DIN EN ISO 17489-2014 Leather - Chemical tests - Determination of tan content in synthetic tanning agents (ISO 17489 2013) German version EN ISO 17489 2013《皮革 化学试验 合成鞣剂中鞣含量的测定 (ISO.pdf

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1、March 2014 Translation by DIN-Sprachendienst.English price group 8No 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 5

2、9.140.30!%,-“2099310www.din.deDDIN EN ISO 17489Leather Chemical tests Determination of tan content in synthetic tanning agents(ISO 17489:2013);English version EN ISO 17489:2013,English translation of DIN EN ISO 17489:2014-03Leder Chemische Prfungen Bestimmung des Gerbanteils in Gerbstoffen (ISO 1748

3、9:2013);Englische Fassung EN ISO 17489:2013,Englische bersetzung von DIN EN ISO 17489:2014-03Cuir Essais chimiques Dtermination de la teneur en tanin dans les agents de tannage synthtiques(ISO 17489:2013);Version anglaise EN ISO 17489:2013,Traduction anglaise de DIN EN ISO 17489:2014-03www.beuth.deD

4、ocument comprises 12 pagesIn case of doubt, the German-language original shall be considered authoritative.02.14 DIN EN ISO 17489:2014-03 2 A comma is used as the decimal marker. National foreword This document (EN ISO 17489:2013) has been prepared by Technical Committee CEN/TC 289 “Leather” (Secret

5、ariat: UNI, Italy) in collaboration with the International Union of Leather Technologists and Chemists Societies (IULTCS). The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-52 AA Chemisc

6、he Prfverfahren fr Leder. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 3696 DIN ISO 3696 ISO 14088 DIN EN ISO 14088 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test

7、 methods DIN EN ISO 14088, Leather Chemical tests Quantitative analysis of tanning agents by filter method EUROPEAN 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 1

8、7489:2013) Cuir Essais 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 comp

9、ly 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 standards may be obtained on application to the CEN-CENELEC

10、 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 notified to the CEN-CENELEC Management Centre has the sa

11、me 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg

12、, 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 Management Centre: Avenue Marnix 17, B-1000 Brussels 20

13、13 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17489:2013 E Contents PageForeword 3Introduction 41 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 55 Reagents 56 Apparatus . 57 Procedure. 67.1 Prepar

14、ation of the synthetic tanning agent solution for analysis . 67.2 Determination of the total residual dry content (duplicate determination) .6 67.3 Determination of the non-tanning agent content (i.e. non-adsorbable fraction) 78 Calculation and expression of results . 79 Test report . 7Annex A (info

15、rmative) Interlaboratory trial results for the determination of the tan content 8Annex B (informative) Sources of chemicals 9Bibliography 10DIN EN ISO 17489:2014-03 EN ISO 17489:2013 (E) 266Foreword This document (EN ISO 17489:2013) has been prepared by IULTCS “International Union of Leather Technol

16、ogists 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 publication of an identical text or by endorsement, at the latest by May 2014, and

17、conflicting national 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

18、 to the CEN-CENELEC 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, Gre

19、ece, Hungary, Iceland, 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 with

20、out any modification. ”DIN EN ISO 17489:2014-03 EN ISO 17489:2013 (E) 3IntroductionThe 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 agent that is adsorbed

21、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 component in the tanni

22、ng 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 cartridges. In addition,

23、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 for removing polyph

24、enolic 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 and precision of re

25、peat 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 adsorbing substrate.DIN EN

26、ISO 17489:2014-03 EN ISO 17489:2013 (E) 41 ScopeThis International Standard specifies a simple and practical method of determining the adsorbable fraction of synthetic tanning agents using a polymer-based product. It is particularly suitable for measuring the batch-to-batch consistency of synthetic

27、tanning agents.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 references, the latest edition of the referenced document (inclu

28、ding any amendments) applies.ISO 3696:1987, Water for analytical laboratory use Specification and test methods3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1tan contentadsorbable fraction of a synthetic tanning agent when mixed in a water solut

29、ion with a crosslinked, insoluble vinylimidazole/ vinylpyrrolidone copolymer product4 PrincipleAn acidified synthetic tanning agent solution and an insoluble copolymer product are mixed at room temperature. The insoluble copolymer absorbs polyphenols from the tanning agent. The dry content of the so

30、lution before and after mixing with the absorbing copolymer are measured. The difference is the adsorbable fraction, called the tan content.5 Reagents5.1 Crosslinked, insoluble vinylimidazole/vinylpyrrolidone copolymer (see Annex B).5.2 Formic acid solution, a mass fraction of 50 %.5.3 Gelatine, pur

31、e, 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 and the following items:DIN EN ISO 17489:2014-03 EN ISO 17489:2013 (E) 56.1 Analytical balance, accurate to 0,1 mg.6.2 Drying oven, ventilate

32、d, capable of maintaining a temperature of 105 C 2 C.6.3 Magnetic stirrer.6.4 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 si

33、ze or a suitable analytical grade filter paper.6.8 Glass beakers, 1 000 ml and 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

34、tanning agents: accurately weigh 1,3000 g to 1,7000 g of the powder and record 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

35、water (5.5) at room temperature.Stir so that the synthetic tanning agent is dissolved, 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 t

36、he mark with deionised or distilled water (5.5). This is the tanning solution 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, d

37、ry stainless steel dish (6.5). With an analytical 50 ml pipette (6.10), add 50 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 ap

38、proximately 2 h in a desiccator (6.6) with a drying agent, for example, either calcium chloride (CaCl2) or silica gel. Weigh the dish (P1).The % dry content is calculated as follows:% dry content = ()PTm1110 100DIN EN ISO 17489:2014-03 EN ISO 17489:2013 (E) 67.3 Determination of the non-tanning agen

39、t content (i.e. non-adsorbable fraction)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 u

40、pper aqueous phase is not clear, it can 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 approx

41、imately 130 ml of filtrate is needed.7.3.2 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

42、the filtrate (7.3.1), add approximately 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/vinylpyrr

43、olidone 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 the water carefully on a suitable

44、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 calcium chloride (CaCl2) or silica gel. Weigh the dish (P2).The non-tanning agent content is calcu

45、lated as follows:% Non-tanning agent content = ()PTm2210 1008 Calculation and expression of results8.1 Calculate the tan content (i.e. the adsorbable fraction) as follows:% tan content = (% dry content) (% non-tanning agent content) 8.2 Make two determinations per synthetic tanning agent sample. For

46、 the final result, calculate the mean value from the two single results. If the difference in the two results for % tan content exceeds 0,5 %, repeat the determination.9 Test reportThe test report shall include the following:a) reference to this International Standard (i.e. ISO 17489);b) a descripti

47、on of the synthetic tanning agent sample tested;c) the % tan content result obtained (average of two determinations, to one decimal place in %);d) any deviations from the procedure specified in this International Standard.DIN EN ISO 17489:2014-03 EN ISO 17489:2013 (E) 7Annex A (informative) Interlab

48、oratory trial results for the determination of the tan contentA series of seven different synthetic tanning agents were analysed by six laboratories in an interlaboratory trial in 1997, see Reference 2 in the Bibliography for full details.Table A.1 Interlaboratory trial Results for adsorbable fractionSynthetic tanning agentLab 1(%)Lab 2(%)Lab 3(%)Lab 4(%)Lab 5(%)Lab 6(%)Mean value(%)A 72,9 0,5 74,1 0,6 75,6 2,1 68,4 2,3 72,6 0,9 73,7 0,3 72,9B 59,0 0,3 61,1 2,