EN ISO 17075-2007 Leather - Chemical tests - Determination of chromium(VI) content《皮革 化学试验 氯(VI)含量的测定[被代替 CEN CEN TS 14495]》.pdf

1、BRITISH STANDARDBS EN ISO 17075:2007Leather Chemical tests Determination of chromium(VI) contentThe European Standard EN ISO 17075:2007 has the status of a British StandardICS 59.140.30g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55

2、g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN ISO 17075:2007This British Standard was

3、 published under the authority of the Standards Policy and Strategy Committee on 31 December 2007 BSI 2007ISBN 978 0 580 56381 2National forewordThis British Standard is the UK implementation of EN ISO 17075:2007. It supersedes DD CEN/TS 14495:2003 which is withdrawn.The UK participation in its prep

4、aration was entrusted to Technical Committee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this 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 f

5、or its correct application.Compliance with a British Standard cannot confer immunity from legal obligations. Amendments issued since publicationAmd. No. Date CommentsCopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking per

6、mitted without license from IHS-,-,-EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 17075November 2007ICS 59.140.30 Supersedes CEN/TS 14495:2003 English VersionLeather - Chemical tests - Determination of chromium(VI)content (ISO 17075:2007)Cuir - Essais chimiques - Dtermination de la teneur en

7、chrome(VI) (ISO 17075:2007)Leder - Chemische Prfungen - Bestimmung desChrom(VI)-Gehalts (ISO 17075:2007)This European Standard was approved by CEN on 24 October 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStand

8、ard the status of a national standard without any alteration. Up-to-date lists and bibliographical 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,

9、German). A version in any other language made by translationunder the responsibility of a CEN member 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

10、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 COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE

11、 NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 17075:2007: ECopyright European Committee for Standardization Provided by IHS

12、 under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Foreword This document (EN ISO 17075:2007) has been prepared by Technical Committee CEN/TC 289 “Leather“, the secretariat of which is held by UNI, in collaboration with the International Union o

13、f 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 May 2008, and conflicting national standards shall be withdrawn at the latest by May 2008.

14、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 CEN/TS 14495:2003. According to the CEN/CENELEC Internal Regu

15、lations, 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, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Neth

16、erlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 17075:2007 has been approved by CEN as a EN ISO 17075:2007 without any modification. EN ISO 17075:2007Copyright European Committee for Standardization

17、 Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Reference numberISO 17075:2007(E)IULTCS/IUC 18:2007(E)INTERNATIONAL STANDARD ISO17075IULTCS/IUC18First edition2007-11-15Leather Chemical tests Determination of chromium(VI) conte

18、nt Cuir Essais chimiques Dtermination de la teneur en chrome(VI) EN ISO 17075:2007Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ii Copyright European Committee for Standardizat

19、ion Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Terms and definitions .1 4 Principle1 5 Reagents.2 6 Apparatus .2 7 Procedure .3 7.1 Sampling and preparation

20、 of samples.3 7.2 Preparation of analytical solution3 7.3 Determination of chromium(VI) in the solution obtained from the extraction procedure3 7.4 Blank solution 4 7.5 Calibration 4 7.6 Determination of the recovery rate 4 7.6.1 Influence of the matrix 4 7.6.2 Influence of the RP material .5 8 Calc

21、ulation and expression of results.5 8.1 Calculation of chromium(VI) content.5 8.2 Recovery rate (according to 7.6.1).6 8.3 Expression of results 6 9 Test report 6 Annex A (informative) Reversed phase material7 Annex B (informative) Accuracy 8 EN ISO 17075:2007Copyright European Committee for Standar

22、dization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Int

23、ernational 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 w

24、ith ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of techni

25、cal committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn

26、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 such patent rights. ISO 17075:2007 was prepared by the Chemical Test Commission of the International Union of Leather Technologists and Chem

27、ists Societies (IUC Commission, IULTCS) in collaboration with the European Committee for Standardisation (CEN) Technical Committee CEN/TC 289, Leather, the secretariat of which is held by UNI, in accordance with the Agreement on technical co-operation between ISO and CEN (Vienna Agreement). IULTCS,

28、originally 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 I

29、ULTCS as an international standardizing body for the preparation of test methods for leather. This first edition of ISO 17075 cancels and replaces the first edition of CEN TS 14495:2003, which has been technically revised. EN ISO 17075:2007Copyright European Committee for Standardization Provided by

30、 IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-1Leather Chemical tests Determination of chromium(VI) content 1 Scope This International Standard specifies a method for determining chromium(VI) in solutions leached from leather under defi

31、ned conditions. The method described is suitable to quantify the chromium(VI) content in leathers down to 3 mg/kg. This document is applicable to all leather types. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references,

32、 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, Water for analytical laboratory use Specification and test met

33、hods ISO 4044, Leather Chemical tests Preparation of chemical test samples ISO 4684, Leather Chemical tests Determination of volatile matter 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 chromium(VI) content amount of chromium(VI) in leathe

34、r determined by this method after extraction with an aqueous salt solution at pH 7,5 to 8,0 NOTE The chromium(VI) content is reported as chromium(VI) in milligrams per kilogram (mg/kg), expressed as the dry mass of the sample. 4 Principle Soluble chromium(VI) is leached from the sample in phosphate

35、buffer at pH 7,5 to 8,0 and 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 quantified photometrically at 540 nm.

36、The results obtained from the described 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 this standard. EN ISO

37、17075:2007Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-2 5 Reagents All reagents used shall have at least analytical grade purity. 5.1 Extraction solution. Dissolve 22,8 g dip

38、otassiumhydrogenphosphate 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 nitrogen. 5.2 Diphenylcarbazide solution. Dissolve 1,0 g 1,5-diphenylcarbazide CO(NHNHC6H5)2in 100 ml acetone (CH3)2CO and acidified with one drop of gl

39、acial 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 solution. 700 ml o-phosphoric acid, = 1,71 g/ml, made up to 1 000 ml with distilled water. 5.4 Chromium(VI) stock solution. Dissolve 2,829 g potassium dichromat

40、e (K2Cr2O7) (5.8) 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. 5.5 Chromium(VI) standard solution. Pipette 1 ml of solution (5.4) into a 1 000 ml volumetric flask and make up to the mark with extraction solution (5.1). 1 ml of th

41、is solution contains 1 g of chromium. 5.6 Argon or nitrogen, oxygen-free. Preference should be given to argon as an inert gas instead of nitrogen because argon has a higher specific mass than air. 5.7 Distilled water, Grade 3 quality as specified in ISO 3696. 5.8 Potassium dichromate (K2Cr2O7), drie

42、d for 16 h 2 h at 102 C 2 C. 5.9 Methanol, HPLC grade. 6 Apparatus 6.1 Suitable mechanical shaker, 50 min1to 150 min1.6.2 Conical flask, of capacity 250 ml, with stopper. 6.3 Aeration tube and flow meter. 6.4 pH meter, with glass electrode. 6.5 Membrane filter, 0,45 m pore size (polytetrafluoroethyl

43、ene or nylon). 6.6 Volumetric flasks, of capacity 25 ml, 100 ml and 1 000 ml. 6.7 Pipettes, various nominal volumes. EN ISO 17075:2007Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-

44、,-,-36.8 Spectrophotometer or filterphotometer, wavelength 540 nm. 6.9 Photometric cell, quartz, 4 cm length or any other suitable cell length. 6.10 Glass or polypropylene cartridges filled with suitable reversed phase material, e.g. reversed phase (RP) 18. 6.11 Solid Phase Extraction (SPE) system,

45、with vacuum device or solvent resistant medical syringe. 7 Procedure 7.1 Sampling and preparation of samples If possible, sample in accordance with ISO 2418 and grind leather in accordance with ISO 4044. Grinding should take place shortly prior to the extraction process. If sampling in accordance wi

46、th ISO 2418 is not possible (e.g. leathers from finished products like shoes, garments), details about sampling shall be given together with the test report. 7.2 Preparation of analytical solution Weigh 2 g 0,01 g of ground leather to the nearest 0,001 g. Pipette 100 ml of degassed solution (5.1) in

47、to a 250 ml conical flask (6.2). Displace oxygen by passing oxygen-free argon (or nitrogen) (5.6) into the flask for 5 min (50 ml/min 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 leather powder suspension 3

48、 h 5 min on a mechanical shaker to extract the chromium(VI). Gently shake the suspension in a smooth circular movement to keep the leather powder from adhering to the wall of the flask. Avoid shaking it too quickly. Immediately after completing 3 h of extraction, filter the content of the conical flask through a membrane filter into a glass bottle with screw cap. Check the pH of the solution. The pH of the solution shall be between 7,5 and 8,0. If the pH of the solution is not within this range, start the complete procedure again. 7.3