBN 978 0 580 55577 0National forewordThis British Standard is the UK implementation of EN ISO 5398-4:2007.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
4、 committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since p
5、ublicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 5398-4August 2007ICS 59.140.30English VersionLeather - Chemical determination of chromic oxide content - Part4: Quantification by inductively coupled plasma - opticalemission spectrometer (ICP-OES) (ISO 5398-4:2007
6、)Cuir - Dosage chimique de loxyde de chrome - Partie 4:Quantification par plasma couplage inductif -spectromtre dmission optique (ICP-OES) (ISO 5398-4:2007)Leder - Chemische Bestimmung des Chromoxidgehaltes -Teil 4: Bestimmung durch induktiv gekoppeltesPlasma/optisches Spektrometer (ICP-OES) (ISO 53
7、98-4:2007)This European Standard was approved by CEN on 28 July 2007.CEN members are bound 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 bibliographica
8、l references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN mem
9、ber into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, La
10、tvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussel
11、s 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 5398-4:2007: EForeword This document (EN ISO 5398-4:2007) has been prepared by Technical Committee CEN/TC 289 “Leather“, the secretariat of which is held by UNI, in collabora
12、tion with the International Union of Leather Technologists and Chemists Societies (IULTCS). 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 February 2008, and conflicting national standards shall
13、be withdrawn at the latest by February 2008. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, German
14、y, 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 5398-4:2007IULTCS/IUC8:4:2007Reference numberISO 5398-4:2007(E)IULTCS/IUC 8:4:2007(E)INTERN
15、ATIONAL STANDARD ISO5398-4IULTCS/IUC8:4First edition2007-08-01Leather Chemical determination of chromic oxide content Part 4: Quantification by inductively coupled plasma optical emission spectrometer (ICP-OES) Cuir Dosage chimique de loxyde de chrome Partie 4: Quantification par plasma couplage ind
16、uctif spectromtre dmission optique (ICP-OES) EN ISO 5398-4:2007IULTCS/IUC8:4:2007ii iiiContents Page Foreword iv Introduction v 1 Scope 1 2 Normative references 1 3 Terms and definitions .1 4 Principle2 5 Sampling and sample preparation.2 6 Reagents.2 6.1 Wet oxidation method .2 6.2 ICPOES .2 7 Appa
17、ratus .2 8 Methods 3 8.1 Preparation of analytical solution3 8.2 Measurement of the aqueous solution3 9 Calculation and expression of results.4 10 Test report 5 Annex A (informative) Determination of water and other volatile matter6 EN ISO 5398-4:2007IULTCS/IUC8:4:2007iv Foreword ISO (the Internatio
18、nal 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 committee has been
19、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 electrotechnical standar
20、dization. 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 member bodies for v
21、oting. 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 identifying any or all s
22、uch patent rights. This part of ISO 5398 was prepared by the Chemical Tests 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, Leather, t
23、he secretariat of which is held by UNI, in accordance with the agreement on technical co-operation between ISO and CEN (Vienna Agreement). It is based on IUC 8 originally published in J. Soc. Leather Trades Chemists 49, p. 17, (1965) and declared an official method of the IULTCS in 1965. IULTCS, ori
24、ginally 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 sampling and testing of leather. ISO recognizes IULT
25、CS as an international standardizing body for the preparation of test methods for leather. ISO 5398 consists of the following parts, under the general title Leather Chemical determination of chromic oxide content: Part 1: Quantification by titration Part 2: Quantification by colorimetric determinati
26、on Part 3: Quantification by atomic absorption spectrometry Part 4: Quantification by inductively coupled plasma optical emission spectrometer (ICP-OES) EN ISO 5398-4:2007IULTCS/IUC8:4:2007vIntroduction ISO 5398 has been split into four parts, each describing methods suitable for the determination o
27、f the chromic oxide content in leather. The different techniques have been described to reflect the variations in industrial practice compared with the more sensitive analytical equipment available for test laboratories. Variations also exist in the range of chromic oxide that the methods are deemed
28、 suitable to quantify. ISO 5398-4 describes a technique that is suitable for determining chromium more precisely than those described in ISO 5398-1 and ISO 5398-2. It requires the use of sophisticated analytical equipment, such as inductively coupled plasma and atomic absorption spectroscopy. EN ISO
29、 5398-4:2007IULTCS/IUC8:4:2007blank1Leather Chemical determination of chromic oxide content Part 4: Quantification by inductively coupled plasma optical emission spectrometer (ICP-OES) 1 Scope This part of ISO 5398 describes a method for the determination of chromium in aqueous solution obtained fro
30、m leather. This is an analysis for total chromium in leather; it is not compound specific or specific to its oxidation state. This method describes the determination of chromium by inductively coupled plasma optical emission spectrometry and is applicable to leathers which are expected to have chrom
31、ic oxide contents in excess of 1 mg/kg. Two techniques for the preparation of the solution to be analysed are included. In the case of dispute, the wet oxidation technique is to be used. 2 Normative references The following referenced documents are indispensable for the application of this document.
32、 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 location ISO 3696:1987, Water for analytical laboratory use
33、 Specification and test methods ISO 4044, Leather Chemical tests Preparation of chemical test samples EN 14602, Footwear Test methods for the assessment of ecological criteria ISO 4684, Leather Chemical tests Determination of volatile matter ISO 11885, Water quality Determination of selected element
34、s by inductively coupled plasma optical emission spectroscopy (ICP-OES) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 chromic oxide content amount of chromium in leather, determined by this method and reported as chromic oxide NOTE The chro
35、mic oxide content is expressed in milligrams per kilogram (mg/kg), based on dry matter. EN ISO 5398-4:2007IULTCS/IUC8:4:20072 4 Principle The chromium present in the leather is solubilized in the hexavalent state followed by analysis of the solution by inductively coupled plasma optical emission spe
36、ctrometer. 5 Sampling and sample preparation If possible, sample in accordance with ISO 2418 and grind leather in accordance with ISO 4044. If sampling in accordance with ISO 2418 is not possible (an in the case of leathers from finished products like shoes, garments), details about sampling shall b
37、e given together with the test report. Weigh 2 g of the ground leather to the nearest 0,001 g. From every leather, a minimum of two determinations shall be made. 6 Reagents Unless otherwise stated, only analytical grade chemicals are to be used. The water shall be grade 3 in accordance with ISO 3696
38、:1987. All solutions are aqueous solutions. 6.1 Wet oxidation method 6.1.1 Nitric acid, 70 %. 6.1.2 Sulfuric acid, concentrated (98 %), and perchloric acid (60 % to 70 %), mixed together in the ratio of 1:3 by volume. 6.2 ICPOES 6.2.1 Potassium dichromate (K2Cr2O7), dried for 16 h 2 h at 102 C 2 C.
39、6.2.2 Standard dichromate solution: dissolve 2,829 g potassium dichromate (6.2.1) in water in a volumetric flask and make up to 1 000 ml with water. 1 ml of this solution contains 1 mg of chromium. 7 Apparatus Usual laboratory apparatus is required and, in particular, the following. 7.1 Conical flas
40、k, 500 ml, with ground glass stopper. 7.2 Inductively coupled plasma optical emission spectrometer, as described in ISO 11885. 7.3 Filtration device, using glass fibre (GFC) or membrane type filters. 7.4 Antibumping granules (or similar) (wet oxidation method). EN ISO 5398-4:2007IULTCS/IUC8:4:200738
41、 Methods 8.1 Preparation of analytical solution 8.1.1 Wet oxidation method WARNING It is imperative that nitric acid is added first because of the possible explosive reaction of perchloric acid with leather. Accurately weigh a mass of leather (see Clause 5) into the conical flask (7.1). Add 10 ml of
42、 nitric acid (6.1.1) and allow to stand for 2 min. Add 15 ml of mixed sulfuric/perchloric acids (6.1.2) and a few antibumping granules (7.4). Place a funnel or splash bulb in the neck of the flask and heat to boiling on a wire gauze over a moderate flame. As soon as the reaction mixture begins to tu
43、rn orange, lower the flame. After a complete change of colour, heat gently for at least 2 min. Allow to cool in air for 5 min and dilute to approximately 200 ml. Boil for 10 min to eliminate any chlorine. The use of a sulfuric/perchloric acid mixture is preferred to the use of the individual acids a
44、s it prevents the accidental use of perchloric acid alone. In the case of incomplete oxidation (i.e. the solution does not change to an orange colour), it is permissible to add further mixed sulfuric/perchloric acid to the sample. 8.1.2 Microwave digestion The sample for analysis can also be prepare
45、d through application of microwave-assisted digestion (MAD). If this is to be used, then the procedure described in EN 14602 shall be followed. 8.2 Measurement of the aqueous solution 8.2.1 General Prepare the inductively coupled plasma optical emission spectrometer (7.2) by following the manufactur
46、ers instructions for adjusting all the instruments parameters. Below are some recommended settings; however, ICP manufacturers have their own recommended settings for chromium which should be used when available. For further information, refer to ISO 11885. Plasma argon flow: 15 l/min Auxiliary argo
47、n flow: 0,5 l/min Nebulizer argon flow: 0,8 l/min Power: 1 300 W Gas: Argon 4.6 Sample flow rate: 1,3 ml/min Sample flash rate: 4,0 ml/min Replicates: 3 Peak algorithms: Peak area, 3 points with 2 points background correction Wavelength: 357 nm, 869 nm EN ISO 5398-4:2007IULTCS/IUC8:4:20074 Before ca
48、rrying out the spectrometric measurements, set up the spectrometer according to the manufacturers instructions by aspirating a 1,0 mg/l Mn2+(axial view torch) calibration solution. Optimize the aspiration and plasma condition (aspiration rate, position of the torch module). Aspirate distilled water
49、and adjust controls to give a steady zero (base line) reading. 8.2.2 Preparation of calibration graph Prepare standard solutions by pipetting 10 ml of the standard dichromate solution (6.2.2) into a 100 ml volumetric flask and making up to volume with distilled water. Pipette 1,0 ml, 2,0 ml, 4,0 ml and 6,0 ml aliquots of this solution into 100 ml volumetric flasks and make up to volume with distilled water. These solutions contain 1,0 g/ml, 2,0 g/ml, 4,0 g/ml and 6,0 g/ml of chromium, respectively.
