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1、BRITISH STANDARD CONFIRMED JULY 1990 BS 3582:1981 Incorporating Amendment No. 1 Method for Determination of oils, fats and waxes in wool UDC 677.014.242:665.1:677.31 Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 This British S
2、tandard, having been prepared under the direction of the Fibres, Yarns and Fabrics Standards Committee, was published under the authority of the Executive Board and comes into effect on 30 January 1981 BSI 08-1999 First published January 1963 First revision January 1981 The following BSI references
3、relate to the work on this standard: Committee reference TCM/26 Draft for comment 80/35943 DC ISBN 0 580 12046 5 Cooperating organizations The Fibres, Yarns and Fabrics Standards Committee, under whose direction this British Standard was prepared, consists of representatives from the following: Asso
4、ciation of Jute Spinners and Manufacturers British Man-made Fibres Federation* British Nonwoven Manufacturers Association British Railways Board British Textile Employers Association* Central Council of the Irish Linen Industry Consumer Standards Advisory Committee of BSI Department of industry (Che
5、micals and Textiles) Institute of Purchasing and Supply International Wool Secretariat* Knitting Industries Federation Ltd.* Manchester Chamber of Commerce and Industry Ministry of Defence* Narrow Fabrics Federation Textile Institute* Warp Knitters Association Ltd. The organizations marked with an a
6、sterisk in the above list, together with the following, were directly represented on the Technical Committee entrusted with the preparation of this British Standard: British Carpet Manufacturers Association Confederation of British Wool Textiles Limited Department of Industry (Laboratory of the Gove
7、rnment Chemist) Manchester Chamber of Commerce Testing House and Laboratories Soap and Detergent Industry Association Society of Dyers and Colourists Society of Motor Manufacturers and Traders Limited Textile Research Council Amendments issued since publication Amd. No.Date of issueComments 5665Augu
8、st 1987Indicated by a sideline in the margin Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 BSI 08-1999i Contents Page Cooperating organizationsInside front cover Forewordii 1Scope1 2References1 3Principle1 4Reagents and appara
9、tus1 5Atmosphere for conditioning and testing1 6Test sample1 7Test procedure1 8Calculation and expression of results2 9Test report2 Publications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 ii BSI
10、 08-1999 Foreword This British Standard has been prepared under the direction of the Fibres, Yarns and Fabrics Standards Committee and is a revision of the 1963 edition. It is based on test method IWTO-10-66 drawn up by the International Wool Textile Organization (IWTO) and is technically equivalent
11、 to ISO 3074:1975 “Wool Determination of dichloromethane-soluble matter in combed sliver” published by the International Organization for Standardization, except that ISO 3074 is applicable only to 100 % wool. Wool textiles may contain solvent extractable substances that are chiefly derived from a)
12、the wool grease occurring naturally in raw wool, b) oils added to assist textile processing, c) detergents taken up during scouring, and d) special finishing agents. The total amount of these substances present depends on the stage of manufacture and its estimation is important for determining the c
13、lean wool content of a sample. These different materials cannot be estimated individually by solvent extraction methods since there are no known solvents that are specific for each component. Hence it is only possible to determine the amount of these substances extracted by a given solvent under spe
14、cified conditions, any additional information being obtained by detailed analysis of the extracted material. Dichloromethane is recognized as a suitable solvent for extracting oils and fats and this standard specifies a method for determining the amount of extractable matter present in a sample of w
15、ool. Extraction with dichloromethane under the prescribed conditions does not completely remove all the fatty matter present in a sample of wool. More fatty matter, possibly of a similar character will usually be extracted by the use of solvents that cause greater swelling of the wool fibres. A Brit
16、ish Standard does not purport to include all the necessary provisions of a contract. Users of 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 fron
17、t cover, an inside front cover, pages i and ii, pages 1 and 2, an inside back cover and a back 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. Licensed Copy: sheffieldun shef
18、fieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 BSI 08-19991 1 Scope This British Standard describes a method for the determination of oils, fats and waxes in wool in any processed form including certain wool blends (see note to 4.1.1). It is not applicable t
19、o unscoured, raw wool. 2 References The titles of the publications referred to in this standard are listed on the inside back cover. 3 Principle A known mass of wool is extracted in a Soxhlet apparatus with dichloromethane. The dichloromethane and extract is filtered, the solvent is evaporated and t
20、he residue is weighed. 4 Reagents and apparatus 4.1 Reagents 4.1.1 Dichloromethane (methylene chloride), complying with the requirements of BS 1994, boiling range 39 C to 41 C. When 100 ml of the solvent is evaporated the residue shall not exceed 1 mg. WARNING. This reagent is toxic; the use of a fu
21、me hood is recommended. NOTEDichloromethane will dissolve or cause a mass loss on some fibres, e.g. acetate, polyester and some types of nylon. If these fibres are present in a blend with wool, light petroleum of boiling range 40 C to 60 C should be used as the solvent. 4.1.2 Acetone, analytical rea
22、gent quality, complying with the requirements of BS 509-1. 4.2 Apparatus 4.2.1 Soxhlet extractors (see BS 2071), capacity 200 ml to 300 ml. 4.2.2 Extraction flasks flat-bottomed, capacity 250 ml to 500 ml. 4.2.3 Water-cooled reflux condensers (see BS 5922). 4.2.4 Heating unit temperature controlled,
23、 for use with the Soxhlet extractors. 4.2.5 Conical flasks 100 ml. 4.2.6 Distillation unit e.g. water or steam bath. 4.2.7 Balances a) With an accuracy of at least 50 mg, preferably with a large scale-pan. b) Analytical balance with an accuracy of 0.1 mg. 4.2.8 Desiccator 4.2.9 Drying oven 4.2.10 Fa
24、t-free filter papers1) 4.2.11 Funnel 5 Atmosphere for conditioning and testing The test shall be conducted in ordinary laboratory conditions. If the result is required to be expressed as a percentage of the conditioned mass of the fat-free specimen, prior to the testing the specimen shall be conditi
25、oned for not less than 24 h in the standard atmosphere for testing as specified in BS 1051 i.e. a relative humidity of 65 2 % and a temperature of 20 2 C. 6 Test sample Take a sample in accordance with BS 4658 that is representative of the bulk and of sufficient size for at least two specimens of 5
26、g to 20 g. If results are to be calculated based on the conditioned mass of the fat-free specimen (see 8.1), weigh the test specimen in the standard atmosphere to an accuracy of 0.05 g. If the results are to be calculated on a dry fat-free basis (see 8.2) weighing is not necessary at this stage, but
27、 condition the sample in the ordinary laboratory atmosphere for at least 24 h. NOTEIf it is necessary to pre-dry do not heat above 50 C. 7 Test procedure NOTELight petroleum should be used as the solvent if certain wool blends are being tested (see note to 4.1.1). Take a test specimen representative
28、 of the sample, of mass 5 g to 20 g. If desired a test specimen of mass not more than 10 g may be enclosed in a glass or paper thimble2). Assemble the extraction apparatus, place the specimen in the Soxhlet apparatus and pour dichloromethane slowly through the condenser until the siphon operates. Ad
29、d a further 10 ml to 20 ml of dichloromethane. Heat the flask (4.2.4) so that the dichloromethane siphons at least six times per hour for 4 h, if necessary adding more dichloromethane through the condenser. 1) Schleicher No 597, Whatman No. 2 are suitable. 2) Whatman thimble, 41 mm 123 mm, single th
30、ickness, previously extracted with dichloromethane, is suitable. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 2 BSI 08-1999 At the end of the prescribed time remove the specimen first allowing the solvent to drain back into t
31、he Soxhlet barrel. Siphon the solvent back into the flask and continue to distil the dichloromethane until approximately 25 ml of extract remains in the extraction flask. Filter the contents of the extraction flask into a 100 ml conical flask which has previously been dried, cooled and weighed. Wash
32、 the extraction flask and filter with three separate 10 ml portions of dichloromethane, ensuring that the filter paper is thoroughly washed to remove all traces of oil adding the filtrate to the conical flask. Evaporate the solvent (4.2.6). If any droplets of water are present in the conical flask,
33、add 2 ml to 5 ml of acetone and continue heating, repeating the process, if necessary, until no water is visible. Heat the conical flask for 30 min in an oven at 105 2 C. Introduce for a few seconds a tube connected to a pump and suck out vapour from the flask. Heat for a further 5 min in the oven,
34、cool in a desiccator and weigh. If the result of the test is to be expressed on the dry fat-free3) mass of the test specimen, determine the dry mass of the extracted specimen after drying to a constant mass4) at a temperature of 105 2 C. 8 Calculation and expression of results Calculate the mass of
35、the dry extract as a percentage as specified in 8.1 or 8.2. 8.1 For the conditioned mass of the fat-free, extracted specimen, the dichloromethane soluble extract (in %) is given by the formula: where m is the mass of the extract M is the conditioned mass of the test specimen before extraction 8.2 Fo
36、r the dry mass of the fat-free, extracted specimen, (dry fat-free basis) the dichloromethane soluble extract (in %) is given by the formula: where m is the mass of the extract Md is the dry mass of the extracted specimen 8.3 Calculate the mean of the results of two or more determinations and round t
37、o the nearest 0.1 %. 9 Test report The report shall include the following: a) Reference to this British Standard. b) The basis on which the results were calculated, i.e. conditioned mass of the fat-free specimen or dry fat-free basis. c) The mean result to the nearest 0.1 % calculated as specified i
38、n clause 8. d) Details of any deviation from the test method, e.g. the use of light petroleum as the solvent. 3) See foreword. 4) Constant mass is achieved when the residue suffers no more than 0.0005 g loss of mass on drying for a further 30 min. m100 Mm - - m100 Md - - Licensed Copy: sheffieldun s
39、heffieldun, na, Wed Nov 29 07:01:39 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3582:1981 BSI 08-1999 Publications referred to BS 509, Acetone for industrial use. BS 509-1, Specification. BS 1051, Glossary of terms relating to the conditioning, testing and mass determination of textiles. BS 1994,
40、Specification for dichloromethane (methylene chloride). BS 2071, Specification for Soxhlet extractors. BS 4658, Methods of test for textiles Preparation of laboratory test samples and test specimens for chemical testing. BS 5922, Specification for glass condensors for laboratory use. Licensed Copy:
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