1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 13365:2011Leather Chemical tests Determination of thepreservative (TCMTB, PCMC,OPP, OIT) content in leather byliquid chromatography (ISO13365:2011)BS EN ISO 13365:2011
2、BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO13365:2011.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can beobtained on request
3、 to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 68834 8ICS 59.140.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard
4、 was published under the authority of theStandards Policy and Strategy Committee on 31 January 2011.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 13365 January 2011 ICS 59.140.30 English Version Leather - Chemical tests - Determination
5、of the preservative (TCMTB, PCMC, OPP, OIT) content in leather by liquid chromatography (ISO 13365:2011) Cuir - Essais chimiques - Dosage des agents de conservation (TCMTB, PCMC, OPP, OIT) dans le cuir par chromatographie en phase liquid (ISO 13365:2011) Leder - Chemische Prfungen - Bestimmung von K
6、onservierungsmitteln (TCMTB, CMK, OPP, OIT) in Leder mittels Flssigchromatographie (ISO 13365:2011) This European Standard was approved by CEN on 14 January 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standar
7、d 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 (English,
8、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, Bulga
9、ria, Croatia, Cyprus, Czech 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
10、STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 13365:2011: EBS EN ISO 13365:2011EN ISO 133
11、65:2011 (E) 3 Foreword This document (EN ISO 13365:2011) has been prepared by Technical Committee CEN/TC 289 “Leather“, the secretariat of which is held by UNI, in collaboration with Technical Committee IULTCS “International Union of Leather Technologists and Chemists Societies”. This European Stand
12、ard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by July 2011, and conflicting national standards shall be withdrawn at the latest by July 2011. Attention is drawn to the possibility that some of the elements of this do
13、cument may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard
14、: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech 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 the United Kin
15、gdom. BS EN ISO 13365:2011ISO 13365:2011(E) IULTCS/IUC 29:2011(E) ISO 2011 All rights reserved iiiForeword 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 ca
16、rried 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, also take part in the work
17、. 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 technical committees is to prepare Intern
18、ational 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 to the possibility that some of the
19、 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 13365 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with the Chemical Test
20、 Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, IULTCS), in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement). This method is technically similar to the method in IUC 29. IULTCS, originally formed in
21、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 IULTCS as an internati
22、onal standardizing body for the preparation of test methods for leather. BS EN ISO 13365:2011BS EN ISO 13365:2011INTERNATIONAL STANDARD ISO 13365:2011(E)IULTCS/IUC 29:2011(E) ISO 2011 All rights reserved 1Leather Chemical tests Determination of the preservative (TCMTB, PCMC, OPP, OIT) content in lea
23、ther by liquid chromatography 1 Scope This International Standard specifies a test method for the determination of the content of the following preservative agents: 2-(thiocyanomethylthio)-benzothiazole (TCMTB); 4-chloro-3-methylphenol (PCMC); 2-phenylphenol (OPP); 2-octylisothiazol-3(2H)-one (OIT);
24、 in leather by liquid chromatography. Preservative agents are necessary to protect leather from microbiological attack. NOTE The preservative agents 4-chloro-3-methylphenol (PCMC) and 2-phenylphenol (OPP) can also be determined according to ISO 17070 and quantified by means of gas chromatography/mas
25、s spectroscopy (GC/MS). 2 Normative references The following 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. IS
26、O 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location ISO 4044, Leather Chemical tests Preparation of chemical test samples ISO 4684, Leather Chemical tests Determination of volatile matter 3 Principle The leather sample is extracted with a suitable solvent using ult
27、rasonic waves. The filtered extract is analysed by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection. 4 Reagents 4.1 TCMTB, minimum 99,7 %. 4.2 TCMTB stock solution, 500 mg/l in acetonitrile. BS EN ISO 13365:2011ISO 13365:2011(E) IULTCS/IUC 29:2011(E) 2 ISO 2011 All right
28、s reserved4.3 PCMC, minimum 99,5 %. 4.4 PCMC stock solution, 500 mg/l in acetonitrile. 4.5 OPP, minimum 99,5 %. 4.6 OPP stock solution, 500 mg/l in acetonitrile. 4.7 OIT, minimum 97,0 %. 4.8 OIT stock solution, 500 mg/l in acetonitrile. 4.9 Acetonitrile, HPLC grade. 4.10 Water, HPLC grade. 5 Apparat
29、us and materials Usual laboratory apparatus is required and, in particular, the following. 5.1 Analytical balance, weighing to an accuracy of 0,1 mg. 5.2 HPLC system, with UV detection or other suitable detectors. 5.3 Separation column, reversed phase C8 or C18 with corresponding pre-column. 5.4 Ult
30、rasonic bath, e.g. 40 kHz. 5.5 Membrane filter, polyamide, 0,45 m. 6 Procedure 6.1 Sampling and sample preparation If possible, sample in accordance with ISO 2418 and grind in accordance with ISO 4044. If sampling in accordance with ISO 2418 is not possible (e.g. leathers from finished products, suc
31、h as shoes or garments), details of the sampling shall be given, together with the test report. Wet intermediates like wet blue and wet white shall be dried as described in ISO 4044 prior to grinding. 6.2 Preparation of analytical solution Weigh (1 0,01) g of ground leather to the nearest 0,001 g in
32、 a 100 ml conical flask. Pipette 20 ml of acetonitrile (4.9) and add it to the leather. The leather sample is extracted in an ultrasonic bath (5.4) for 1 h 5 min (80 % ultrasound power) at room temperature. During extraction, the temperature in the mixture increases to about 35 C. Subsequently, a pa
33、rt of the extract is filtered through a membrane filter (5.5) into a suitable vial. The filtrate is analysed by HPLC (5.2) and detected preservatives are quantified. BS EN ISO 13365:2011ISO 13365:2011(E) IULTCS/IUC 29:2011(E) ISO 2011 All rights reserved 36.3 Chromatographic conditions Proposal: Sep
34、aration column: reversed-phase (RP) column (C18 HD, 250 mm/4 mm, 100 , 5 m) with pre-column Flow rate: 0,8 ml/min Mobile phase: A: water, B: acetonitrile Gradient: 60 % B for 6 min isocratic, then linear to 95 % B in 9 min Column oven: 30 C UV detection: 275 nm Injection volume: 20 l 6.4 Calibration
35、 Calibration is carried out by means of an external standard. Prepare adequate dilutions (in acetonitrile) of preservative stock solutions (4.2, 4.4, 4.6 and 4.8). Calibration shall be done using at least six concentration levels. The calibration is effected by plotting a graph of the preservative p
36、eak area versus its concentration, in micrograms per millilitre (g/ml). As very different preservative concentrations can be expected, it is not possible to cover the whole range with a single calibration curve. 7 Calculation Calculate the mass fraction, wi, of every preservative detected, in millig
37、rams per kilogram (mg/kg) of leather, using the following equation: i10001000VFwm=where wiis the mass fraction, expressed in milligrams per kilogram (mg/kg), of a certain preservative in leather; is the mass concentration of preservative obtained from the calibration, in micrograms per millilitre (g
38、/ml); V is the extract volume, in millilitres (ml); F is the dilution factor; m is the quantity of sample weighed, in grams (g). The mass fraction of each preservative is given in milligrams per kilogram (mg/kg), rounded to the nearest 0,1 mg. BS EN ISO 13365:2011ISO 13365:2011(E) IULTCS/IUC 29:2011
39、(E) 4 ISO 2011 All rights reservedThe mass fraction of preservative referred to dry matter, according to ISO 4684, can be calculated using the following equation: dmwwD= where wdmis the mass fraction of preservative, expressed in milligrams per kilogram (mg/kg), of sample referred to dry matter; w i
40、s the mass fraction of preservative, expressed in milligrams per kilogram (mg/kg), of the sample being tested; D is the recalculation factor for dry matter v100100Dw=wvis the mass fraction of volatile matter, based on ISO 4684, expressed as a percentage. 8 Test report The test report shall include t
41、he following information: a) a reference to this International Standard, i.e. ISO 13365:2011; b) the type, origin and designation of the analysed product and the sampling method used; c) the type of liquid chromatography detection; d) the analytical result for each mass fraction of preservative, in
42、milligrams per kilogram (mg/kg) rounded to one decimal place; e) any deviation from the analytical procedure. BS EN ISO 13365:2011ISO 13365:2011(E) IULTCS/IUC 29:2011(E) ISO 2011 All rights reserved 5Bibliography 1 ISO 17070, Leather Chemical tests Determination of pentachlorophenol content This pag
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