EN ISO 4047-1998 en Leather - Determination of Sulphated Total Ash and Sulphated Water-Insoluble Ash《皮革 硫酸盐总灰分和硫酸盐水不溶物灰分的测定 ISO 4047-1977》.pdf

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1、- STD.BS1 BS EN IS0 40Li7-ENGL 2978 lb24bb9 0738088 950 = BRITISH STANDARD Leather - Determination of sulphated total ash and sulphated water-insoluble ash * m * The European Standard EN Is0 40471998 has the status of a British Standard ICs 59.140.30 BS EN IS0 4047:1998 NO COPYING WITHOUT BSI PERMIS

2、SION EXCEPT AS PERMITTED BY COPYRIGHT LAW STD-BSI BS EN IS0 Li01i7-ENGL L998 Lb24bb7 0738087 897 been prepared under the direction of the Sector Committee for Materiais and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 1998 Amd. No. O BS

3、I 1998 ISBN O 680 30781 6 BS EN IS0 4047:1998 Date Text affected National foreword This British Standard is the English language version of EN IS0 40471998. It is identical with IS0 4047 1977. It supersedes BS 1309 1974, clause 6, which is withdrawn by amendment. The UK participation in its preparat

4、ion was entrusted to Technical Committee TCV69, Footwear and leather, which has the responsibility to: - aid enquirers to understand the text; - present to the responsible intemational/European committee any enquiries on the interpretaion, or proposals for change, and keep the UK interests informed

5、- monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC standards normaily include an annex which l

6、ists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Stan

7、dards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include aii the necessary provisions of a contract Users of British Standards are responsible for their correct application. Compliance with a British Standa

8、rd does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 titie page, the IS0 foreword page, pages 1 and 2, an inside back cover and a back cover. STD.BS1 BS EN

9、 IS0 qOq-ENGL 1998 Lb24bb 0738090 509 EUROPEAN STANDARD EN IS0 4047 NORME EUROPENNE EUROPISCHE NORM September 1998 ICs 59.140.30 Descriptors: see IS0 document English version Leather - Determination of sulphated total ash and sulphated water-insoluble ash (IS0 4047: 1977) Cuir - Dosage des cendres s

10、ulfatbs totales et des cendres sulfaths insolubles dans leau (IS0 447:1977) Leder - Bestimmung der sulfatierten Gesamtasche und der sulfatierten wasserunlslkhen Asctte (IC0 4047:1977) This European Standard was approved by CEN on 9 August 1998. CEN members are bound to comply with the CEWCENELEC Int

11、emal 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 Central Secretariat or to any CEN membe

12、r. 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 Central Secretariat has the same status as the official versions. CEN members

13、are the national standards bodies of Austria, Belgium, Czech Repubiic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland. Italy, Luxembourg. Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMEE FOR STANDARDIZATION EUROPISCHES KOMITEE FUR NORMUNG COM

14、ITE EUROPEEN DE NORMALISATION Central Secretariat rue de Stassart, 36 6-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means resewed worldwide for CEN national Members. Ref. No. EN IS0 40471998 E STD-BSI BS EN IS0 4047-ENGL 1918 I 1b24bb7 0738073 L(i5 I EN IS0 4047:1998 For

15、eword The text of the international Standard from Technical Committee ISO/TC 120 “Leather“ of the international Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC 289 “Leather“, the secretariat of which is held by UNI. This European Stand

16、ard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 1999, and conflicting national standards shall be withdrawn at the latest by March 1999. According to the CENKENELEC Internal Regulations, the national standards

17、 organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement not

18、ice The text of the International Standard IS0 4047:19n has been approved by CEN as a European Standard without any modification. STD-BSI BS EN IS0 4047-ENGL 1798 O Lb2LibbS 0738072 381 II EN IS0 4047:1998 INTERNATIONAL STANDARD 4047 INTERNATIONAL ORGANIZATION FOR STANDARDIZATION .MEYAYHAWilHAI 0PAH

19、)iJAUHI II0 CTAHIIAPTHUUHH .ORGANISATION INTERNATIONALE DE NORMALISATION Leather - Determination of sulphated total ash and sulphated water-insoluble ash Cuir - Dosage des cendres sulfates totales et des cendres sulfates insolubles dans leau - First edition - 1977-1 1-01 - E e - - UDC 675 : 543.82 R

20、ef. No. IS0 4047-1977 (E) Dawiptorr : leather, chemical analysis, determination of content, ash, mineral matter, sulphating analysis. Price based on 2 pages STD-BSI BS EN IS0 Li047-ENGL 1798 Lb24bb7 0738073 2LB EN IS0 4047:1998 FOREWORD IS0 (the International Organization for Standardization) is a w

21、orldwide federation of national standards institutes (IS0 member bodies). The work of developing International Standards is carried out through IS0 technical committees. Every member body interested in a subject for which a technical committee has been set up has the right to be represented on that

22、committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the IS0

23、 Council. International Standard IS0 4047 was developed by Technical Committee ISO/TC 120, Leazher, and was circulated to the member bodies in July 1976. It has been approved by the member bodies of the following countries : Australia Brazil Canada Chile Czechoslovakia Egypt, Arab Rep. of France Ger

24、many Hungary Poland India Romania Iran South Africa, Rep. of Israel Turkey Italy United Kingdom Mexico Yugoslavia Netherlands New Zealand No member body expressed disapproval of the document. This International Standard is based on method IUC/7 of the International Union of Leather Technologists and

25、 Chemists Societies. O Intunitional 0rg.niution for Stindirdiutkn, 1977 o STD-BSI BS EN IS0 4OY7-ENGL 1778 I 1b24Lb 0738Dq 154 EN IS0 4047:1998 Leather - Determination of sulphated total ash and sulphated water- inso lu b le ash O INTRODUCTION The amount of mineral substances found by ashing leather

26、 may differ from the actual content owing to decomposition, reduction, or the escape by volatilization of certain salts. By treating the ash with sulphuric acid, the salts and oxides are converted into sulphates, but some salts will again be transformed into oxides at the selected temperature of ign

27、ition. To determine the total mineral content, for example within the framework of a complete leather analysis. the water- soluble and water-insoluble inorganic substances can be ascertained by calculation or determined separately. Ammonium salts are not determined by this method (compare with IS0 4

28、098). 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a method for the determination of the sulphated total ash and the sulphated water-insoluble ash of leather. The method is applicable to all types of leather. The determination may be inaccurate by the extent to which the le

29、ather contains organo-metallic compounds, for example silicone (see note 1 in 8.1 ). 2 REFERENCES IS0 2418, Leather - Laboratory samples - Location and identification. IS0 2588, Leather - Sampling - Number of items for a gross sample. IS0 4044. Leather - Pnparation of chemical test samples. IS0 4098

30、. Leather - Determination of water-soluble matter, water-soluble inorganic matter and water-soluble organic matter. 1 3 DEFINITIONS For the purposes of this International Standard, the following definitions apply : 3.1 sulphated total ash : The residue obtained from carbonized leather at 800 OC afte

31、r sulphating the ash under the specified conditions. 3.2 sulphated water-insoluble ash : The residue obtained when leather, previously extracted with water as specified in IS0 4098, is carbonized after sulphating the ash under the specified conditions. 4 PRINCIPLE Carbonization of the leather follow

32、ed by treatment with sulphuric acid and ashing in an open crucible. 5 REAGENTS During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. 5.1 Sulphuric acid, approximately 2 N solution. 5.2 Ammonium nitrate, approximately 100 g/I sol

33、ution. 6 APPARATUS Ordinary laboratory apparatus and in particular 6.1 Crucibles and dishes of glazed porcelain, platinum or quartz. 6.2 Muffle furnace, capable of being maintained at a temperature close to, but not exceeding, 800 OC (see note 4 in 8.1). 1) At present at the stage of draft. 1 STD-BS

34、I BS EN IS0 LiOLi7-ENGL 1998 m LbZqbbS 0738095 O90 m EN IS0 4047:1998 7 SAMPLING 7.1 Whole pieces of leather In the absence of any other agreement on sampling between the interested parties, the procedure specified in IS0 2588 for sampling from a lot shall be followed. Samples shall be taken from th

35、e pieces as specified in IS0 2418. 7.2 Other applications Sampling shall be carried out as required by the relevant specification or contract. 8 PROCEDURE 8.1 Sulphated total ash Prepare the sample as specified in IS0 4044 (see note 1). Weigh, to the nearest 0,001 g, 2 to 5 g of the sample and caref

36、ully carbonize it over a low flame in a crucible (6.1) which has been previously heated to 8OO0C, cooled and weighed, so that the leather burns with a small flame. Carbonize fat-liquored leather particularly carefully so that the grease burns very slowly. Then thoroughly moisten with the sulphuric a

37、cid solution (5.1) and heat over a low flame until sulphur trioxide fumes are no longer visible. Heat more vigorously, and then ignite in the furnace (6.21, maintained at 800 OC, until completely ashed (see notes 2, 3 and 4). Cool in a desiccator and weigh. Repeat the addition of acid and the heatin

38、g, cooling and weighing operations until the mass of the residue is constant (see note 5). NOTES 1 It is advisable to extract leather impregnated with volatile organo-metallic compounds with dichloromethane before deter- mining the sulphated total ash. 2 If a carbon-free residue cannot be obtained i

39、n spite of heating at 800 OC, the residue should be moistened with a little ammonium nitrate solution (5.2) and the heating repeated until the ash is free from carbon. 3 If complete ashing is not possible, even with the aid of ammonium nitrate, extract the contents of the crucible with hot water and

40、 filter through an ash-free filter paper. Ash the carbon residue together with the filter paper, add the filtrate to the contents of the crucible, evaporate on a water bath, again heat at 800 “C until the last traces of visible carbon are removed, cool in a desiccator and weigh. 4 At temperatures ab

41、ove 800C. some loss of mass from the residue is possible due to volatilization of certain inorganic salts. For this reason, close control is essential to prevent the maximum furnace temperature from exceeding 800 “C. 5 The sulphated total ash should be retained, if required for the determination of

42、its components (for example chromic oxide, aluminium oxide, iron oxide) and for the determination of the cations present in the mineral impurities. 8.2 Sulphated water-insoluble ash Extract the water-soluble substances from the prepared ground leather as specified in ISO4098. Air-dry the extracted s

43、ample (see note). Continue as specified in 8.1. NOTE - For the separate determination of sulphated water- insoluble ash, it is not absolutely necessary for the whole of the extracted and dried leather left after determination of the water- soluble matter, in accordance with IS0 4098, to be ashed. Th

44、e residual airdried leather can be mixed and weighed and an adequate part of it ashed. 9 EXPRESSION OF RESULTS 9.1 Calculation 9.1.1 The sulphated total ash is given, as a percentage by mass, by the formula m1 -x 100 mo 2 where mo leather; m, is the mass, in grams, of the original sample of is the m

45、ass, in grams, of sulphated total ash. 9.2.1 The sulphated water-insoluble ash is given, as a percentage by mass, by the formula m2 -x 100 mo where mo leather; m2 insoluble ash. is the mass, in grams, of the original sample of is the mass, in grams, of the sulphated water- NOTE - The percentage of s

46、ulphated water-insoluble ash may alternatively be calculated by deducting from the percentage of total sulphated ash the percentage of sulphated ash from the water- soluble matter, if this has been separately determined. 9.2 Repeatability The results of duplicate determinations by the same operator

47、should not differ by more than 0.1 %, calculated on the original sample mass. If the difference is greater, the determination shall be carried out once more. 10 TEST REPORT The test report shall include the following particulars : a) a reference to this International Standard; b) complete identifica

48、tion of the sample; c) the results obtained, to one decimal place, and the mean value; d) details of any special circumstances which may have affected the results. STD.BS1 BS EN IS0 qOq7-ENGL 1798 111 LbSqbb 073807b T27 BS EN IS0 4047: 1998 BSI 389 Chiswick High Road London w4 4AL BSI - British Stan

49、dards Institution BSI is the independent national body responsible for preparing British standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant alln of BSI to improve the ty of our products and services. We would be gratefui if anyone finding an inaccuracy or ambiguity while using th