1、BRITISH STANDARD BS 8459:2005 Incorporating Corrigendum No. 1 Determination of extractable matter in textiles Method ICS 59.080.01 BS 8459:2005 This British Standard was published under the authority of the Standards Policy and Strategy Committee on 28 April 2005 BSI 16 May 2005 The following BSI re
2、ferences relate to the work on this standard: Committee reference TCI/80 Draft for comment 02/122925 DC ISBN 0 580 45860 1 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee TCI/80, Chemical testing of textiles, upon which t
3、he following bodies were represented:Association of Consulting Scientists British Apparel and Textile Confederation British Measurement and Testing Association British Retail Consortium British Textile Technology Group Carpet Foundation Co-operative Union Defence Procurement Agency Home Laundering C
4、onsultative Council Laboratory of the Government Chemist SATRA Technology Centre Society of Dyers and Colourists Textiles Institute UK Cleaning Products Industry Association UKTLF UK Textile Laboratory Forum Woolmark Company Co-opted members Amendments issued since publication Amd. No. Date Text aff
5、ected 15668 16 May 2005 Correction to titleBS 8459:2005 BSI 16 May 2005 i Contents Page Committees responsible inside front cover Foreword ii 1S c o p e 1 2 Normative references 1 3 Definition 1 4 Principle 1 5 Solvents and testing apparatus 1 6 Atmosphere for testing and conditioning 2 7T e s t s a
6、 m p l e 2 8 Test procedure 2 9 Calculation and expression of results 3 10 Test report 5 Annex A (normative) Solvents for extraction 6 Table A.1 Solvents for extraction 6BS 8459:2005 ii BSI 16 May 2005 Foreword This British Standard was prepared by TCI/80. Textiles can contain solvent extractable su
7、bstances that do not constitute an integral part of their component fibres. These can originate from the raw materials themselves, or be lubricants added to assist processing, detergents or surfactants applied in scouring, and special finishing agents. The total amount of these substances will depen
8、d on the type and stage of manufacture of the material, and its estimation is important for determining the clean fibre content of a sample. In general, different substances cannot be extracted individually, unless there are known specific solubilities and selective solvents available. It is possibl
9、e, however, to extract types of material from textiles, e.g. fatty/oil based substances and water-soluble salts, and to use particular solvents to provide a degree of separation of the different components present. This standard describes a general procedure for the extraction of certain soluble mat
10、erials from textiles using organic solvents by conventional Soxhlet extraction. Suitable solvents for the estimation of particular types of substance from individual fibre types or blends are given in Annex A. This standard is drafted from the following standards that have been withdrawn: BS 3477:19
11、62, Method for the determination of oils, fats and waxes in cotton; BS 3582:1981, Method for determination of oils, fats and waxes in wool; BS 3845:1990, Method for determination of added oil content of jute yarn, rove and fabric. Future revisions of this standard will reflect other developments in
12、extraction techniques such as micro-extraction, accelerated solvent extraction and supercritical fluid extraction. Use of chlorinated solvents such as dichloromethane might well become unacceptable in the future and alternative extractants will need to be developed. At present other types of extract
13、able matter in other fibre types and blends are routinely determined, in some instances using solvents other than those mentioned in Annex A. When sufficient data is available to validate such procedures, these could also be incorporated. CAUTION In addition to removing extractable substances, some
14、solvents in use can also dissolve material from within the structure of the textile itself. The selection of the most appropriate solvent for any particular textile fibre/extractable matter combination is therefore of the utmost importance and should be based on sound knowledge of the materials conc
15、erned. While the solvents given in Annex A are believed to be suitable for the fibre- extract examples shown, no responsibility can be accepted for any undesired effects that can occur. Light mineral oil, as an oil-in-water emulsion, is added to jute fibres during conversion to yarn, and some or all
16、 of this oil is present in jute at later stages of manufacture. This standard describes a method for the determination of added oil in jute, based on the extraction of the oil by an organic solvent. All organic solvents, however, extract some of the natural constituents of jute and an allowance has
17、to be made in quantitative determinations of the added oil. The solvent used in this method has been found to extract less of the natural constituents than any other common solvent, and hence the necessary allowance is at a minimum. Depending on the type used, the procedure extracts between 0.1 % an
18、d 0.2 % of the natural constituents of the jute. WARNING This British Standard calls for the use of substances that may be injurious to health if adequate precautions are not taken. It refers only to technical suitability and does not absolve the user from legal obligations relating to health and sa
19、fety at any stage. It has been assumed in the drafting of this British Standard that the execution of its provisions is entrusted to appropriately qualified and experienced people.BS 8459:2005 BSI 16 May 2005 iii A British Standard does not purport to include all the necessary provisions of a contra
20、ct. 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 front cover, an inside front cover, pages i to iii, pages 1 to 6 and a back cover. Th
21、e BSI copyright notice displayed in this document indicates when the document was last issued.blankBS 8459:2005 BSI 16 May 2005 1 1 Scope This British Standard describes a method for the determination of certain types of extractable matter in certain textiles with solvents, as listed in the Annex A.
22、 It is applicable to materials in any form but, where the textile is of a dense construction, certain preparations might be necessary to ensure adequate penetration and accessibility of the solvent used. 2 Normative references The following referenced documents are indispensable for the application
23、of this document. For dated references, only the reference cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. BS 245, Specification for mineral solvents (white spirit and related hydrocarbon solvents) for paints and other purposes
24、. BS 1994, Specification for dichloromethane (methylene chloride). BS 2071, Specification for Soxhlet extractors. BS 5922 (ISO 4799), Specification for glass condensers for laboratory use. BS ISO 6348, Textiles Determination of mass Vocabulary. ISO 139, Textiles Standard atmospheres for conditioning
25、 and testing. ISO 5089, Textiles Preparation of laboratory test samples and test specimens for chemical testing. 3 Definition The terms and definitions in BS ISO 6348 apply. 4 Principle A known mass of the textile is extracted in a Soxhlet apparatus with solvent. The extract is filtered, the solvent
26、 is evaporated and the residue is weighed. 5 Solvents and testing apparatus 5.1 Solvents Suitable solvents are: a) dichloromethane as specified in BS 1994; and b) light petroleum as specified in BS 245. These shall be selected as specified in Annex A. 5.2 Apparatus 5.2.1 Soxhlet extractors, conformi
27、ng to BS 2071, with a capacity of 100 ml to 300 ml. 5.2.2 Extraction flasks, with a capacity of 250 ml to 500 ml. NOTE The volume of the flask should be greater than that of the extractor barrel, e.g. for a 300 ml barrel, a 500 ml flask is suitable. 5.2.3 Cooled reflux condensers, conforming to BS 5
28、922. 5.2.4 Temperature-controlled heating unit, for use with the Soxhlet extractors. 5.2.5 Conical flasks, with a minimum capacity of 150 ml, in order to hold 25 ml extract, plus three separate 30 ml portions of fresh solvent. 5.2.6 Temperature-controlled distillation/heating unit, e.g. water or ste
29、am bath, or electrical heating device. 5.2.7 Suction pump and adapter, available for use when jute fibres are extracted. 5.2.8 Balances. Two balances are required:BS 8459:2005 2 BSI 16 May 2005 a) an analytical balance with an accuracy of 0.1 mg; b) a second balance with an accuracy of 50 mg for det
30、ermining the approximate weight of the textile prior to testing. 5.2.9 Desiccator, having fresh desiccant to absorb moisture. 5.2.10 Drying oven, with an adjustable temperature control. 5.2.11 Sintered glass extraction thimbles, sintered glass, having a porosity of 1. 5.2.12 Cellulosic extraction th
31、imbles, for routine measurements, of a size suitable for the extractor being used and previously extracted with the solvent to be used in the determination concerned. See Clause 8. NOTE Cellulosic thimbles can absorb moisture during the weighing process. Rapid weighing is needed to obtain a correct
32、result. 5.2.13 Glass wool. 6 Atmosphere for testing and conditioning The test shall be conducted in normal laboratory conditions. Conditioning shall be carried out in accordance with the requirements of ISO 139 for a minimum of 24 h. 7 Test sample Take a sample representative of the bulk in accordan
33、ce with ISO 5089 that is sufficient for at least two specimens of 5 g to 20 g. If the results are to be calculated on a dry, extract-free basis (see 9.2), weighing is not necessary at this stage. Condition the sample in the normal laboratory atmosphere for at least 24 h in accordance with ISO 139. I
34、f the results are to be calculated on the basis of the unconditioned mass of the sample as received, weigh the sample. Conditioning is unnecessary. 8 Test procedure Take two test specimens, of mass 5 g to 20 g (duplicate determinations are made). Enclose each specimen in a clean, previously tared gl
35、ass extraction thimble, or a cellulosic thimble previously extracted with the solvent to be used for the extraction. If it is considered that there is a likelihood of fibrous material being lost from the specimen during extraction, cover the top of the thimble with a glass wool plug to prevent such
36、loss during siphoning. Assemble the extraction apparatus, place the specimen (contained in the thimble) in the barrel of the Soxhlet apparatus and pour solvent slowly through the condenser until the siphon operates. Allow the siphon to complete, then add further solvent until the Soxhlet barrel is a
37、pproximately half full. Do not overfill the barrel. Heat the flask (5.2.2) so that the solvent is siphoned as follows: for cotton, at a rate of 6 times per hour for 3 hours; for wool, at a rate of 6 times per hour for 4 hours; for jute, not less than 10 times. If necessary, more solvent should be ad
38、ded through the condenser. NOTE Thermal decomposition of the extract can occur if too little solvent is used. This is important if chemical characterization is to be carried out on the extract.BS 8459:2005 BSI 16 May 2005 3 The procedure adopted for evaporation of the solvent depends on the fibre. a
39、) For cotton and wool, evaporate the solvent using the apparatus specified in 5.2.6. At the end of the prescribed extraction time and after cooling, remove the thimble and specimen, first allowing all solvent to drain back into the Soxhlet barrel. Siphon the solvent back into the flask and continue
40、to distil, emptying the barrel as it becomes full and collecting the distilled solvent. When approximately 25 ml of solventextract mixture remains in the extraction flask, filter the contents of the flask into a clean, previously tared 100 ml conical flask. Wash the extraction flask and filter with
41、not more than three separate 30 ml portions of fresh solvent if cellulosic thimbles are used, or not more than two if glass thimbles are used, ensuring that the glass wool plug is thoroughly washed to remove all traces of extract, and adding the filtrate to the conical flask. b) For jute, disconnect
42、 the apparatus and remove the bulk of the solvent by distillation. Remove the remainder of the solvent by the following method. Connect the flask (5.2.2) by means of a suitable adapter to a suction pump (5.2.7). Reduce the pressure in the flask to 1.33 kPa to 4.00 kPa if possible for not less than 1
43、2 min and not more than 15 min while warming the flask at 60 C to 65 C. Release the vacuum through a side tube fitted with a cotton wool filter before disconnecting the adapter. If the pressure of 1.33 kPa to 4.00 kPa cannot be obtained, pass a stream of air through the flask using the following met
44、hod. Stopper the flask with a stopper containing an inlet and outlet tube, neither of which projects below the neck of the flask. Heat the flask on water bath at 60 C to 65 C, and by means of a vacuum supply draw a stream of air (3 000 ml/min measured at atmospheric pressure) through the flask for 1
45、5 min, with the pressure inside the flask reduced to approximately 26.60 kPa. For all fibre types, place the test specimen contained in the extraction thimble in a drying oven at an appropriate temperature (this will depend on the textile being tested generally, 105 C is used), and dry for four hour
46、s. At the end of this period, remove the thimble and the specimen from the oven and allow it to cool in a desiccator. Remove the paper from the thimble, taking care not to lose any fibrous matter, and determine the constant mass of the thimble plus specimen. Heat the conical flask for 30 min at a te
47、mperature at which the solvent will be driven off, but the extract unaffected. NOTE This temperature will vary for different solvent and extractable matter combinations. Introduce a tube connected to a suction pump into the volume of the conical flask for several seconds to extract residual solvent
48、vapour, without allowing contact with the extracted matter at the bottom of the flask. Heat for a further 15 min in the drying oven, then cool in the desiccator and weigh until constant mass has been achieved. 9 Calculation and expression of results 9.1 General Subtract the mass of the clean, tared
49、conical flask from the mass of the dried flask and its extract to obtain the mass of the extract. Subtract the mass of the tared extraction thimble from that of the thimble plus specimen to determine the dry mass of the extracted specimen. 9.2 Wool and cotton 9.2.1 If the result is to be expressed on the dry, extract-free mass of the tested specimen, calculate the amount of extractable matter as follows: where m extractable is the percentage extractable matter (g)
