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1、w - INTERNATIONAL STANDARD. INTERNATIONAL ORGANIZATION FOR STANDARDIZATIONMEXAYHAPOAHAfl OPrAHM3AUMA I-IO CTAHAAPTM3AUMWORGANISATION INTERNATIONALE DE NORMALISATION Leather - Determination of sulphated total ash and sulphated water-insoluble ash Cuir - Dosage des cendres sulfatees totales et des cen
2、dres sulfatkes insolubles dans leau First edition - 1977-11-01 UDC 675 : 543.82 Ref. No. ISO 4047-1977 (E) Descriptors : leather, Chemical analysis, determination of content, ash, mineral matter, sulphating analysis. Price based on 2 pages Copyright International Organization for Standardization Pro
3、vided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 21:43:45 MDTNo reproduction or networking permitted without license from IHS -,-,- FOREWORD ISO (the International Organization for Standardization) is a worldwide federation of national Sta
4、ndards institutes (ISO member bodies). The work of developing International Standards is carried out through 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 organizati
5、ons, 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 ISO Council. International Standard IS
6、O 4047 was developed by Technical Committee ISO/TC 120, Leather, and was circulated to the member bodies in July 1976. lt has been approved by the member bodies of the following countries : Austral ia Hungary Brazil India Canada Iran Chile Israel Czechoslovakia I taly Egypt, Arab Rep. of Mexico Fran
7、ce Netherlands Germany New Zealand Poland Romania South Africa, Rep. of Turkey United Kingdom Yugoslavia No member body expressed disapproval of the document. This International Standard is based on method lUC/7 of the International Union of Leather Technologists and Chemists Societies. 0 Internatio
8、nal Organkation Printed in Switzerland Standardkation, Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 21:43:45 MDTNo reproduction or networking permitted without license from IH
9、S -,-,- INTERNATIONAL STANDARD ISO4047-1977 (E) Leather - Determination of sulphated total ash and sulphated watet=insoluble ash 0 INTRODUCTION The amount of mineral substances found by ashing leather may differ from the actual content owing to decomposition, reduction, or the escape by volatilizati
10、on 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 total mineral content, for example within the framework of a complete leathe
11、r analysis, the water- soluble and water-insoluble inorganic substances tan be ascertained by calculation or determined separately. Ammonium salts are not determined by this method (compare with ISO 4098). 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a method for the determ
12、ination of the sulphated total ash and the sulphated watet-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-metallic compounds, for example Silicone (see note 1 in 8.1). 3 DEFINITIONS Fo
13、r the purposes of this International Standard, the following definitions apply : 3.1 sulphated total ash : The residue obtained from carbonized leather at 800 C after sulphating the ash under the specif ied conditions. 3.2 sulphated water-insoluble ash : The residue obtained when leather, previously
14、 extracted with water as specified in ISO 4098, is carbonized after sulphating the ash under the specif ied conditions. 4 PRINCIPLE Carbonization of the leather followed by treatment with sulphuric acid and ashing in an open crucible. 5 REAGENTS During the analysis, use only reagents of recognized a
15、nalytical 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. 2 REFERENCES ISO 2418, Leather - Laboratory samples - Location and iden tifica tion. ISO 2588, Leather - Sampling - Number of
16、items for a gross Sample. ISO 4044, Leather - Preparation of Chemical test samples. i ) ISO 4098, Leather - Determination of water-soluble matter, wa ter-soluble inorganic matter and wa ter-soluble organic matter. 1 ) 6 APPARATUS Ordinary laboratory apparatus and in particular 6.1 Crucibles and dish
17、es of glazed porcelain, platinum or quartz. 6.2 Muffle furnace, capable of being maintained at a temperature close to, but not exceeding, 800 “C (see note 4 in 8.1). 1) At present at the Stage of draft. 1 Copyright International Organization for Standardization Provided by IHS under license with ISO
18、 Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 21:43:45 MDTNo reproduction or networking permitted without license from IHS -,-,- 1 4047-1977 (E) 7 SAMPLING 7.1 Whole pieces of leather In the absence of any other agreement on sampling between the interested Parties, the p
19、rocedure specified in ISO 2588 for sampling from a lot shall be followed. Samples shall be taken from the pieces as specified in ISO 2418. 7.2 Other applications Sampl ing shall be ca rried specif icat on or contr act. out as required by the relevant 8 PROCEDURE 8.1 Sulphated total ash Prepare the S
20、ample as specified in ISO 4044 (see note 1). Weigh, to the nearest 0,001 g, 2 to 5 g of the Sample and carefully carbonize it over a low flame in a crucible (6.1) which has been previously heated to 800 C, cooled and weighed, so that the leather burns with a small flame. Carbonize fat-liquored leath
21、er 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 vigorously, and then ignite in the furnace (6.2), maintained at 800 C, until complete
22、ly ashed (see notes 2, 3 and 4). Cool in a desiccator and weigh. Repeat the addition of acid and the heating, cooling and weighing sperations until the mass of the residue is constant (see note 5). 1 lt is advisable to extract leather impregnated with volatile organo-metallic compounds with dichloro
23、methane before deter- mining the sulphated total ash. 2 lf a carbon-free residue cannot be obtained in 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 pos
24、sible, 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 to the contents of the crucible, evaporate on a water bath, again heat at 800 “C unti
25、l the last traces of visible carbon are removed, cool in a desiccator and weigh. 4 At temperatures above 800 OC, some loss of mass from the residue is possible due to volatilization of certain inorganic salts. or this reason, close control is essential to prevent the maximum furnace temperature from
26、 exceeding 800 “C. 5 The 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 cations present in the mineral impurities. 8.2 Sulphated water-insoluble ash Extract the wate
27、r-soluble substances from the prepared ground leather as specified in ISO 4098. Air-dry the extracted Sample (see note). Continue as specified in 8.1. NOTE - or the separate determination of sulphated water- insoluble ash, it is not absolutely necessary for the whole of the extracted and dried leath
28、er left after determination of the water- soluble matter, in accordance with ISO 4098, to be ashed. The residual air-dried leather tan 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 th
29、e formula “1 -x 100 mO where mO is the mass, in grams, of the original Sample of leather; “1 is 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 m2 -x 100 “0 where mO is the mass, in grams, of the original Sample of
30、 leather; m2 is the mass, in grams, of the sulphated water- insoluble ash. NOTE - The percentage of sulphated 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 s
31、eparately determined. 9.2 Repeatability The resuits of duplicate determinations by the Same Operator should not differ by more than 0,l %, calculated on the original Sample mass. If the differente is greater, the determination shall be carried out once more. 10 TEST REPORT The test report shall incl
32、ude 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 the results. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/25/2007 21:43:45 MDTNo reproduction or networking permitted without license from IHS -,-,-