1、BS EN ISO 17075-1:2017Leather Chemicaldetermination of chromium(VI)content in leatherPart 1: Colorimetric method (ISO17075-1:2017)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 17075-1:2017 BRITISH STANDARDNational forewordThis British Standard is the UK i
2、mplementation of EN ISO 17075-1:2017. Together with BS EN ISO 17075-2:2017, it supersedes BS EN ISO 17075:2007 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented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 comm
3、ittee 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. The British Standards Institution 2017.Published by BSI Standards Limited 2017ISBN 978 0 580 86630 2 ICS 59.14
4、0.30 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD
5、 NORME EUROPENNE EUROPISCHE NORM EN ISO 17075-1 February 2017 ICS 59.140.30 English Version Leather - Chemical determination of chromium(VI) content in leather - Part 1: Colorimetric method (ISO 17075-1:2017) Cuir - Dtermination chimique de la teneur en chrome(VI) du cuir - Partie 1: Mthode colorimt
6、rique (ISO 17075-1:2017) Leder - Bestimmung des Chrom(VI)-Gehalts in Leder - Teil 1: Kolorimetrisches Verfahren (ISO 17075-1:2017)This European Standard was approved by CEN on 30 December 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions f
7、or 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 application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in thr
8、ee 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 has the same status as the official versions. CEN members are the national standards bo
9、dies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Sl
10、ovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserv
11、ed worldwide for CEN national Members. Ref. No. EN ISO 17075-1:2017 EBS EN ISO 17075-1:2017EN ISO 17075-1:2017 (E) 3 European foreword This document (EN ISO 17075-1:2017) has been prepared by Technical Committee CEN/TC 289 “Leather” the secretariat of which is held by UNI, in collaboration with Tech
12、nical Committee IULTCS “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 2017, and conflicting national standards shall
13、be withdrawn at the latest by August 2017. 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 Internal Regul
14、ations, 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, It
15、aly, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 17075-1:2017 has been approved by CEN as EN ISO 17075-1:2017 without any modification.
16、BS EN ISO 17075-1:2017ISO 17075-1:2017(E)IULTCS/IUC 18-1:2017(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Chemicals . 26 Apparatus and materials 37 Procedure. 37.1 Sampling and preparation of samples 37.2 Preparation of analytical solution 37.3 Determina
17、tion of chromium(VI) in the solution obtained from the extraction procedure 47.4 Blank solution 47.5 Calibration 57.6 Determination of the recovery rate . 57.6.1 Influence of the matrix . 57.6.2 Influence of the SPE material (6.9) 58 Calculation and expression of results . 68.1 Calculation of chromi
18、um(VI) content 68.2 Recovery rate (according to 7.6.1) . 68.3 Expression of results 79 Test report . 7Annex A (informative) Solid phase extraction (SPE) material . 8Annex B (informative) Accuracy 9Annex C (informative) Comparison between the colorimetric method (ISO 17075-1) and the ionic chromatogr
19、aphy method (ISO 17075-2) .11 ISO 2017 All rights reserved iiiContents PageBS EN ISO 17075-1:2017ISO 17075-1:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standar
20、ds 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 non-governmental, in liaison with ISO, also take
21、 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In part
22、icular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).Attention is drawn to the possibility that some of the elements o
23、f this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see
24、 www .iso .org/ patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence
25、 to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .htmlISO 17075-1 was prepared by the Chemical Test Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, IUL
26、TCS) in collaboration with the European Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of which is held by UNI, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).IULTCS, originally formed in 1897, is a world
27、-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 IULTCS as an international standardizi
28、ng body for the preparation of test methods for leather.This first edition of ISO 17075-1, together with ISO 17075-2, cancels and replaces ISO 17075:2007, which has been technically revised.The main changes compared to ISO 17075:2007 are as follows: the sample preparation has been revised; mechanica
29、l shaking in 7.1, 7.2 and 7.3 has been revised.A list of all parts in the ISO 17075 series can be found on the ISO website.IULTCS/IUC 18-1:2017(E)iv ISO 2017 All rights reservedBS EN ISO 17075-1:2017INTERNATIONAL STANDARDISO 17075-1:2017(E)IULTCS/IUC 18-1:2017(E)Leather Chemical determination of chr
30、omium(VI) content in leather Part 1: Colorimetric method1 ScopeThis document specifies a method for determining chromium(VI) in solutions leached from leather under defined conditions. The method described is suitable to quantify the chromium(VI) content in leathers down to 3 mg/kg.This document is
31、applicable to all leather types.The results obtained from this method are strictly dependent on the extraction conditions. Results obtained by using other extraction procedures (extraction solution, pH, extraction time, etc.) are not comparable with the results produced by the procedure described in
32、 this document.If a leather sample is tested with both this document and ISO 17075-2, the results obtained with ISO 17075-2 are considered as the reference. The advantage of the method described in ISO 17075-2 is that there are no interferences from the colour of the extract. Nevertheless, interlabo
33、ratory trials do not show significant differences (see Annex C) and the results are comparable between both methods.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated reference
34、s, 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 locationISO 3696, Water for analytical laboratory use Specification and test met
35、hodsISO 4044:2017, Leather Chemical tests Preparation of chemical test samplesISO 4684, Leather Chemical tests Determination of volatile matter3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in
36、standardization at the following addresses: ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp IEC Electropedia: available at h t t p :/ www .electropedia .org/ 3.1chromium(VI) contentamount of chromium(VI) in leather determined after extraction with an aqueous salt solution at
37、 pH 7,0 to 8,0Note 1 to entry: The chromium(VI) content is reported as chromium(VI) in milligrams per kilogram (mg/kg), expressed as the dry mass of the sample. ISO 2017 All rights reserved 1BS EN ISO 17075-1:2017ISO 17075-1:2017(E)4 PrincipleExtractable chromium(VI) is leached from the sample in ph
38、osphate buffer at pH 7,0 to 8,0 and co-extracted coloured substances which influence the detection are removed by solid phase extraction if necessary. The chromium(VI) in solution oxidizes 1,5-diphenylcarbazide to 1,5-diphenylcarbazone to give a red/violet complex with chromium which can be quantifi
39、ed photometrically at 540 nm.5 ChemicalsAll reagents used shall have at least analytical grade purity.5.1 Extraction solutionDissolve 22,8 g dipotassium hydrogenphosphate, K2HPO43H2O, in 1 000 ml water, adjusted to pH 8,0 0,1 with phosphoric acid (5.3). Degas this solution with either argon or nitro
40、gen (5.6) or ultrasonic bath.Standard practice is to make up a fresh solution each day. However, the solution can be kept for up to one week in a refrigerator at (4 3) C but shall be warmed to room temperature and degassed prior to use.5.2 Diphenylcarbazide (DPC) solutionDissolve 1,0 g 1,5-diphenylc
41、arbazide, CO(NHNHC6H5)2, in 100 ml acetone, (CH3)2CO, and acidified with one drop of glacial acetic acid, CH3COOH.The solution should be kept in a brown glass bottle. The shelf life is up to 14 days at 4 C.5.3 Phosphoric acid solution700 ml o-phosphoric acid, = 1,71 g/ml, made up to 1 000 ml with de
42、ionised water (5.7).First add approximately 200 ml of deionised water (5.7) to a 1 000 ml volumetric flask, then add the 700 ml of o-phosphoric acid and dilute to the mark with deionised water.5.4 Chromium(VI) stock solutionDissolve 2,829 g potassium dichromate (K2Cr2O7) (5.8) in water in a volumetr
43、ic flask and make up to 1 000 ml with water. One millilitre of this solution contains 1 mg of chromium.A stock solution at this concentration level of hexavalent chromium is an alternative available commercially.5.5 Chromium(VI) standard solutionPipette 1 ml of solution (5.4) into a 1 000 ml volumet
44、ric flask and make up to the mark with extraction solution (5.1). One millilitre of this solution contains 1 g of chromium.The solution can be kept for up to one week in a refrigerator at (4 3) C but shall be warmed to room temperature prior to use.A stock solution at this concentration level of hex
45、avalent chromium is an alternative available commercially.5.6 Argon or nitrogen, oxygen-freePreference should be given to argon as an inert gas instead of nitrogen because argon has a higher specific mass than air.IULTCS/IUC 18-1:2017(E)2 ISO 2017 All rights reservedBS EN ISO 17075-1:2017ISO 17075-1
46、:2017(E)5.7 Distilled or deionised water, Grade 3 quality as specified in ISO 3696.5.8 Potassium dichromate (K2Cr2O7), dried for (16 2) h at (102 2) C.5.9 Methanol, HPLC grade.6 Apparatus and materialsUsual laboratory equipment and, in particular, the following.6.1 Suitable mechanical orbital shaker
47、, (100 10) min1.6.2 Conical flask, of capacity 250 ml, with stopper.6.3 Aeration tube and flow meter, suitable for a flow rate of (50 10) ml/min.6.4 Membrane filter, 0,45 m pore size polytetrafluoroethylene (PTFE) or polyamide 66.6.5 Volumetric flasks, of capacity 25 ml, 100 ml and 1 000 ml.6.6 Pipe
48、ttes, various nominal volumes.6.7 Spectrophotometer or filterphotometer, wavelength 540 nm.6.8 Photometric cell, quartz, 40 mm length or any other suitable cell length.6.9 Glass or polypropylene cartridges filled with a suitable solid phase extraction (SPE) material, e.g. reversed phase (RP) C18 or
49、a suitable activated magnesium silicate, see Annex A for examples of SPE materials.6.10 Solid phase extraction (SPE) system, with vacuum device or solvent-resistant medical syringe.6.11 Sharp cutting tool or blade, suitable for cutting the leather into 3 mm to 5 mm pieces.6.12 Analytical balance, capable of weighing to the nearest 0,1 mg.7 Procedure7.1 Sampling and preparation of samplesIf possible, sample in accordance with ISO 2418. If sampling in accordance with ISO 2418 is not possible (e.g. leathers from fin
