BS EN ISO 4098-2007 Leather - Chemical tests - Determination of water-soluble matter water-soluble inorganic matter and water-soluble organic matter《皮革 化学试验 水溶物、水溶无机物和水溶有机物的测定》.pdf

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1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58water-soluble inorganic matter and water-soluble organic matterThe European Standard EN ISO 4098:20

2、06 has the status of a British StandardICS 59.140.30Leather Chemical tests Determination of water-soluble matter, BRITISH STANDARDBS EN ISO 4098:2006BS EN ISO 4098:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2007 BSI 2007IS

3、BN 978-0-580-49985-2Amendments issued since publicationAmd. No. Date Commentscontract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard was published by BSI. It is the UK implemen

4、tation of EN ISO 4098:2006. The UK participation in its preparation was entrusted to Technical Committee TCI/69, Footwear, leather and coated fabrics.A list of organizations represented on TCI/69 can be obtained on request to its secretary.This publication does not purport to include all the necessa

5、ry provisions of a EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 4098January 2006ICS 59.140.30English VersionLeather - Chemical tests - Determination of water-solublematter, water-soluble inorganic matter and water-soluble organicmatter (ISO 4098:2006)Cuir - Essais chimiques - Dtermination d

6、es matiressolubles dans leau, des matires inorganiques solublesdans leau et des matires organiques solubles dans leau(ISO 4098:2006)Leder - Chemische Prfungen - Bestimmungwasserlslicher Substanzen, wasserlslicher anorganischerSubstanzen und wasserlslicher organischer Substanzen(ISO 4098:2006)This Eu

7、ropean Standard was approved by CEN on 28 December 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

8、concerning such nationalstandards may be obtained on application 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 translationunder the responsibility of a CEN member into its ow

9、n language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg

10、, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2006 CEN All rights of ex

11、ploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 4098:2006: EForeword This document (EN ISO 4098:2006) has been prepared by Technical Committee IULTCS “the International Union of Leather Technologists and Chemists Societies“ in collaboration with Tec

12、hnical 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 July 2006, and conflicting national standards shall be withdrawn at

13、the latest by July 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, I

14、reland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 4098:2006 has been approved by CEN as EN ISO 4098:2006 without any modifications. EN ISO 4098:200

15、6Reference numberISO 4098:2006(E)IULTCS/IUC 6:2006(E)INTERNATIONAL STANDARD ISO4098IULTCS/IUC6First edition2006-01-15Leather Chemical tests Determination of water-soluble matter, water-soluble inorganic matter and water-soluble organic matter Cuir Essais chimiques Dtermination des matires solubles d

16、ans leau, des matires inorganiques solubles dans leau et des matires organiques solubles dans leau EN ISO 4098:2006ii iiiContents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Terms and definitions. 2 5 Reagents 2 6 Apparatus 2 7 Sampling and preparation of samples 3 8 Pro

17、cedure 3 8.1 General. 3 8.2 Water-soluble matter 3 8.3 Water-soluble inorganic matter. 3 9 Remarks on the procedure 3 10 Calculation and expression of results 4 11 Test report . 5 12 Repeatability 5 EN ISO 4098:2006iv Foreword ISO (the International Organization for Standardization) is a worldwide f

18、ederation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that co

19、mmittee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accor

20、dance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requir

21、es approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 4098 was prepared by the Europe

22、an Committee for Standardization (CEN) Technical Committee CEN/TC 289, Leather, in collaboration with the Chemical Tests Commission of the International Union of Leather Technologists and Chemists Societies (IUC Commission, IULTCS), in accordance with the Agreement on technical cooperation between I

23、SO and CEN (Vienna Agreement). It is based on IUC 6 originally published in J. Soc. Leather Trades Chemists, 49, p. 13, 1965 and declared an official method of the IULTCS in 1965. IULTCS, originally formed in 1897, is a world-wide organization of professional leather societies to further the advance

24、ment of leather science and technology. IULTCS has three Commissions, which are responsible for establishing international methods for the sampling and testing of leather. ISO recognizes IULTCS as an international standardizing body for the preparation of test methods for leather. EN ISO 4098:20061L

25、eather Chemical tests Determination of water-soluble matter, water-soluble inorganic matter and water-soluble organic matter 1 Scope This International Standard specifies a method of determination of water-soluble matter, water-soluble inorganic matter and water-soluble organic matter. It is applica

26、ble to all leather types. The result obtained by this analysis depends on factors such as: the degree to which the leather is ground; the extraction temperature; the extraction period; the ratio of leather to water. To obtain comparable results, it is consequently imperative that test conditions sho

27、uld be accurately reproduced. In all cases, any ammonium salts in the filtrate are included as part of the water-soluble matter and are then decomposed on ignition. Thus they contribute towards the result for water-soluble organic substances. The concentration of the ammonium salts can be determined

28、 in the filtrate separately if required. 2 Normative 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 amendm

29、ents) applies. ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling location ISO 3696, Water for analytical laboratory use Specification and test methods ISO 4044, Leather Preparation of chemical test samples ISO 4048, Leather Determination of matter soluble in dichloromet

30、hane ISO 4684, Leather Chemical tests Determination of volatile matter 3 Principle Following aqueous extraction of a prepared sample under specified conditions, the water-soluble matter is quantified by evaporation and drying at (102 2) C. Sulfating and ashing of the residue at 700 C yields the wate

31、r-soluble inorganic matter. The water-soluble organic matter is derived by difference. EN ISO 4098:20062 4 Terms and definitions For the purposes of this document, the following terms and definitions apply. 4.1 water soluble matter substance which, under the conditions described in this method, is d

32、issolved out of the leather by water 4.2 water soluble inorganic matter sulfated ash of the water-soluble matter prepared in accordance with this method 4.3 water soluble organic matter difference between total water-soluble matter and water-soluble inorganic matter 5 Reagents 5.1 Sulfuric acid solu

33、tion,1 mol/l. 5.2 Distilled or deionized water, conforming to the requirements of Grade 3 of ISO 3696. 6 Apparatus Usual laboratory apparatus is required and, in particular the following: 6.1 Flasks, with a wide neck and a close fitting stopper (650 ml to 750 ml capacity should be suitable). 6.2 Gra

34、duated measuring cylinder, capacity 500 ml. 6.3 Pipette, capacity 50 ml. 6.4 Evaporating basin, quartz, platinum or porcelain, with flat bottom, and a working capacity of at least 50 ml. 6.5 Appropriate shaking apparatus operating at (50 10) cycles per minute. 6.6 Thermometer of range from 0 C to 50

35、 C. 6.7 Fluted filter paper of fast qualitative grade. 6.8 Boiling water or steam bath. 6.9 Oven, capable of being maintained at 102 C 2 C. 6.10 Muffle furnace, capable of being maintained at a temperature close to but not exceeding 700 C (see 9.4) 6.11 Desiccator. 6.12 Analytical balance weighing t

36、o an accuracy of 0,001 g. EN ISO 4098:200637 Sampling and preparation of samples If possible, sample in accordance with ISO 2418 and grind leather in accordance with ISO 4044. If sampling in accordance with ISO 2418 is not possible (e.g. in the case of leathers from finished products such as shoes o

37、r garments), details about sampling have to be given together with the test report. Weigh accurately approximately 10 g of ground leather and record the mass (m0). Extract the leather in accordance with ISO 4048 before determination of the water-soluble matter. If the result is to be presented on th

38、e basis of dry substance, then a further sample of the same leather should tested in accordance with ISO 4684, so that the moisture content can be calculated. 8 Procedure 8.1 General Quantitatively transfer the air-dried, ground, dichloromethane-extracted leather obtained from Clause 7 into a flask

39、(6.1). Add 500 ml 10 ml of deionised water (5.2) at 22,5 C 2,5 C, close the stopper securely and shake mechanically (6.5) at (50 10) cycles per minute for 2 h 10 min at (22,5 C 2,5) C (see 9.1). Filter the contents of the flask through a fluted filter paper (6.7) until the filtrate is clear. Discard

40、 the first 50 ml. Determine the water-soluble organic matter and inorganic matter in subsequent 50 ml aliquot portions of the filtrate (see 9.2 and 9.3) 8.2 Water-soluble matter Pipette 50,0 ml (6.3) of filtrate into a basin (6.4) which has previously been prepared by heating at 700 C (6.10), cooled

41、 in a desiccator and accurately weighed. Evaporate the filtrate over the water-bath (6.8) and dry the residue at 102 C 2 C (6.9) for approximately 2 h. Cool in a desiccator, using only one basin at a time in a small desiccator, and no more than two in a large desiccator. Weigh quickly, and repeat th

42、e drying, cooling and weighing procedure either until the further reduction in mass does not exceed 2 mg, or the total drying time equals 8 h. Record the final mass and calculate the mass of dry residue (m1). 8.3 Water-soluble inorganic matter Thoroughly wet the residue obtained in 8.2 (see 9.2) in

43、the basin (6.4) with just sufficient 1 mol/l sulfuric acid, and heat gently over a low flame until no more sulfur trioxide fumes are visible. Heat more strongly until the basin approaches red heat. Transfer to the muffle furnace (6.10) at 700 C for 15 min (see 9.4). Cool in the desiccator and weigh

44、as quickly as possible. Repeat the addition of acid, heating, cooling and weighing until the further reduction in mass does not exceed 2 mg, or the total drying time equals 8 h. Record the final mass and calculate the mass of the sulfated residue, (m2). 9 Remarks on the procedure 9.1 If the specifie

45、d extraction temperature of 22,5 C 2,5 C cannot be maintained in the test room, it is advisable to use a vacuum flask of 650 ml to 750 ml capacity. The range of values of the total water-soluble matter, wT,ws, is likely to differ by about 0,5 % over the permitted temperature range. 9.2 The water sol

46、uble matter and the water-soluble inorganic matter can each be determined separately. Water-soluble matter can be determined by evaporating 50 ml portions of the filtrate in previously dried platinum, quartz, silver, porcelain or glass dishes at 102 C 2 C, in accordance with 8.2. Water-soluble inorg

47、anic matter can be determined by evaporation of separate 50 ml portions in previously heated quartz, platinum or glazed porcelain dishes in accordance with 8.3. EN ISO 4098:20064 9.3 If the mass of water-soluble inorganic matter is likely to be less than 2,0 % of the leather mass, it is recommended

48、that a 100 ml or 200 ml aliquot portion should be used. In cases where the result is likely to be less than 1,0 %, a 100 ml or 200 ml portion should always be used. 9.4 At temperatures above 700 C some loss of mass from the residue, owing to volatilisation of certain inorganic salts is possible. For

49、 this reason close control is essential to prevent the maximum furnace temperature from exceeding 700 C. 10 Calculation and expression of results Calculate the following percentages when the evaporated volume of water is 1/10 of the total volume. If other volumes are used then the factor 10 must be changed appropriately. a) Total water-soluble matter, wT,ws(mass fraction in percent): 1T,ws010 100mwm= where m1is the mass of the dry residue; m0is th

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