DIN EN ISO 17070-2015 Leather - Chemical tests - Determination of tetrachlorophenol- trichlorophenol- dichlorophenol- monochlorophenol-isomers and pentachlorophenol content (ISO 17.pdf

1、May 2015 Translation by DIN-Sprachendienst.English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 59

2、.140.30!%Bj+“2317108www.din.deDDIN EN ISO 17070Leather Chemical tests Determination of tetrachlorophenol-, trichlorophenol-, dichlorophenol-,monochlorophenol-isomers and pentachlorophenol content(ISO 17070:2015);English version EN ISO 17070:2015,English translation of DIN EN ISO 17070:2015-05Leder C

3、hemische Prfungen Bestimmung des Gehalts an Tetrachlorphenol-, Trichlorphenol-, Dichlorphenol-,Monochlorphenol-Isomeren und Pentachlorphenol (ISO 17070:2015);Englische Fassung EN ISO 17070:2015,Englische bersetzung von DIN EN ISO 17070:2015-05Cuir Essais chimiques Dtermination de la teneur en isomre

4、s de monochlorophnol, dichlorophnol,trichlorophnol, ttrachlorophnol et en pentachlorophnol (ISO 17070:2015);Version anglaise EN ISO 17070:2015,Traduction anglaise de DIN EN ISO 17070:2015-05SupersedesDIN EN ISO 17070:2007-01www.beuth.deDocument comprises 16 pagesIn case of doubt, the German-language

5、 original shall be considered authoritative.05.15 DIN EN ISO 17070:2015-05 2 A comma is used as the decimal marker. National foreword This document (EN ISO 17070:2015) has been prepared by “International Union of Leather Technologists and Chemists Societies (IULTCS)” in collaboration with the Techni

6、cal Committee CEN/TC 289 “Leather” (Secretariat: UNI, Italy). The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-51 AA Anforderungen und physikalische Prfverfahren fr Leder und se

7、ine Ausgangsprodukte. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 2418 DIN EN ISO 2418 ISO 3696 DIN ISO 3696 ISO 4044 DIN EN ISO 4044 ISO 4684 DIN EN ISO 4684 Amendments This standard differs from DIN EN ISO 17070:2007-01 as follows

8、: a) the additional chlorinated phenol substances tetrachlorophenol-, trichlorophenol-, dichlorophenol-, and monochlorophenol-isomers have been included; b) a new Clause 3 has been included to list the chlorophenol abbreviations; c) the examples of chromatographic conditions, previously in 7.4, have

9、 been moved to a new Annex A. The former Annex A is now Annex B; d) the standard has been editorially revised. Previous editions DIN 53313: 1996-02 DIN CEN/TS 14494: 2003-08 DIN EN ISO 17070: 2007-01 DIN EN ISO 17070:2015-05 3 National Annex NA (informative) Bibliography DIN EN ISO 2418, Leather Che

10、mical, physical and mechanical and fastness tests Sampling location DIN EN ISO 4044, Leather Chemical tests Preparation of chemical test samples DIN EN ISO 4684, Leather Chemical tests Determination of volatile matter DIN ISO 3696, Water for analytical laboratory use Specification and test methods D

11、IN EN ISO 17070:2015-05 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17070 February 2015 ICS 59.140.30 Supersedes EN ISO 17070:2006English Version Leather - Chemical tests - Determination of tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochl

12、orophenol-isomers and pentachlorophenol content (ISO 17070:2015) Cuir - Essais chimiques - Dtermination de la teneur en isomres de monochlorophnol, dichlorophnol, trichlorophnol, ttrachlorophnol et en pentachlorophnol (ISO 17070:2015) Leder - Chemische Prfungen - Bestimmung des Gehalts an Tetrachlor

13、phenol-, Thrichlorphenol-, Dichlorphenol-, Monochlorphenol-Isomeren und Pentachlorphenol(ISO 17070:2015) This European Standard was approved 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 Sta

14、ndard 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 three official versions (Engli

15、sh, 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 bodies of Austria, Belgium, B

16、ulgaria, 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,

17、 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 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membe

18、rs. Ref. No. EN ISO 17070:2015 EContents PageForeword 3Introduction 41 Scope . 52 Normative references 53 Abbreviations. 54 Principle 55 Apparatus . 66 Reagents 66.1 Chlorinated phenol mix .67 Sampling and preparation of samples . 78 Procedure. 78.1 Steam-distillation 78.2 Liquid-liquid-extraction a

19、nd acetylation 88.3 Preparation of calibration mixture for acetylated CP and TCG . 88.4 Gas chromatography (GC) . 99 Expression of results 910 Test report . 9Annex A (informative) Chromatographic analyses . 10Annex B (informative) Reliability of the method 12DIN EN ISO 17070:2015-05 EN ISO 17070:201

20、5 (E) 2 Foreword This document (EN ISO 17070:2015) has been prepared by Technical 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 Standa

21、rd shall be given the status of a national standard, either by publication 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

22、 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 EN ISO 17070:2006. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countrie

23、s 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, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland

24、, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey 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. DIN EN ISO 17070:2015-05 EN ISO 17070:2015 (E) 3 IntroductionThis International St

25、andard describes a procedure where the chlorinated phenols (CP) are acetylated before the chromatographic detection and the amount of the detected chlorinated phenyl acetate is quantified via an internal standard correction.DIN EN ISO 17070:2015-05 EN ISO 17070:2015 (E) 4 1 ScopeThis International S

26、tandard specifies a method for determining the content of tetrachlorophenol-, trichlorophenol-, dichlorophenol-, monochlorophenol-isomers, and pentachlorophenol, its salts, and esters in leather.NOTE Bromophenol isomers can also be determined using this method.2 Normative referencesThe following doc

27、uments, 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 references, the latest edition of the referenced document (including any amendments) applies.ISO 2418, Leather Chemica

28、l, physical and mechanical and fastness tests Sampling locationISO 3696, Water for analytical laboratory use Specification and test methodsISO 4044, Leather Chemical tests Preparation of chemical test samplesISO 4684, Leather Chemical tests Determination of volatile matter3 AbbreviationsThe followin

29、g abbreviations are used for chlorinated phenols in this International Standard:CP chlorinated phenolsDiCP dichlorophenolMoCP monochlorophenolPCP pentachlorophenolTCG tetrachloroguaiacol (tetrachloro-o-methoxyphenol)TeCP tetrachlorophenolTriCP trichlorophenol4 PrincipleFirst of all, the leather samp

30、le 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 by gas-chromatography with an electron capture detector (ECD) or mass selective detector (MSD). Quantification is per

31、formed by an external standard and a correction made with an internal standard.DIN EN ISO 17070:2015-05 EN ISO 17070:2015 (E) 5 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 distill

32、ation.5.4 Shaking machine, capable of at least 200 cycles per minute.5.5 Volumetric flasks, 500 ml and 50 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 Past

33、eur-pipettes, graduated pipettes, suitable auto-pipettes.5.9 Strainer with paper filter, grade 4, diameter 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 mi

34、x of the chlorinated phenols which contains the following isomers at a concentration of 100 g/ml in acetone.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

35、 CAS-Number: 5837882,6-Dichlorophenol CAS-Number: 876503,4-Dichlorophenol CAS-Number: 957723,5-Dichlorophenol 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.DIN EN ISO 17070

36、:2015-05 EN ISO 17070:2015 (E) 6 2,4,5-Trichlorophenol CAS-Number: 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

37、 CAS-Number: 87865NOTE This chlorinated phenol mix is available from 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 res

38、idue analysis.6.5 Potassium carbonate, K2CO3.6.6 Acetic anhydride, 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 sam

39、ple into small pieces or grind the leather in accordance with ISO 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 toget

40、her with the test report.8 Procedure8.1 Steam-distillationAccurately 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 us

41、ing a suitable steam distillation apparatus. Use a 500 ml volumetric 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.DIN EN ISO 17070:2015-05 EN ISO

42、 17070:2015 (E) 7 8.2 Liquid-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 mechanic

43、al shaker (5.4) with a shaking 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 hig

44、h 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 mechanical shaker (5.4).8.2.3 After phase separation, transfer the organic layer to

45、a 100 ml conical flask (5.6) and shake the aqueous layer for a further 30 min with an additional 20 ml of n-hexane.8.2.4 Dehydrate the combined n-hexane extracts by adding anhydrous sodium sulfate (6.7) to the flask (5.6) and leaving to stand for approximately 10 min.8.2.5 Filter (5.9) the n-hexane

46、extract quantitatively, washing with n-hexane into a 50 ml volumetric flask (5.5).8.2.6 Make up to volume (50 ml) with n-hexane.8.2.7 Analyse this solution by one of the gas chromatographic methods (5.1).8.3 Preparation of calibration mixture for acetylated CP and TCG8.3.1 Derivatization of chlorinated phenol mix and TCG standard for recovery rateTo calculate the recovery, prepare a CP/TCG standard mixture like the sample.Measure 100 l of the chlorinated phenol mix solution (6.1) and 100 l TCG (6.2) into the distillation vessel together with 20 ml sulfuric acid (6.3). Treat th