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1、BRITISH STANDARD BS 3568:1988 Method for Determination of solubility of wool in alkali UDC 677.31.01:541.8 Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 This British Standard, having been prepared under the direction of the Te
2、xtiles and Clothing Standards Committee, was published under the authority of the Board of BSI and comes into effect on 30 September 1988 BSI 11-1999 First published November 1962 First revision September 1988 The following BSI references relate to the work on this standard: Committee reference TCM/
3、26 Draft for comment 87/38081 DC ISBN 0 580 16674 0 Committees responsible for this British Standard The preparation of this British Standard was entrusted by the Textiles and Clothing Standards Committee (TCM/-) to Technical Committee TCM/26, upon which the following bodies were represented: Britis
4、h Carpet Manufacturers Association Ltd. Department of Trade and Industry (Laboratory of the Government Chemist) International Wool Secretariat Man-made Fibres Producers Committee Ministry of Defence Textile Research Council Amendments issued since publication Amd. No.Date of issueComments Licensed C
5、opy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 BSI 11-1999i Contents Page Committees responsibleInside front cover Forewordii 1Scope1 2Principle1 3Reagents1 4Apparatus1 5Test specimens1 6Procedure1 7Expression of results2 8Test report2 P
6、ublications referred toInside back cover Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 ii BSI 11-1999 Foreword This British Standard has been prepared under the direction of the Textiles and Clothing Standards Committee and is
7、 a revision of BS 3568:1962, which is withdrawn. The appendix, which described a method for determining acid content, has been omitted and is published separately as BS 6981:1988. This is because there may be reasons for wishing to determine acid content other than for correcting alkali solubility v
8、alues, e.g. when investigating finishing faults, cases of skin irritation, etc. The solubility of wool in alkali provides a useful index of the extent of the change in its chemical properties brought about by certain agencies. Treatment with acids or with oxidizing or reducing agents, or exposure to
9、 heat or light, causes an increase in the solubility, whereas treatment with mild alkali, as used in normal processing, or with crosslinking agents causes the solubility to decrease. The more severe the treatment, the greater is the change in solubility. The test is most useful when an untreated con
10、trol sample is available and when the nature of the treatment of the sample under test is known. When the sample has been treated by two agencies having opposite effects on the solubility, the interpretation of the results, even when an untreated control sample is available, is difficult, and other
11、tests are necessary to supplement the information. This British Standard is technically equivalent to ISO 3072:1975. A British 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
12、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 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 amendm
13、ents incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 BSI 11-19991 1 Scope This British Standard describes a method for determination of the s
14、olubility of wool in alkali. This procedure is applicable to wool textiles in any form, i.e. loose fibre, silver, roving, yarn or fabric, but is not applicable if the specimen has been dyed with any metallized dye. NOTEThe titles of the publications referred to in this standard are listed on the ins
15、ide back cover. 2 Principle A test specimen is immersed in a solution of sodium hydroxide of known concentration under specified conditions of time, temperature and volume. The loss in mass is determined as the difference between the dry masses of the test specimen before and after treatment. 3 Reag
16、ents 3.1 Sodium hydroxide solution, c(NaOH), 0.1 mol/L. 3.2 Acetic acid solution. Dilute 10 mL of glacial acetic acid, approximately 99.7 % (m/m), approximately 1.06 g/mL, to 1 L with water (3.3). 3.3 Water, complying with grade 3 of BS 3978. 3.4 Petroleum spirit, boiling range 40 C to 60 C. 4 Appar
17、atus 4.1 Soxhlet extraction apparatus, complying with BS 2071. 4.2 Water-bath, thermostatically controlled at 66 0.5 C. 4.3 Conical flasks, 100 mL capacity, fitted with stoppers. 4.4 Sintered-glass filter crucibles, 30 mL capacity, of porosity P160 complying with BS 1752. NOTEIf possible, these cruc
18、ibles should have ground glass stoppers. 4.5 Filter-flask, filter-pump and adaptor 4.6 Ventilated oven, for drying specimens at 105 3 C. 4.7 Stoppered weighing bottles, for weighing the test specimens. 4.8 Balance, accurate to 0.0002 g. 4.9 Desiccator 5 Test specimens Take a sample representative of
19、 the bulk and not less than 10 g, sufficient to provide wool for the following test specimens: a) one test specimen weighing approximately 1 g for determining the dry mass (see 6.2); b) two test specimens each weighing approximately 1 g for determining the solubility in alkali (see 6.3). NOTE 1If it
20、 is suspected that the sample contains acid (see 6.4) two further test specimens each weighing approximately 2 g may be taken from the sample for determining acid content by the method described in BS 6981. NOTE 2Useful information on sampling is given in BS 2545. NOTE 3The precision of results may
21、be quite high given a very uniform sample, but, for example, with samples from bleached wool, or with samples having an alkali solubility of 20.0 % (m/m), the variations within the batch may be 2 % or more and fresh test specimens may be needed. 6 Procedure 6.1 Preparation of sample Extract the samp
22、le in the Soxhlet extraction apparatus (4.1) with petroleum spirit (3.4) for 1 h at a minimum rate of six cycles per hour. Allow the petroleum spirit to evaporate and then remove all vegetable and other obvious foreign matter. Disintegrate the sample into short lengths of approximately 10 mm and all
23、ow it to come to equilibrium within the laboratory atmosphere. 6.2 Determination of dry mass Place the 1 g test specimen (see clause 5) in a weighing bottle (4.7) and dry it in the ventilated oven (4.6) at 105 30 C. Stopper the bottle, cool it in the desiccator (4.9) and weigh it. Repeat these dryin
24、g, cooling and weighing operations until the results of two consecutive weighings do not differ from each other by more than 0.0005 g, i.e. the mass is virtually constant. Remove the test specimen, weigh the weighing bottle and hence calculate the dry mass of the test specimen. 6.3 Determination of
25、solubility in alkali Measure 100 mL portions of the sodium hydroxide solution (3.1) into separate flasks (4.3), stopper loosely, and fix the flasks in the water-bath (4.2) by any suitable means so that the level of the water outside the flasks is at least 50 mm higher than the level of the solution
26、inside. NOTEThis procedure is essential for precise control of temperature. When the temperature of the sodium hydroxide solution reaches 65 0.5 C, introduce separate test specimens of known mass (see clause 5) into the flasks, replace the stoppers and gently shake the flasks to ensure complete wett
27、ing of the test specimens. Shake the flasks gently again after 15, 30 and 45 min, the time of shaking not exceeding 5 s on each occasion. Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 2 BSI 11-1999 After 1 h transfer the conte
28、nts of each flask to separate sintered-glass filter crucibles (4.4) of known mass and drain the crucibles by suction. Wash any fibrous material remaining in each flask into the crucibles with water (3.3). Wash each residue in each crucible six times with water (3.3), draining completely after each w
29、ash, and release the suction. Fill each crucible twice successively with the acetic acid solution (3.2). Allow to stand for 1 min and drain each crucible by suction. Finally, wash each residue six times with water (3.3), draining completely between each wash. Dry the crucibles and contents at 105 3
30、C for 3 h minimum, cool them in the desiccator and weigh them. Repeat these drying, cooling and weighing operations until the results of two consecutive weighings do not differ from each other by more than 0.0005 g, i.e. the mass is virtually constant. 6.4 Determination of acid content Determine the
31、 pH of the aqueous extract by the method described in BS 3266. If an aqueous extract of the material has a pH value less than 4.0, determine the acid content by the method described in BS 6981. 7 Expression of results 7.1 Samples not containing acid The solubility in alkali, S, calculated as the los
32、s in mass of the test specimen and expressed as a percentage of its calculated dry mass, is given by the equation: S = 100 7.2 Samples containing acid The corrected solubility in alkali, S, calculated as the loss in mass of the test specimen and expressed as a percentage of its calculated dry, acid-
33、free mass, is given by the equation: S = (S s) Express the results to one decimal place. 8 Test report The test report shall include the following information: a) the number and date of this British Standard, i.e. BS 3568:1988; b) a description or reference of the sample tested; c) the individual re
34、sults and their mean, expressed as in clause 7; d) any departure from the method described, e.g. owing to insufficient material being available. where m1is the dry mass of the test specimen determined as described in 6.2 (in g); m2is the dry mass of the residue determined as described in 6.3 (in g).
35、 m1m2 m1 - where Sis the solubility in alkali calculated as described in 7.1; sis the percentage of acid determined as described in BS 6981. 100 100s - - Licensed Copy: sheffieldun sheffieldun, na, Wed Nov 29 07:03:54 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS 3568:1988 BSI 11-1999 Publications r
36、eferred to BS 1752, Specification for laboratory sintered or fritted filters including porosity grading. BS 2071, Specification for Soxhlet extractors. BS 2545, Methods of fibre sampling for testing. BS 3266, Methods of test for determination of conductivity, pH, water-soluble matter, chloride and s
37、ulphate in aqueous extracts of textile materials. BS 3978, Specification for water for laboratory use. BS 6981, Method for determination of acid content of wool. ISO 3072, Wool Determination of solubility in alkali1). 1) Referred to in the foreword only. Licensed Copy: sheffieldun sheffieldun, na, W
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