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1、 Reference number ISO 17075:2007(E) IULTCS/IUC 18:2007(E) ISO 2007 INTERNATIONAL STANDARD ISO 17075 IULTCS/IUC 18 First edition 2007-11-15 Leather Chemical tests Determination of chromium(VI) content Cuir Essais chimiques Dtermination de la teneur en chrome(VI) Copyright International Organization f
2、or Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or networking permitted without license from IHS -,-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) PDF disclaimer This PDF file may contain
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5、ers were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2007 All right
6、s reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the
7、requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2007 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with
8、ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or networking permitted without license from IHS -,-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) ISO 2007 All rights reserved iii Contents Page Foreword iv 1 Scope 1 2 Normative references1 3
9、Terms and definitions .1 4 Principle1 5 Reagents.2 6 Apparatus .2 7 Procedure .3 7.1 Sampling and preparation 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 solution4 7.5 Calibration4 7.6 Determ
10、ination of the recovery rate4 7.6.1 Influence of the matrix 4 7.6.2 Influence of the RP material .5 8 Calculation 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 report6 Annex A (informative) Reversed p
11、hase material7 Annex B (informative) Accuracy8 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or networking permitted without license from IHS -,
12、-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) iv ISO 2007 All rights reserved Foreword ISO (the International 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
13、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 part in the work. ISO collaborates clo
14、sely 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 technical committees is to prepare International Standards. Dra
15、ft 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 to the possibility that some of the elements of this docu
16、ment 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 Chemists Societies (IUC Commission, IULTCS) in collaboration
17、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, originally formed in 1897, is a world-wide organization o
18、f 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 standardizing body for the prep
19、aration 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. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, Use
20、r=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 17075:2007(E) IULTCS/IUC 18:2007(E) ISO 2007 All rights reserved 1 Leather Chemical tests Determination of chromium(VI) content 1 Scope This Internati
21、onal Standard 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 applicable to all leather types. 2 Normative references The fo
22、llowing 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 2418, Leather Chemical, physical and mechanical and
23、 fastness tests Sampling location ISO 3696, Water for analytical laboratory use Specification and test methods 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 docu
24、ment, the following terms and definitions apply. 3.1 chromium(VI) content amount of chromium(VI) in leather 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), expresse
25、d as the dry mass of the sample. 4 Principle Soluble chromium(VI) is leached from the sample in phosphate 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-diphen
26、ylcarbazone to give a red/violet complex with chromium which can be quantified photometrically at 540 nm. 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 tim
27、e, etc.) are not comparable with the results produced by the procedure described in this standard. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction
28、 or networking permitted without license from IHS -,-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) 2 ISO 2007 All rights reserved 5 Reagents All reagents used shall have at least analytical grade purity. 5.1 Extraction solution. Dissolve 22,8 g dipotassiumhydrogenphosphate K2HPO43H2O in 1 000 ml water,
29、 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)2 in 100 ml acetone (CH3)2CO and acidified with one drop of glacial acetic acid CH3COOH. The solution should be kept
30、 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 dichromate (K2Cr2O7) (5.8) in water in a volumetric flask and m
31、ake 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 this solution contains 1 g of chromium. 5.6 Argon or nit
32、rogen, 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), dried for 16 h 2 h at 102 C 2 C. 5.9 Methanol, HPLC grade.
33、 6 Apparatus 6.1 Suitable mechanical shaker, 50 min1 to 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 (polytetrafluoroethylene or nylon). 6.6 Volumetric flasks, of capacity 25
34、 ml, 100 ml and 1 000 ml. 6.7 Pipettes, various nominal volumes. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or networking permitted without l
35、icense from IHS -,-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) ISO 2007 All rights reserved 3 6.8 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
36、 phase material, e.g. reversed phase (RP) 18. 6.11 Solid Phase Extraction (SPE) system, 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
37、 should take place shortly prior to the extraction process. 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 together with the test report. 7.2 Preparation of analytical solution Weigh 2 g 0,01
38、g of ground leather 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 (50 ml/min 10 ml/min). Remove the aeration tube (6.3), add the leather and close the flas
39、k with a stopper. Record the extract volume as V0. Shake the leather powder suspension 3 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 quick
40、ly. 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 c
41、omplete procedure again. 7.3 Determination of chromium (VI) in the solution obtained from the extraction procedure Pretreat the cartridges in the following way: a) flush the cartridge (6.10) first with 5 ml methanol (5.9), b) afterwards with 5 ml distilled water (5.7) and c) directly afterwards with
42、 10 ml of extraction solution (5.1). Do not dry the cartridges (6.10) during or after the pre-treatment. From the solution obtained in 7.2, take 10 ml (V1) and transfer this quantitatively through the cartridge (6.10) on an SPE system with vacuum device (6.11). Collect the eluate in a 25 ml volumetr
43、ic flask (6.6). Flush the cartridge with 10 ml extraction solution (5.1) into the 25 ml flask. Make up the flask to volume (V2) with extraction solution (5.1). Mark this solution as S1. Pipette (6.7) 10 ml (V3) of solution S1 into a 25 ml volumetric flask. Dilute the solution to 3/4 of the flasks vo
44、lume with extraction solution (5.1). Add 0,5 ml of phosphoric acid solution (5.3) and afterwards 0,5 ml of diphenylcarbazide solution (5.2). Make up the flask to volume (V4) with extraction solution (5.1) and mix well. Allow to stand for 15 min 5 min. Measure the absorbance of the solution at 540 nm
45、 in a 4 cm cell against the blank solution (7.4). Record the absorbance obtained as A1. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 12/17/2007 18:39:36 MSTNo reproduction or network
46、ing permitted without license from IHS -,-,- ISO 17075:2007(E) IULTCS/IUC 18:2007(E) 4 ISO 2007 All rights reserved For each run, pipette another 10 ml aliquot of solution S1 into a 25 ml volumetric flask and treat it as described above, but without the addition of the diphenylcarbazide solution (5.
47、2). Measure the absorbance of this solution in the same way as before and record it as A2. 7.4 Blank solution Fill a 25 ml volumetric flask three quarters full with extraction solution (5.1), add 0,5 ml of phosphoric acid (5.3) and 0,5 ml of diphenylcarbazide solution (5.2) and make up to the mark w
48、ith extraction solution (5.1) and mix well. Prepare this solution daily and store it in the dark. Treat the blank solution in the same way as the analytical solution, excluding the solid phase extraction. 7.5 Calibration Prepare calibrating solutions from the standard solution (5.5). The chromium concentration in these solutions should cover the expected range of measurements. Prepare the calibration solutions in 25 ml volumetric flasks (6.6). Plot a suitable calibration curve by using at least six