1、BSI Standards PublicationBS EN ISO 17489:2013Leather Chemical tests Determination of tan contentin synthetic tanning agents(ISO 17489:2013)BS EN ISO 17489:2013 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO17489:2013.The UK participation in its preparation
2、was entrusted to TechnicalCommittee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its corr
3、ectapplication. The British Standards Institution 2013. Published by BSI StandardsLimited 2013ISBN 978 0 580 77303 7ICS 59.140.30Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy
4、 Committee on 30 November 2013.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 17489 November 2013 ICS 59.140.30 English Version Leather - Chemical tests - Determination of tan content in synthetic tanning agents (ISO 17489:2013) Cuir - E
5、ssais chimiques - Dtermination de la teneur en tanin dans les agents de tannage synthtiques (ISO 17489:2013) Leder - Chemische Prfungen - Bestimmung des Gerbanteils in Gerbstoffen (ISO 17489:2013) This European Standard was approved by CEN on 12 October 2013. CEN members are bound to comply with the
6、 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 standards may be obtained on application to the CEN-CENELEC Management
7、 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 notified to the CEN-CENELEC Management Centre has the same status a
8、s 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Ne
9、therlands, 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 Management Centre: Avenue Marnix 17, B-1000 Brussels 2013 CEN All
10、rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17489:2013 EBS EN ISO 17489:2013EN ISO 17489:2013 (E) 3 Foreword This document (EN ISO 17489:2013) has been prepared by IULTCS “International Union of Leather Technologists and Chemists S
11、ocieties“ 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 publication of an identical text or by endorsement, at the latest by May 2014, and conflicting national
12、 standards shall be withdrawn at the latest by May 2014. 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. According to the CEN-CENELEC
13、Internal Regulations, the national standards organizations of the following countries 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, Icelan
14、d, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 17489:2013 has been approved by CEN as EN ISO 17489:2013 without any modification
15、. BS EN ISO 17489:2013ISO 17489:2013(E)IULTCS/IUC 33:2013(E) ISO 2013 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Reagents 16 Apparatus . 17 Procedure. 27.1 Preparation of the synthetic tanning agent soluti
16、on for analysis . 27.2 Determination of the total residual dry content (duplicate determination) . 27.3 Determination of the non-tanning agent content (i.e. non-adsorbable fraction) 38 Calculation and expression of results . 39 Test report . 3Annex A (informative) Interlaboratory trial results for t
17、he determination of the tan content 4Annex B (informative) Sources of chemicals 5Bibliography 6BS EN ISO 17489:2013ISO 17489:2013(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Inter
18、national 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 wit
19、h 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 for its further maintenance are described in the ISO/IEC Directives,
20、 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.org/directives). Attention is drawn to the possibility that some of
21、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 be in the Introduction and/or on the ISO list of patent declarations
22、 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 related to conformity assessment, as well as information about IS
23、Os adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationISO 17489 was prepared by the European Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with the Chemical Tests Commissi
24、on 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).IULTCS, originally formed in 1897, is a worldwide organization of professional leather societies to
25、 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 preparation of test methods for leather
26、.IULTCS/IUC 33:2013(E)iv ISO 2013 All rights reservedBS EN ISO 17489:2013ISO 17489:2013(E)IntroductionThe ISO Standard, ISO 14088, is the traditional method for analysing the tanning component in a tanning agent. It uses chromium (III) tanned hide powder and determines the proportion of tanning agen
27、t that is adsorbed onto the hide powder. The non-adsorbable fraction, consisting largely of inorganic salts, remains in the tanning solution. By determining the dry content of the initial tanning solution and the non-adsorbable fraction, one calculates the adsorbable fraction this is the tanning com
28、ponent in the tanning agent.In this manner, the traditional hide powder method is used to determine the tanning strength of tanning agents. However, for reproducible test results this method requires considerable expertise from the operator in the preparation and packing of hide powder filter cartri
29、dges. In addition, the time for the filtration can be very long and the method is not suitable when results are needed in a short period of time, such as during the production quality control when manufacturing synthetic tanning agents.The co-polymers of vinylimidazole and vinylpyrrolidone are used
30、for removing polyphenolic compounds and metals from wine. This polymer-based powder offers a simple and practical alternative to hide powder for the routine testing of synthetic tanning agents, such as in a manufacturing facility. Interlaboratory trials (given in Table A.1) show the reproducibility
31、and precision of repeat testing is better for the polymer-based powder.The two procedures, ISO 14088 and ISO 17489, use different adsorbing substrates; consequently, the value for the adsorbable fraction will be different and the results obtained can only be compared when made with the same adsorbin
32、g substrate.IULTCS/IUC 33:2013(E) ISO 2013 All rights reserved vBS EN ISO 17489:2013BS EN ISO 17489:2013Leather Chemical tests Determination of tan content in synthetic tanning agents1 ScopeThis International Standard specifies a simple and practical method of determining the adsorbable fraction of
33、synthetic tanning agents using a polymer-based product. It is particularly suitable for measuring the batch-to-batch consistency of synthetic tanning agents.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its a
34、pplication. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 3696:1987, Water for analytical laboratory use Specification and test methods3 Terms and definitionsFor the purposes of this
35、document, the following terms and definitions apply.3.1tan contentadsorbable fraction of a synthetic tanning agent when mixed in a water solution with a crosslinked, insoluble vinylimidazole/ vinylpyrrolidone copolymer product4 PrincipleAn acidified synthetic tanning agent solution and an insoluble
36、copolymer product are mixed at room temperature. The insoluble copolymer absorbs polyphenols from the tanning agent. The dry content of the solution before and after mixing with the absorbing copolymer are measured. The difference is the adsorbable fraction, called the tan content.5 Reagents5.1 Cros
37、slinked, insoluble vinylimidazole/vinylpyrrolidone copolymer (see Annex B).5.2 Formic acid solution, a mass fraction of 50 %.5.3 Gelatine, pure, AR grade.5.4 Sodium chloride, AR grade.5.5 Deionised or distilled water, in compliance with grade 3 in ISO 3696:1987.6 ApparatusNormal laboratory equipment
38、 and the following items:INTERNATIONAL STANDARDISO 17489:2013(E)IULTCS/IUC 33:2013(E) ISO 2013 All rights reserved 1BS EN ISO 17489:2013ISO 17489:2013(E)6.1 Analytical balance, accurate to 0,1 mg.6.2 Drying oven, ventilated, capable of maintaining a temperature of 105 C 2 C.6.3 Magnetic stirrer.6.4
39、pH meter with suitable combination electrode.6.5 Stainless steel, (e.g. AISI 316), or aluminium dishes for evaporating aqueous solutions.6.6 Dessicator, with drying agent.6.7 Membrane filter, 50 mm diameter, 0,45 m pore size or a suitable analytical grade filter paper.6.8 Glass beakers, 1 000 ml and
40、 600 ml.6.9 Volumetric flasks, 500 ml.6.10 Pipette, 50 ml, analytical grade.7 Procedure7.1 Preparation of the synthetic tanning agent solution for analysisIn a 1 000 ml beaker (6.8), add the following.For powder synthetic tanning agents: accurately weigh 1,3000 g to 1,7000 g of the powder and record
41、 the mass (m); add approximately 400 ml of warm deionised water (5.5).For liquid synthetic tanning agents: accurately weigh 2,7000 g to 3,3000 g of the liquid and record the mass (m); add approximately 400 ml of deionised water (5.5) at room temperature.Stir so that the synthetic tanning agent is di
42、ssolved, cool the solution to 23 C 1 C. While stirring, bring the pH to 2,0 to 2,3 by adding dropwise a 50 % formic acid solution (5.2). Transfer the solution quantitatively to a 500 ml volumetric flask (6.9) and fill to the mark with deionised or distilled water (5.5). This is the tanning solution
43、to be used for the following test steps.Prepare duplicate tanning solutions for each synthetic tanning agent to be tested.7.2 Determination of the total residual dry content (duplicate determination)Weigh (T1) the clean, dry stainless steel dish (6.5). With an analytical 50 ml pipette (6.10), add 50
44、 ml of the tanning solution into the dish and evaporate most of the water carefully on a suitable hotplate or water bath. Place the dish in an oven at 105 C 2 C until constant mass is reached. Allow the dish to cool for approximately 2 h in a desiccator (6.6) with a drying agent, for example, either
45、 calcium chloride (CaCl2) or silica gel. Weigh the dish (P1).The % dry content is calculated as follows:% dry content = ()PTm1110 100IULTCS/IUC 33:2013(E)2 ISO 2013 All rights reservedBS EN ISO 17489:2013ISO 17489:2013(E)7.3 Determination of the non-tanning agent content (i.e. non-adsorbable fractio
46、n)7.3.1 In a 600 ml beaker, add the following: 40,0 g 0,1 g insoluble vinylimidazole/vinylpyrrolidone copolymer powder (5.1); 300 g 1 g of the tanning solution.Stir the suspension for approximately 30 min and leave it to settle for approximately 90 min. If the upper aqueous phase is not clear, it ca
47、n be centrifuged for 15 min at approximately 3 000 rpm. Decant the upper aqueous phase through a 0,45 m membrane filter (6.7) or a suitable analytical grade filter paper if no membrane filter is available. Keep the filtrate, to make a double determination approximately 130 ml of filtrate is needed.7
48、.3.2 To check the absence of tanning agent in the filtrate (7.3.1), prepare a gelatine solution by dissolving approximately 10 g gelatine (5.3) and approximately 100 g NaCl (5.4) in 1 000 ml deionised or distilled water (5.5). To an approximately 5 ml sample of the filtrate (7.3.1), add approximatel
49、y 2 ml of the gelatine solution. The test solution must remain clear. If precipitation or cloudiness occurs, then there is still residual tanning agent in the filtrate. Repeat the procedure in 7.3.1 using a larger amount of the insoluble vinylimidazole/vinylpyrrolidone copolymer powder (5.1) until the test solution is clear.7.3.3 Carry out this section in duplicate. Weigh the clean, dry stainless steel dish (T2). With an analytical 50 ml pipette (6.10), add 50 ml of the tanning solution into the dish and evaporate most of
