BS EN ISO 17075-2-2017 Leather Chemical determination of chromium(VI) content in leather Chromatographic method《皮革 皮革中铬(VI)含量的化学测定 色谱法》.pdf

1、BS EN ISO 17075-2:2017Leather Chemicaldetermination of chromium(VI)content in leatherPart 2: Chromatographic method (ISO17075-2:2017)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 17075-2:2017 BRITISH STANDARDNational forewordThis British Standard is the U

2、K implementation of EN ISO17075-2:2017. Together with BS EN ISO 17075-1:2017, it supersedes BS EN ISO 17075:2007 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this com

3、mittee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2017. Published by BSI Standards Limited 2017ISBN 978 0 580 89417 6ICS 59.140.

4、30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 28 February 2017.Amendments/corrigenda issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENN

5、E EUROPISCHE NORM EN ISO 17075-2 February 2017 ICS 59.140.30 Supersedes EN ISO 17075:2007English Version Leather - Chemical determination of chromium(VI) content in leather - Part 2: Chromatographic method (ISO 17075-2:2017) Cuir - Dtermination chimique de la teneur en chrome(VI) du cuir - Partie 2:

6、 Mthode chromatographique (ISO 17075-2:2017) Leder - Chemische Bestimmung des Chrom(VI)-Gehalts in Leder - Teil 2: Chromatographie (ISO 17075-2:2017)This European Standard was approved by CEN on 30 December 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipula

7、te 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 on application to the CEN-CENELEC Management Centre or to any CEN member. This European Sta

8、ndard 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 has the same status as the official versions. CEN members are the na

9、tional standards bodies 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, S

10、erbia, Slovakia, Slovenia, 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

11、by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17075-2:2017 EBS EN ISO 17075-2:2017EN ISO 17075-2:2017 (E) 3 European foreword This document (EN ISO 17075-2:2017) has been prepared by Technical Committee IULTCS “International Union of Leather Technologists and Chemists Soc

12、ieties“ in collaboration with Technical Committee CEN/TC 289 “Leather” the secretariat of which is held by UNI. 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

13、 standards shall 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. This document supersedes E

14、N ISO 17075:2007. 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, Denmark, Estonia, Finland, Former Yugoslav Republic of Mace

15、donia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, 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 17075-2:2017 has been appr

16、oved by CEN as EN ISO 17075-2:2017 without any modification. BS EN ISO 17075-2:2017ISO 17075-2:2017(E)IULTCS/IUC 18-2:2017(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Chemicals . 26 Apparatus and materials 27 Procedure. 37.1 Sampling and preparation of s

17、amples 37.2 Preparation of analytical solution 37.3 Chromatographic conditions 47.4 Calibration 47.5 Determination of the recovery rate . 58 Calculation and expression of results . 58.1 Calculation of chromium(VI) content 58.2 Recovery rate (according to 7.5) . 68.3 Expression of results 69 Test rep

18、ort . 6Annex A (informative) Accuracy 7Annex B (informative) Chromatographic conditions for direct detection method 9Annex C (informative) Chromatographic conditions for method with post-column reaction.12Annex D (informative) Comparison between the colorimetric method (ISO 17075-1) and the ionic ch

19、romatography method (ISO 17075-2) .16 ISO 2017 All rights reserved iiiContents PageBS EN ISO 17075-2:2017ISO 17075-2:2017(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International

20、 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 non-governmental, in liaison with ISO, a

21、lso take 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.

22、 In particular 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 el

23、ements of 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 recei

24、ved (see 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 a

25、dherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .htmlISO 17075-2 was prepared by the Chemical Test Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commiss

26、ion, IULTCS) 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

27、 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 IULTCS as an international sta

28、ndardizing body for the preparation of test methods for leather.This first edition of ISO 17075-2, together with ISO 17075-1, cancels and replaces ISO 17075:2007, which has been technically revised.The main changes compared to ISO 17075:2007 are as follows: the chromatographic analytical technique h

29、as been added; the sample preparation has been revised; mechanical shaking in 7.1 and 7.2 has been revised.A list of all parts in the ISO 17075 series can be found on the ISO website.IULTCS/IUC 18-2:2017(E)iv ISO 2017 All rights reservedBS EN ISO 17075-2:2017INTERNATIONAL STANDARDISO 17075-2:2017(E)

30、IULTCS/IUC 18-2:2017(E)Leather Chemical determination of chromium(VI) content in leather Part 2: Chromatographic 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 chr

31、omium(VI) content in leathers down to 3 mg/kg.This document is 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 com

32、parable with the results produced by the procedure described in this document.If a leather sample is tested with both ISO 17075-1 and this document, the results obtained with this document are considered as the reference. The advantage of the method described in this document is that there are no in

33、terferences from the colour of the extract. Nevertheless, interlaboratory trials do not show significant differences (see Annex D) 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 con

34、tent constitutes requirements 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 locationISO 3

35、696, Water for analytical laboratory use Specification and test methodsISO 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 definiti

36、ons apply.ISO and IEC maintain terminological databases for use in 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 l

37、eather determined after extraction with an aqueous salt solution at 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 17075-2:2017ISO 17075-2:2017(E)4

38、 PrincipleExtractable chromium(VI) is leached from the sample in phosphate buffer at pH 7,0 to 8,0. An aliquot of the filtered extract is analysed for Cr(VI) using ion-exchange chromatography with UV-VIS detection.5 ChemicalsAll reagents used shall have at least analytical grade purity.5.1 Extractio

39、n solutionDissolve 22,8 g dipotassium hydrogenphosphate K2HPO43H2O in 1 000 ml water (5.7), adjusted to pH 8,0 0,1 with phosphoric acid (5.2). Degas this solution with either argon or nitrogen (5.6) or ultrasonic bath.Standard practice is to make up a fresh solution each day. However, the solution c

40、an 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 Phosphoric acid solution700 ml o-phosphoric acid, = 1,71 g/ml, made up to 1 000 ml with water (5.7).First add approximately 200 ml of deionised water (5.7) to a 1 000 ml v

41、olumetric flask, then add the 700 ml of o-phosphoric acid and dilute to the mark with deionised water.5.3 Potassium dichromate (K2Cr2O7), dried for (16 2) h at (102 2) C.5.4 Chromium(VI) stock solutionDissolve 2,829 g potassium dichromate (K2Cr2O7) (5.3) in water (5.7) in a volumetric flask and make

42、 up to 1 000 ml with water (5.7). 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 volumetric flask a

43、nd 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 of hexavalent chromium at this concentration

44、level 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.5.7 Distilled or deionised water, Grade 3 quality as specified in ISO 3696.6 Apparatus and materi

45、alsUsual laboratory equipment and, in particular, the following.IULTCS/IUC 18-2:2017(E)2 ISO 2017 All rights reservedBS EN ISO 17075-2:2017ISO 17075-2:2017(E)6.1 Suitable mechanical orbital shaker, (100 10) min1.6.2 Conical flask, of capacity 250 ml, with stopper.6.3 Aeration tube and flow meter, su

46、itable 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 Common laboratory glassware and pipettes.6.6 Ion-exchange chromatograph, with UV detector or high performance liquid chromatograph (HPLC) with anion-exchange column and U

47、V detector. It is recommended a photo diode array detector (DAD).6.7 Analytical balance, capable of weighing to 0,1 mg.6.8 Suitable vials for HPLC.6.9 Sharp cutting tool or blade, suitable for cutting the leather into 3 mm to 5 mm pieces.7 Procedure7.1 Sampling and preparation of samplesIf possible,

48、 sample in accordance with ISO 2418. If sampling in accordance with ISO 2418 is not possible (e.g. leathers from finished products like shoes, garments), details about sampling shall be given in the test report.Prepare the leather sample by cutting (6.9) into small pieces according to the method spe

49、cified in ISO 4044:2017, 6.3.7.2 Preparation of analytical solutionWeigh (6.7) approximately (2 0,1) g of leather pieces to the nearest 0,001 g. Pipette 100 ml of degassed solution (5.1) into a 250 ml conical flask (6.2). Displace oxygen by passing oxygen-free argon (or nitrogen) (5.6) into the flask for 5 min with a volume flow of (50 10) ml/min. Remove the aeration tube (6.3), add the leather and close the flask with a stopper. Record the extract volume as V0.Shake the conical flask with the leather pieces f