1、BSI Standards PublicationBS EN ISO 17070:2015Leather Chemicaltests Determinationof tetrachlorophenol-,trichlorophenol-,dichlorophenol-,monochlorophenol-isomersand pentachlorophenol contentBS EN ISO 17070:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 1
2、7070:2015. It supersedes BS EN ISO 17070:2006 which iswithdrawn.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 committee can be obtained on request to its secretary.This publication
3、 does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 78785 0 ICS 59.140.30 Compliance with a British Standard cannot confer immunity fro
4、m legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 February 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17070 February 2015 ICS 59
5、.140.30 Supersedes EN ISO 17070:2006English Version Leather - Chemical tests - Determination of tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochlorophenol-isomers and pentachlorophenol content (ISO 17070:2015) Cuir - Essais chimiques - Dtermination de la teneur en isomres de monochlorop
6、hnol, dichlorophnol, trichlorophnol, ttrachlorophnol et en pentachlorophnol (ISO 17070:2015) Leder - Chemische Prfungen - Bestimmung des Gehalts an Tetrachlorphenol-, Thrichlorphenol-, Dichlorphenol-, Monochlorphenol-Isomeren und Pentachlorphenol (ISO 17070:2015) This European Standard was approved
7、by CEN on 3 January 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate 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 stan
8、dards may be obtained on application to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own language and n
9、otified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary,
10、 Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC
11、Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17070:2015 EBS EN ISO 17070:2015EN ISO 17070:2015 (E) 3 Foreword This document (EN ISO 17070:2015) has been prepared by T
12、echnical Committee ISO/TC IULTCS “International Union of Leather Technologists and Chemists Societies” 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 publicatio
13、n of an identical text or by endorsement, at the latest by August 2015, and conflicting national standards shall be withdrawn at the latest by August 2015. 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 n
14、ot be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 17070:2006. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgar
15、ia, 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turk
16、ey and the United Kingdom. Endorsement notice The text of ISO 17070:2015 has been approved by CEN as EN ISO 17070:2015 without any modification. BS EN ISO 17070:2015ISO 17070:2015(E)IULTCS/IUC 25:2015(E) ISO 2015 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative ref
17、erences 13 Abbreviations. 14 Principle 15 Apparatus . 26 Reagents 26.1 Chlorinated phenol mix . 27 Sampling and preparation of samples . 38 Procedure. 38.1 Steam-distillation 38.2 Liquid-liquid-extraction and acetylation 48.3 Preparation of calibration mixture for acetylated CP and TCG . 48.4 Gas ch
18、romatography (GC) . 59 Expression of results 510 Test report . 5Annex A (informative) Chromatographic analyses 7Annex B (informative) Reliability of the method . 9BS EN ISO 17070:2015ISO 17070:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of nation
19、al 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 established has the right to be represented on that committee. Internatio
20、nal 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 standardization.The procedures used to develop this document and those intended
21、for its further maintenance are described in the ISO/IEC Directives, Part 1. 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.
22、org/directives).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 such patent rights. Details of any patent rights identified during the development of the document will b
23、e in the Introduction and/or on the ISO list of patent declarations received (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
24、 related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 17070 was prepared by the Chemical Test Commission of the International Union of Leather Techno
25、logists and Chemists Societies (IUC Commission, 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 Agree
26、ment).IULTCS, 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. IS
27、O recognizes IULTCS as an international standardizing body for the preparation of test methods for leather.This second edition of ISO 17070 cancels and replaces the first edition (ISO 17070:2006), which has been technically revised. ISO 17070:2006 previously replaced CEN/TS 14494.The following chang
28、es have been made: the additional chlorinated phenol substances tetrachlorophenol-, trichlorophenol-, dichlorophenol-, and monochlorophenol-isomers are included; a new Clause 3 has been inserted to list the chlorophenol abbreviations; the examples of chromatographic conditions, previously in 7.4, ha
29、ve been moved to a new Annex A (the previous Annex A becomes Annex B).Annexes A and B are informative.IULTCS/IUC 25:2015(E)iv ISO 2015 All rights reservedBS EN ISO 17070:2015ISO 17070:2015(E)IntroductionThis International Standard describes a procedure where the chlorinated phenols (CP) are acetylat
30、ed before the chromatographic detection and the amount of the detected chlorinated phenyl acetate is quantified via an internal standard correction.IULTCS/IUC 25:2015(E) ISO 2015 All rights reserved vBS EN ISO 17070:2015BS EN ISO 17070:2015Leather Chemical tests Determination of tetrachlorophenol-,
31、trichlorophenol-, dichlorophenol-, monochlorophenol-isomers and pentachlorophenol content1 ScopeThis International Standard specifies a method for determining the content of tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochlorophenol-isomers, and pentachlorophenol, its salts, and esters
32、in leather.NOTE Bromophenol isomers can also be determined using this method.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated re
33、ferences, 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 methodsISO 4044, Leather Chemical tests Preparation
34、of chemical test samplesISO 4684, Leather Chemical tests Determination of volatile matter3 AbbreviationsThe following abbreviations are used for chlorinated phenols in this International Standard:CP chlorinated phenolsDiCP dichlorophenolMoCP monochlorophenolPCP pentachlorophenolTCG tetrachloroguaiac
35、ol (tetrachloro-o-methoxyphenol)TeCP tetrachlorophenolTriCP trichlorophenol4 PrincipleFirst of all, the leather sample is submitted to steam-distillation.After extraction into n-hexane, the chlorinated phenols (CP) are acetylated by acetic anhydride and the chlorinated phenyl acetates are analysed b
36、y gas-chromatography with an electron capture detector (ECD) or mass selective detector (MSD). Quantification is performed by an external standard and a correction made with an internal standard.INTERNATIONAL STANDARDISO 17070:2015(E)IULTCS/IUC 25:2015(E) ISO 2015 All rights reserved 1BS EN ISO 1707
37、0:2015ISO 17070:2015(E)5 Apparatus5.1 Gas chromatography (GC), with ECD or MSD detector.5.2 Analytical balance, weighing to an accuracy of 0,1 mg.5.3 Suitable apparatus designed for steam distillation.5.4 Shaking machine, capable of at least 200 cycles per minute.5.5 Volumetric flasks, 500 ml and 50
38、 ml.5.6 Erlenmeyer (conical) flask, 100 ml.5.7 Separating funnel, 250 ml, or suitable vessel that allows separation of organic and aqueous phases, that can be sealed for vigorous shaking.5.8 Pasteur-pipettes, graduated pipettes, suitable auto-pipettes.5.9 Strainer with paper filter, grade 4, diamete
39、r 125 mm.6 ReagentsUnless otherwise specified, analytical grade chemicals should be used. Water shall be distilled or deionized, Grade 3 in accordance with ISO 3696.6.1 Chlorinated phenol mixA mix of the chlorinated phenols which contains the following isomers at a concentration of 100 g/ml in aceto
40、ne.2-Chlorophenol CAS1)-Number: 955783-Chlorophenol CAS-Number: 1084304-Chlorophenol CAS-Number: 1064892,3-Dichlorophenol CAS-Number: 5762492,4-Dichlorophenol CAS-Number: 1208322,5-Dichlorophenol CAS-Number: 5837882,6-Dichlorophenol CAS-Number: 876503,4-Dichlorophenol CAS-Number: 957723,5-Dichloroph
41、enol CAS-Number: 5913552,3,4-Trichlorophenol CAS-Number: 159506602,3,5-Trichlorophenol CAS-Number: 9337882,3,6-Trichlorophenol CAS-Number: 9337551) CAS Chemical Abstracts Service.IULTCS/IUC 25:2015(E)2 ISO 2015 All rights reservedBS EN ISO 17070:2015ISO 17070:2015(E)2,4,5-Trichlorophenol CAS-Number:
42、 959542,4,6-Trichlorophenol CAS-Number: 880623,4,5-Trichlorophenol CAS-Number: 6091982,3,4,5-Tetrachlorophenol CAS-Number: 49015132,3,4,6-Tetrachlorophenol CAS-Number: 589022,3,5,6-Tetrachlorophenol CAS-Number: 935955Pentachlorophenol CAS-Number: 87865NOTE This chlorinated phenol mix is available fr
43、om laboratory chemical suppliers.6.2 Tetrachloroguaiacol (TCG) (tetrachloro-o-methoxyphenol), at a concentration of 100 g/ml in acetone (internal standard), melting point 118 C to 119 C.6.3 Sulfuric acid, 1 mol/l.6.4 n-hexane, for residue analysis.6.5 Potassium carbonate, K2CO3.6.6 Acetic anhydride,
44、 C4H6O3.6.7 Anhydrous sodium sulphate.6.8 Distilled water, in accordance with Grade 3 of ISO 3696.6.9 Triethylamine.6.10 Acetone.7 Sampling and preparation of samplesIf possible, sample in accordance with ISO 2418. Cut the leather sample into small pieces or grind the leather in accordance with ISO
45、4044. The dimensions of the pieces shall not be larger than 2 mm to 3 mm. 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.8 Procedure8.1 Steam-distillationAccurate
46、ly weigh approximately 1,0 g of the leather sample into the distillation vessel (5.3). Add 20 ml of 1 mol/l sulfuric acid (6.3) and 100 l of the TCG stock solution (6.2). Submit the contents of the vessel to a steam distillation by using a suitable steam distillation apparatus. Use a 500 ml volumetr
47、ic flask (5.5) with 5 g K2CO3(6.5) to collect the distillate.Distill about 450 ml. Make up to volume (500 ml) with distilled water (6.8).In the case of extreme foaming, the heat source should be reduced.IULTCS/IUC 25:2015(E) ISO 2015 All rights reserved 3BS EN ISO 17070:2015ISO 17070:2015(E)8.2 Liqu
48、id-liquid-extraction and acetylation8.2.1 Transfer 100 ml of the distillate obtained in 8.1 into a 250 ml separating funnel (5.7).8.2.2 Add 20 ml n-hexane (6.4), 0,5 ml triethylamine (6.9), and 1,5 ml acetic anhydride (6.6) to the solution and shake for 30 min on a mechanical shaker (5.4) with a sha
49、king rate of at least 200 shakes per min.CAUTION This step shall be carried out in a well-ventilated area or fume cupboard.NOTE The derivatization step is a two-phase reaction and depends very strongly on the intensity of shaking. Use a suitable mechanical shaker with a high shaking frequency (at least 200 cycles/min). Do not try to shake by hand because this will produce inconsistent results. Pressure compensation should be carried out before fixing the separating funnel (5.7) to the
