1、May 2012 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!$|0.“1891311www.din.deDDIN EN ISO 14088Leather Chemical tests Quantitative analysis of tanning agents by filter method(ISO 14088:2012)English translation of DIN EN ISO 14088:2012-05Leder Chemische Prfungen Quantitative Analyse von Gerbstoffen durch Filterverfahren (ISO 14088:2012)Englische b
3、ersetzung von DIN EN ISO 14088:2012-05Cuir Essais chimiques Analyse quantitative des agents de tannage par la mthode au filtre cloche(ISO 14088:2012)Traduction anglaise de DIN EN ISO 14088:2012-05www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document co
4、mprises 15 pages04.12 DIN EN ISO 14088:2012-05 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 289 “Leather” (Secretariat: UNI, Italy) in collaboration with IULTCS, the International Union of Leather Technologists and Chemists
5、Societies. The responsible German body involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-51 AA Anforderungen und physi-kalische Prfverfahren fr Leder und seine Ausgangsprodukte. The DIN Standard corresponding to th
6、e International Standard referred to in this document is as follows: ISO 3696 DIN ISO 3696 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14088 February 2012 ICS 59
7、.140.30 English Version Leather - Chemical tests - Quantitative analysis of tanning agents by filter method (ISO 14088:2012) Cuir - Essais chimiques - Analyse quantitative des agents de tannage par la mthode au filtre cloche Leder - Chemische Prfungen - Quantitative Analyse von Gerbstoffen durch Fil
8、terverfahren (ISO 14088:2012) This European Standard was approved by CEN on 31 January 2012. 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
9、 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, French, German). A version in any other language made by translation u
10、nder 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, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Franc
11、e, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitat
12、ion in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14088:2012: EEUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG (ISO 14088:2012) Contents Page Foreword . 3 1 Scope . 4 2 Normative references . 4 3 Princip
13、le . 4 4 Reagents 4 5 Apparatus . 4 6 Sampling and sample preparation 6 7 Instrumental analysis . 7 7.1 Preparation of the analytical solution . 7 7.1.1 Vegetable tanning agents in powder/solid form 7 7.1.2 Vegetable tanning agents in liquid form . 7 7.1.3 Synthetic tanning agents in powder form 7 7
14、.1.4 Synthetic tanning agents in liquid form . 7 7.1.5 Vegetable tanning agents organic solvent extracted in powder form 7 7.2 Preparation of the bell . 8 7.3 De-tanning the analytical solution (determination of the non-tanning agents) . 8 7.4 Determination of soluble substances . 8 7.5 Determinatio
15、n of total solids 9 8 Calculation and expression of the results . 9 9 Test report 10 Annex A (informative) Approximate quantity of vegetable tannic extract agent in powder/solid form to be weighed . 11 Annex B (normative) Determination of hide powder blank value . 12 Annex C (informative) Suppliers
16、of hide powder . 13 2DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) Foreword This document (EN ISO 14088:2012) 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 Tech
17、nologists and Chemists Societies”. 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 August 2012, and conflicting national standards shall be withdrawn at the latest by August 2012. Attention is dra
18、wn 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 Internal Regulations, the national standards organizations of the followi
19、ng countries are bound to implement this European Standard: 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, Slovaki
20、a, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. 3DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) 1 Scope This International Standard specifies a test method for the determination of tanning agents through filtration of all vegetable and synthetic tanning products. 2 Normative
21、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. ISO 3696, Water for analytical laborat
22、ory use Specification and test methods 3 Principle Indirect gravimetric analysis of vegetable and synthetic tanning agents through fixing of the absorbent compounds on low-chromed hide powder. 4 Reagents 4.1 Distilled water, freshly prepared according to ISO 3696 (Water for analytical laboratory use
23、, Grade 3). The pH value of the water shall be between 5 and 6. When using methyl red, the water should not turn red. The evaporation residue of 100 ml should be less than 1 mg. 4.2 Hide powder1), containing not more than 0,5 % chromium oxide and with a humidity not more than 13 %. The blank value o
24、f the hide powder shall be calculated according to Annex B. 4.3 Gelatine solution, of 1 g gelatine and 10 g sodium chloride, filled up to 100 ml with distilled water, adjusted to pH 4,7. 5 Apparatus The glass equipment shall be resistant to the action of distilled water. The flasks and tubes shall b
25、e Class A. Use normal laboratory equipment and, in particular, the following. 5.1 Desiccator, with an airtight cover and containing silica orange gel. 1) See Annex C. 4DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) 5.2 Evaporation dishes, suitable for slowly evaporating water. These shall be short w
26、ith flat bases and measure 7 cm to 8,5 cm in diameter. Use silver dishes. If this is not possible, preferably use dishes made of stainless steel or, if necessary, ceramic or glass. 5.3 Water bath. 5.4 Drying oven, whose temperature shall be kept at the operating range of (102 r 2) C. 5.5 Analytical
27、balance, with a precision of 0,2 mg at a load of 200 g. 5.6 Technical balance, with a precision of 0,1 g at a load of 1 000 g. 5.7 Procter bell (see Figure 1), composed of a cylindrical glass bell (length of the cylindrical part: 90 mm r 1 mm; internal diameter of the cylindrical part: 28 mm r 1 mm)
28、. A perforated rubber cork is inserted into the narrow part of the bell. A capillary glass tube (internal diameter 1,5 mm) with two right-angled bends is inserted into the hole in the cork as shown in Figure 1. The end of the shortest part can fit right down to the base of the cork. Dimensions in mi
29、llimetres Figure 1 Procter bell 5DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) 5.8 Polyethylene tube, the tube shall be the right size to fit onto the bells capillary glass tube. 5.9 Hoffman clamp. 5.10 1 000 ml volumetric flasks. 5.11 50 ml pipette. 5.12 Vacuum filter system (e.g. Figure 2). Figur
30、e 2 Vacuum filter system 5.13 Cellulose acetate membrane filters, with pores of 0,45 m and 3 m. 5.14 50 ml and 100 ml measuring cylinders. 6 Sampling and sample preparation There should be a generous, representative sample of the tanning agents for analysis; this should be thoroughly mixed. If the p
31、articles are heterogeneous, resort to manual or mechanical milling to homogenize the size of the particles. The particle size should not be smaller than 300 m to avoid blocking the Procter bell. 6DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) 7 Instrumental analysis 7.1 Preparation of the analytical
32、 solution 7.1.1 Vegetable tanning agents in powder/solid form Weigh the appropriate quantity (see Table A.1) of vegetable tanning agents on an analytical balance (5.5). Add this to 800 ml of hot (60 C to 80 C) distilled water in a 1 000 ml volumetric flask (5.10). Shake the flask to fully dissolve t
33、he tanning agents. There may be some residue if there is any insoluble matter in the sample. Leave it to cool down in a water bath at (20 r 2) C and add distilled water (4.1) up to the mark. The aim is to obtain an analytical solution containing between 3,75 g and 4,25 g of substances absorbed by th
34、e hide powder. If the tanning content in the solution goes beyond these limits, repeat the analysis with a sample of suitable quantity. 7.1.2 Vegetable tanning agents in liquid form Weigh the tanning agents on an analytical balance (5.5), taking into account the percentage of content in dry form. Ad
35、d this to in a 1 000 ml volumetric flask (5.10) containing 800 ml of hot (60 C to 80 C) distilled water. Shake the flask to fully dissolve the tanning agents. There may be some residue if there is any insoluble matter in the sample. Leave it to cool down in a water bath at (20 r 2) C and add distill
36、ed water (4.1) up to the mark. The aim is to obtain an analytical solution containing between 3,75 g and 4,25 g of substances absorbed in the hide powder. If the tanning content in the solution goes beyond these limits, repeat the analysis with a sample of suitable quantity. 7.1.3 Synthetic tanning
37、agents in powder form Weigh about (4 r 0,1) g of tanning agents on an analytical balance (5.5). Add this to a 1 000 ml volumetric flask (5.10) containing 800 ml of hot (40 C to 50 C) distilled water. Shake the flask to fully dissolve the tanning agents. There may be some residue if there is any inso
38、luble matter in the sample. Leave it to cool down in a water bath at (20 r 2) C and add distilled water (4.1) up to the mark. In the case of breakthrough of the tanning agent (see 7.3), repeat the analysis using a lower mass. Record this deviation in the test report. 7.1.4 Synthetic tanning agents i
39、n liquid form Weigh about (8 r 0,1) g of tanning agents on an analytical balance (5.5). Add it to a 1 000 ml volumetric flask (5.10) containing 800 ml of hot (40 C to 50 C) distilled water. Shake the flask to fully dissolve the tanning agents. There may be some residue if there is any insoluble matt
40、er in the sample. Leave it to cool down in a water bath at (20 r 2) C and add distilled water (4.1) up to the mark. In the case of breakthrough of the tanning agent (see 7.3), repeat the analysis using a lower mass. Record this deviation in the test report. 7.1.5 Vegetable tanning agents organic sol
41、vent extracted in powder form Weigh about (4 r 0,1) g of tanning agents on an analytical balance (5.5). Add this to a 1 000 ml volumetric flask (5.10) containing 800 ml of hot (40 C to 50 C) distilled water. Shake the flask to fully dissolve the tanning agents. There may be some residue if there is
42、any insoluble matter in the sample. Leave it to cool down in a water bath at (20 r 2) C and add distilled water (4.1) up to the mark. Select the amount in function of the quality of the extract desired. The final concentration of the analytical solution should contain about 4 g of tanning compound p
43、er litre. 7DIN EN ISO 14088:2012-05 EN ISO 14088:2012 (E) 7.2 Preparation of the bell Place a layer of cotton wool at the top of the bell to prevent the hide powder from entering the capillary tube. Put the rubber cork containing the glass capillary tube in the bell. Weigh 7,0 g of hide powder (4.2)
44、 on a technical balance (5.6) and introduce it uniformly in the bell, pressing it down, up to the top of the rim. Check that the hide powder is fully pressed down to ensure that it will be completely tanned. Put the polyethylene tube in the glass capillary tube and use the Hoffman clamp (5.9). 7.3 D
45、e-tanning the analytical solution (determination of the non-tanning agents) Place the bell containing hide powder in a beaker of suitable capacity. Fill the beaker with the unfiltered analytical solution up to the neck of the bell. When the hide powder is completely soaked, suck on the longer end of
46、 the capillary tube to create a slight depression and start siphoning the solution. Use the Hoffman clamp (5.9) to adjust the flow of the solution so that about 8 to 10 drops of the de-tanned solution drip through per minute. The resulting solution shall be clear. Collect a total of 90 ml in (120 r
47、10) min. The first 30 ml of the filtrate should be collected in a 50 ml glass measuring cylinder (5.14) and disposed of. The next 60 ml should be collected in a perfectly dry 100 ml glass measuring cylinder (5.14) to determine the non-tanning agents. To control the breakthrough of tanning agents use
48、 5 ml of the collected solution and add 0,5 ml gelatine solution (4.3). The pH of the total solution should be lower than 5. If necessary, use a few drops of formic acid to reduce the pH. A white precipitate is an indication of a breakthrough. In this case, repeat the analysis with a lower sample mass. The solution should be at a temperature no less than 18 C and no more than 20 C. Use the pipette (5.11) to transfer 50 ml of the filtered solution into a previously dried and weighed silver
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