BS EN ISO 4047-1998 Leather - Determination of sulphated total ash and sulphated water-insoluble ash《皮革 硫酸盐总灰分和硫酸盐水溶灰分的测定》.pdf

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1、BRITISH STANDARD BS EN ISO 4047:1998 Leather Determination of sulphated total ash and sulphated water-insoluble ash The European Standard EN ISO4047:1998 has the status of a British Standard ICS 59.140.30BSENISO4047:1998 This British Standard, having been prepared under the directionof the Sector Co

2、mmitteefor Materials and Chemicals, was published underthe authority of the Standards Committee and comesinto effect on 15 November1998 BSI 06-1999 ISBN 0 580 30781 6 National foreword This British Standard is the English language version of EN ISO4047:1998. It is identical with ISO4047:1977. It sup

3、ersedes BS1309:1974, clause 6, which is withdrawn by amendment. The UK participation in its preparation was entrusted to Technical Committee TCI/69, Footwear and leather, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committe

4、e any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; 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-referenc

5、es Attention is drawn to the fact that CEN and CENELEC standards normally include an annex which lists normative references to international publications with their corresponding European publications. The BritishStandards which implement international or European publications referred to in this do

6、cument may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of

7、 British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN ISO title page, page 2, the ISO title p

8、age, pageii, pages 1 and 2 and aback cover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBSENISO4047:1998 BSI 06-1999 i

9、Contents Page National foreword Inside front cover Foreword 2 Foreword ii Text of ISO 4047 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 4047 September 1998 ICS 59.140.30 Descriptors: See ISO document English version Leather Determination of sulphated total ash and sulphated wate

10、r-insoluble ash (ISO 4047:1977) Cuir Dosage des cendres sulfates totales et des cendres sulfates insolubles dans leau (ISO4047:1977) Leder Bestimmung der sulfatierten Gesamtasche und der sulfatierten wasserunlslichen Asche (ISO4047:1977) This European Standard was approved by CEN on 9 August1998. CE

11、N 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 lists and bibliographical references concerning such national standards may be obtained on app

12、lication to the Central Secretariat 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 Central Secretariat has

13、 the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Comm

14、ittee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4047:1998 EENISO4047:1998 BSI

15、 06-1999 2 Foreword The text of the International Standard from Technical Committee ISO/TC120 “Leather” of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC289 “Leather”, the secretariat of which is held by UNI. This Eu

16、ropean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March1999, and conflicting national standards shall be withdrawn at the latest by March1999. According to the CEN/CENELEC Internal Regulations, the nationa

17、l standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and theUnitedKingdom. Endorse

18、ment notice The text of the International Standard ISO4047:1977 has been approved by CEN as a European Standard without any modification. Contents Page Foreword 2 0 Introduction 1 1 Scope and field of application 1 2 References 1 3 Definitions 1 4 Principle 1 5 Reagents 1 6 Apparatus 1 7 Sampling 1

19、8 Procedure 2 9 Expression of results 2 10 Test report 2ENISO4047:1998 ii BSI 06-1999 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards institutes (ISO member bodies). The work of developing International Standards is carried out throug

20、h ISO 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 committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. Draft Internationa

21、l Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the ISO Council. International Standard ISO4047 was developed by Technical Committee ISO/TC120, Leather, and was circulated to the member bodies in J

22、uly1976. It has been approved by the member bodies of the following countries: 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 Chemists Societies. Australia Hungary Poland Brazil India

23、Romania Canada Iran South Africa, Rep. of Chile Israel Turkey Czechoslovakia Italy United Kingdom Egypt, Arab Rep. of Mexico Yugoslavia France Netherlands Germany New ZealandENISO4047:1998 BSI 06-1999 1 0 Introduction The amount of mineral substances found by ashing leather may differ from the actua

24、l 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 ignition. To determine the to

25、tal 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 ISO4098). 1 Scope and field of a

26、pplication 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 leather contains organo-metall

27、ic compounds, for example silicone (see note1 in 8.1). 2 References ISO 2418, Leather Laboratory samples Location and identification. ISO 2588, Leather Sampling Number of items for a gross sample. ISO 4044, Leather Preparation of chemical test samples 1) . ISO 4098, Leather Determination of water-so

28、luble 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 at800C after sulphating the ash under the specified

29、conditions 3.2 sulphated water-insoluble ash the residue obtained when leather, previously extracted with water as specified in ISO4098, is carbonized after sulphating the ash under the specified conditions 4 Principle Carbonization of the leather followed by treatment with sulphuric acid and ashing

30、 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/l solution. 6 Apparatus Ordinary laboratory apparat

31、us 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, 800C (seenote4 in 8.1) 7 Sampling 7.1 Whole pieces of leather In the absence of any other agreement on sampling between

32、the interested parties, the procedure specified in ISO2588 for sampling from a lot shall be followed. Samples shall be taken from the pieces as specified in ISO2418. 7.2 Other applications Sampling shall be carried out as required by the relevant specification or contract. 1) At present at the stage

33、 of draft.ENISO4047:1998 2 BSI 06-1999 8 Procedure 8.1 Sulphated total ash Prepare the sample as specified in ISO4044 (seenote 1). Weigh, to the nearest 0,001g, 2to 5g of the sample and carefully carbonize it over a low flame in a crucible (6.1) which has been previously heated to 800C, cooled and w

34、eighed, 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 acid solution (5.1) and heat over a low flame until sulphur trioxide fumes are no longer visible. Heat more vig

35、orously, and then ignite in the furnace (6.2), maintained at800C, until completely ashed (see notes 2, 3 and4). Cool in a desiccator and weigh. Repeat the addition of acid and the heating, cooling and weighing operations until the mass of the residue is constant (see note5). NOTE 1It is advisable to

36、 extract leather impregnated with volatile organo-metallic compounds with dichloromethane before determining the sulphated total ash. NOTE 2If a carbon-free residue cannot be obtained in spite of heating at 800C, the residue should be moistened with a little ammonium nitrate solution (5.2) and the h

37、eating repeated until the ash is free from carbon. NOTE 3If complete ashing is not possible, even with the aid of ammonium nitrate, extract the contents of the crucible with hot water and filter through an ash-free filter paper. Ash the carbon residue together with the filter paper, add the filtrate

38、 to the contents of the crucible, evaporate on a water bath, again heat at800C until the last traces of visible carbon are removed, cool in a desiccator and weigh. NOTE 4At temperatures above 800C, some loss of mass from the residue is possible due to volatilization of certain inorganic salts. For t

39、his reason, close control is essential to prevent the maximum furnace temperature from exceeding 800C. NOTE 5The sulphated total ash should be retained, if required for the determination of its components (for example chromic oxide, aluminium oxide, iron oxide) and for the determination of the catio

40、ns 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 sample (see note). Continue as specified in 8.1. NOTEFor the separate determination of sulphated water-insolubl

41、e 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 ISO4098, to be ashed. The residual air-dried leather can be mixed and weighed and an adequate part of it ashed. 9 Expression of results 9.1

42、Calculation 9.1.1 The sulphated total ash is given, as a percentage by mass, by the formula where m 0is the mass, in grams, of the original sample of leather; m 1is the mass, in grams, of sulphated total ash. 9.2.1 The sulphated water-insoluble ash is given, as a percentage by mass, by the formula w

43、here m 0is the mass, in grams, of the original sample of leather; m 2is the mass, in grams, of the sulphated water-insoluble ash. NOTEThe percentage of sulphated water-insoluble ash may alternatively be calculated by deducting from the percentage of total sulphated ash the percentage of sulphated as

44、h from the water-soluble matter, if this has been separately determined. 9.2 Repeatability The results of duplicate determinations by the same operator 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 on

45、ce more. 10 Test report The test report shall include the following particulars: a) a reference to this International Standard: b) complete identification 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

46、 the results. m 1 m 0 -100 m 2 m 0 -100 blankBS EN ISO 4047:1998 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It

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