EN ISO 4098-2018 Leather - Chemical tests - Determination of water-soluble matter water-soluble inorganic matter and water-soluble organic matter.pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Leather - Chemical tests - Determination of water-soluble matter, water-soluble inorganic matter and water-soluble organic matterBS EN ISO 4098:2018National forewordThis British Standard is the UK implementation of EN I

2、SO 4098:2018. It is identical to ISO 4098:2018. It supersedes BS EN ISO 4098:2006, which will is withdrawn.The UK participation in its preparation was entrusted to Technical Committee TCI/69, Footwear the extraction temperature; the extraction period; the ratio of leather to water.To obtain comparab

3、le results, it is consequently imperative that test conditions 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.

4、 The concentration of the ammonium salts can be determined in the filtrate separately if required.2 Normative referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the editio

5、n cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 2418, Leather Chemical, physical and mechanical and fastness tests Sampling locationISO 3696, Water for analytical laboratory use Specification and test methodsISO 4048, Leat

6、her Chemical tests Determination of matter soluble in dichloromethane and free fatty acid contentISO 4044, Leather Chemical tests Preparation of chemical test samplesISO 4684, Leather Chemical tests Determination of volatile matter3 Terms and definitionsFor the purposes of this document, the followi

7、ng terms and definitions apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: ISO Online browsing platform: available at https:/www.iso.org/obp IEC Electropedia: available at http:/www.electropedia.org/INTERNATIONAL STANDARDISO 4098:2018(E) ISO 2

8、018 All rights reserved 1BS EN ISO 4098:2018ISO 4098:20183.1water-soluble mattersubstance which, under the conditions described in this method, is dissolved out of the leather by water3.2water-soluble inorganic mattersulfated ash of the water-soluble matter (3.1) prepared in accordance with this met

9、hod3.3water-soluble organic matterdifference between total water-soluble matter (3.1) and water-soluble inorganic matter (3.2)4 PrincipleFollowing aqueous extraction of a prepared sample under specified conditions, the water-soluble matter is quantified by evaporation and drying at (102 2) C. Sulfat

10、ing and ashing of the residue at 700 C yields the water-soluble inorganic matter. The water-soluble organic matter is derived by the difference.5 Reagents5.1 Sulfuric acid solution,1 mol/l.5.2 Distilled or deionized water, conforming to the requirements of Grade 3 of ISO 3696.6 ApparatusThe usual la

11、boratory apparatus is required, 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 Graduated measuring cylinder, capacity 500 ml.6.3 Pipette, capacity 50 ml.6.4 Evaporating basin, quartz, platinum or porcelain, with

12、 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 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 2)

13、 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.2 ISO 2018 All rights reservedBS EN ISO 4098:2018ISO 4098:20186.12 Analytical balance weighing to an accuracy of 0,001 g.7 Sampling and preparation of samplesSample in acco

14、rdance 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 or garments), details about sampling shall be given together with the test report.Weigh accurately approxima

15、tely 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 the basis of dry substance, then a further sample of the same leather shall be tested in accordance with ISO 4684

16、, so that the moisture content can be calculated.8 Procedure8.1 GeneralQuantitatively transfer the air-dried, ground, dichloromethane-extracted leather obtained from Clause 7 into a flask (6.1). Add (500 10) ml of deionised water (5.2) at (23,5 3,5) C, close the stopper securely and shake mechanical

17、ly (6.5) at (50 10) cycles per minute for (120 min 10) min at (23,5 3,5) C (see 9.1).Filter the contents of the flask through a fluted filter paper (6.7) until the filtrate is clear. Discard the first 50 ml. Determine the water-soluble organic matter and inorganic matter in subsequent 50 ml aliquot

18、portions of the filtrate (see 9.2 and 9.3).8.2 Water-soluble matterPipette 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 in a desiccator (6.11) and accurately weighed (6.12). Evaporate the filtrate over the water bath (6.8) and dry

19、 the residue at (102 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 the drying, cooling and weighing procedure either until the further reduction in mass does not exce

20、ed 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 matterThoroughly wet the residue obtained in 8.2 (see 9.2) in the basin (6.4) with just sufficient 1 mol/l sulfuric acid (5.1), and heat gently over a low flame

21、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 as quickly as possible. Repeat the addition of acid, heating, cooling and weighing until the

22、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 procedure9.1 If the specified extraction temperature of (23,5 3,5) C cannot be maintained in the test room, it is advisable

23、 to use a vacuum flask of 650 ml to 750 ml capacity. The range of values of the total water-soluble matter, wT, ws, see Clause 10 a) is likely to differ by about 0,5 % over the permitted temperature range.9.2 The water-soluble matter and the water-soluble inorganic matter can each be determined sepa

24、rately. 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 2) C, in accordance with ISO 2018 All rights reserved 3BS EN ISO 4098:2018ISO 4098:20188.2. Water-soluble inorganic matter can

25、be determined by the evaporation of separate 50 ml portions in previously heated quartz, platinum or glazed porcelain dishes in accordance with 8.3.9.3 If the mass of water-soluble inorganic matter is likely to be less than 2,0 % of the leather mass, it is recommended that a 100 ml or 200 ml aliquot

26、 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 is possible, owing to volatilisation of certain inorganic salts. For this reason close control is es

27、sential to prevent the maximum furnace temperature from exceeding 700 C.10 Calculation and expression of resultsCalculate 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 shall be changed appropriately.a) Total wa

28、ter-soluble matter, wT,ws(mass fraction in per cent), see Formula (1):wmmT,ws=1010 100(1)wherem1is the mass of the dry residue;m0is the mass of the original sample of leather.b) Water-soluble inorganic matter, wI,ws, (mass fraction in per cent), see Formula (2):wmmI,ws=2010 100(2)wherem2is the mass

29、of sulfated residue;m0is the mass of the original sample of leather.c) Water-soluble organic matter, wO,ws(mass fraction in per cent). To obtain the percentage water-soluble organic matter, calculate the difference between the percentage total water-soluble matter and the percentage water-soluble in

30、organic matter, see Formula (3):ww wO,ws T,ws I,ws=()()(3)If the results are to be reported on the basis of dry substance, the results above shall be multiplied by the factor 100/(100 w), where w is the mass fraction of the volatile matter in per cent according to ISO 4684. If the results are presen

31、ted on the basis of dry substance, this shall be clearly mentioned in the test report.11 Test reportThe test report shall include the following information:a) reference to this document, i.e. ISO 4098;b) the results obtained to one decimal place;4 ISO 2018 All rights reservedBS EN ISO 4098:2018ISO 4

32、098:2018c) acknowledgement if the results are determined on the basis of the dry substance;d) a description of the sample tested;e) details of any deviations from the procedure, or special circumstances which may have affected the results.12 RepeatabilityThe results of duplicate determinations shoul

33、d not differ by more than 0,2 %, calculated on the original mass of leather. If determinations differ by more than 0,2 %, then a further set of duplicate determinations shall be made and the results reported. ISO 2018 All rights reserved 5BS EN ISO 4098:2018This page deliberately left blankBSI is th

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