1、BRITISH STANDARD BS4032:1978 Method of test for The determination of certain water-or alkali-soluble additives in cellulosic or synthetic fibres, yarns and fabrics or yarns and fabrics made from blends of such fibres UDC 677.46.07+677.494.07:677.014.25BS4032:1978 This British Standard, having been p
2、repared under the directionof the Fibres, Yarns andFabrics Standards Committee, was published underthe authority of the Executive Board on 31August1978 BSI 08-1999 First published May1966 First revision August1978 The following BSI references relate to the work on this standard: Committee reference
3、FBT/16 Draft for comment77/35821 DC ISBN 0 580 10255 6 Cooperating organizations The Fibres, Yarns and Fabrics Standards Committee, under whose direction this British Standard was prepared, consists of representatives from the following Government departments and scientific and industrial organizati
4、ons: Association of Jute Spinners and Manufacturers British Man-made Fibres Federation* British Nonwovens Manufacturers Association British Railways Board British Textile Employers Association* Central Council of the Irish Linen Industry Consumer Standards Advisory Committee of BSI Department of Ind
5、ustry, Chemicals and Textiles International Wool Secretariat* Knitting Industries Federation Ltd.* Manchester Chamber of Commerce and Industry Ministry of Defence* Narrow Fabrics Federation Retail Trading Standards Association Textile Institute* Warp Knitters Association The organizations marked wit
6、h an asterisk in the above list, together with the following, were directly represented on the committee entrusted with the preparation of this British Standard: British Carpet Manufacturers Association British Polyolefin Textiles Association British Textile Confederation Department of Industry, Lab
7、oratory of the Government Chemist Manchester Chamber of Commerce Testing House Soap and Detergent Industry Association Society of Dyers and Colourists Textile Research Council Wool Textile Delegation Amendments issued since publication Amd. No. Date of issue CommentsBS4032:1978 BSI 08-1999 i Content
8、s Page Cooperating organizations Inside front cover Foreword ii 1 Scope 1 2 References 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Test sample and test specimen 1 7 Test procedure 1 8 Calculation and expression of results 2 9 Test report 3 Publications referred to Inside back coverBS4032:1978 ii BS
9、I 08-1999 Foreword This British Standard was originally published by arrangement between the Textile Institute and the British Standards Institution and was based on Tentative Textile Standard No.74 (seeJ. Text. Inst., 1963,54, S6). The size used for spun textile yarns consists essentially of an adh
10、esive and a lubricant; an antiseptic may be present and sometimes hygroscopic and weighting materials are included. The adhesive is generally starch or soluble starch, but certain other carbohydrates, for example locust bean gum, and water- or alkali-soluble synthetic polymers, for example polyvinyl
11、 alcohol or polyacrylic acid, may be used alone or in mixtures with starch. The filling applied to cloth in finishing may contain starch or dextrins, with or without a lubricant, and sometimes a substantial proportion of weighting material such as china clay. Films of dried starch do not readily dis
12、solve in water but they are attacked and made soluble by amylases (i.e.starch-degrading enzymes) derived from malt, pancreatic extracts, or certain bacterial preparations. These enzymes are troublesome to prepare in the laboratory, but efficient commercial preparations of each type are available. Th
13、e procedure described in this British Standard is based on the one given in Shirley Institute Test Leaflet No. Chem4 but differs from it by the provision that, after the starch has been hydrolyzed by the enzyme, the specimens are treated in a solution of soap and soda ash which will also remove alka
14、li-soluble sizing materials such as acrylic and vinyl polymers. The procedure is applicable where test specimens of about2g are available. Weighting materials, if present, are mainly removed along with the starch; the residual amount of weighting material may be determined by ashing the desized spec
15、imen and, provided that the amount of residual mineral matter is small, changes in its mass produced during ashing may be neglected. Grey cotton and certain unbleached man-made fibres lose mass in the desizing process and a correction factor for the loss has to be applied to the mass of the residue.
16、 The correction factor can be determined if a specimen of the corresponding unsized yarn is available. In the absence of such a specimen, the values for the correction factor are assumed. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Stan
17、dards 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, pagesi andii, pages1 to4, an inside back cover and a back cover. This stan
18、dard 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.BS4032:1978 BSI 08-1999 1 1 Scope This British Standard describes a procedure for the quantitative removal of size and filling from cotton, vis
19、cose, or synthetic fibres, yarns and fabrics in which the adhesive is starch, a chemically-degraded starch, a vegetable gum or some other water- or alkali-soluble polymer. It is not applicable where the starch has been made insoluble, as in formaldehyde-containing finishes. The standard is not inten
20、ded for use when determining small amounts of residual starch or fatty materials. 2 References The titles of the publications referred to in this standard are listed on the inside back cover. 3 Principle A weighed amount of the dry sized material is extracted with light petroleum and then reweighed
21、accurately. The starch and gum are then removed by treating the extracted specimen, first in a suitable enzyme solution, and then in an alkaline soap solution, followed by hot water. The enzyme treatment is omitted when starch is shown to be absent when tested with iodine. The size 1)content is then
22、 the loss in dry mass, corrected for losses suffered by corresponding unsized material, and expressed as a percentage of the dry mass of the original unsized material. 4 Reagents The following reagents are required. 4.1 Light petroleum, boiling range40 C to60 C. 4.2 Amylase solution 2) . A solution
23、containing0.5%of active bacterial amylase specially prepared according to the manufacturers instructions and also containing a suitable amount of a nonionic wetting agent 3) . 4.3 Alkaline soap solution. A filtered solution containing5g/l of sodium oleate or other suitable high titre soap and2.5g/l
24、of anhydrous sodium carbonate. 4.4 Distilled or deionized water, as specified in BS3978. 5 Apparatus The following apparatus is required. 5.1 Sintered disk filter crucibles, porosity1 (seeBS1752), of capacity not less than60ml, fitted with a ground-glass stopper or other suitable cover. 5.2 Suitable
25、 ignition crucibles and covers 5.3 Muffle furnace, or other suitable equipment, for heating crucibles to a temperature of about700 C (dull red heat). 5.4 Soxhlet apparatus (seeBS2071). 5.5 Ventilated oven 5.6 Desiccator, containing self-indicating silica gel. 5.7 Analytical balance, accurate to0.000
26、2g. 5.8 Cellulose extraction thimble, 25mm 80mm. 6 Test sample and test specimen Take a sample representative of the bulk and sufficient for two or more test specimens, each approximately2g in mass. Follow the sampling procedure described in BS4658. Cut the specimens into pieces of convenient size f
27、or treatment in the crucible. 7 Test procedure 7.1 General instructions 7.1.1 Precautions. Do not handle the crucibles with bare hands during the drying, cooling and weighing operations. 7.1.2 Drying operations. Conduct all drying operations for4h to16h at105 3 C in a ventilated oven with the oven d
28、oor closed throughout. 7.1.3 Drying of crucibles and residues. Dry the filter crucible with its stopper or cover beside it. After drying, cover the crucible and transfer it quickly to a desiccator, putting no more than two crucibles in each desiccator. 7.1.4 Cooling. Conduct all cooling operations f
29、or30min with the desiccator beside the balance. 7.1.5 Weighing. After cooling, complete the weighing of the crucible within2min of its removal from the desiccator. Weigh to an accuracy of0.0002g. 1) The word “size” here and elsewhere in this British Standard includes, for brevity, “filling”. 2) Nerv
30、anase10X (A B M Industrial Products Ltd.,) is suitable. Amylases from other sources may be used but it is essential that the hydrolysis be performed at the optimum temperature and pH and with such additions as are required for maximum activity. The conditions may differ from those suitable for the n
31、amed enzyme. 3) It is essential that care be taken to use a wetting agent which is not an enzyme inhibitor.0.025%by mass of Lissapol NX (ICILimited) has been found to be suitable.BS4032:1978 2 BSI 08-1999 7.2 Procedure 7.2.1 Extraction with light petroleum ether. Place about2g of the prepared specim
32、en in the cellulose extraction thimble. Place in a Soxhlet apparatus and extract with light petroleum for1h at a minimum siphoning rate of6cycles per hour. Evaporate the extract in a tared100ml flask and determine the mass of residue according to the method described in BS3477. Transfer the extracte
33、d specimen to the tared crucible, dry the crucible and specimen and determine the mass of the dry specimen. 7.2.2 Removal of starch and gum. If starch is shown to be present by the iodine test, transfer the dried specimen to a250ml flask and add100ml of bacterial enzyme at70 C to the flask. Maintain
34、 this temperature for30min, shaking the contents of the flask by any convenient means, continuously or at5min intervals, during this time. Decant the solution through the filter crucible, add a fresh100ml portion of enzyme solution at70 C to the flask and repeat the extraction. Decant the second por
35、tion of solution through the filter crucible. Transfer the enzyme-treated specimen to a400ml beaker with200ml of alkaline soap solution. If starch is not present, transfer the dried specimen from the filter crucible to a400ml beaker and add200ml of the alkaline soap solution. Heat to70 C with stirri
36、ng and maintain at this temperature for30min. Collect the desized specimen in the filter crucible with suction and wash with3litres of hot tap water, then with500ml distilled water. If the washings are opalescent with mineral filling continue till clear. 7.2.3 Determination of dry mass of desized sp
37、ecimen. Dry the crucible and contents and determine the mass of the desized specimen. 7.3 Residual mineral filling If the sample is thought to contain a substantial amount of insoluble mineral filling, for example china clay, transfer the weighed desized specimen to an ignition crucible, which has b
38、een previously ignited with its lid at700 C, cooled and weighed. Place the open crucible at the front of the muffle furnace and burn off the fibre while manipulating the crucible lid to prevent the fibre from flaming. Move the crucible to the interior of the furnace, without the lid, and continue th
39、e combustion at700 C until no carbonaceous residue remains. Cool and weigh the crucible and its content, and calculate the mass of ash. Correct the mass of the desized specimen by subtracting the mass of ash. 8 Calculation and expression of results Fatty matter and adhesive/filler, if any, may be ca
40、lculated and reported separately as a percentage of the dry mass of the original unsized material. The percentage of total size is given by the following formula. If an unsized control is available, determine the value of f experimentally using the test procedure given in7.2 as the ratio. Otherwise
41、f may be assumed to have the following values: 1.03 for grey cotton 1.02 for unbleached viscose 1.00 for all other fibres For fibre mixtures and union fabrics containing a first component for which the factor is f 1 , and a second component for which the factor is f 2 , the factor f mfor the mixture
42、 of union is given by the following equation. where M is the dry mass of the sized specimen, after solvent extraction F is the mass of fatty matter extracted by solvent M d is the dry mass of the desized specimen, corrected where necessary by subtracting the mass of residual mineral filler as determ
43、ined by ashing the residue f is a factor for converting the mass of the dry desized specimen into the mass of the dry specimen before the addition of size. where P is the fractional proportion by mass of the first component in the mixture or union. Express the result to the nearest0.1%. 100 MFfM d +
44、() fM d - Dry mass of unsized control Dry mass of control after treatment - f m Pf 1 1 P ()f 2 + =BS4032:1978 BSI 08-1999 3 9 Test report The test report shall contain the following information. a) State that the test was conducted in accordance with this standard. b) State the total percentage of s
45、ize calculated as in clause8 for each specimen. c) State the fibre composition of the unsized specimen. d) Give details of any items likely to have had an effect on the result.4 blankBS4032:1978 BSI 08-1999 Publications referred to BS1752, Laboratory sintered or fritted filters. BS2071, Soxhlet extr
46、actors. BS3477, Determination of oils, fats and waxes in cotton. BS3978, Water for laboratory use. BS4658, Methods of test for textiles Preparation of laboratory test samples and test specimens for chemical testing. BS4032:1978 BSI 389 Chiswick High Road London W4 4AL BSIBritishStandardsInstitution
47、BSI is the independent national body responsible for preparing BritishStandards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions BritishStandards are updated by amendment or revision. Users of BritishStandards should make
48、sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this BritishStandard would inform the Secretary of the technical committee respon
49、sible, the identity of which can be found on the inside front cover. Tel:02089969000. Fax:02089967400. BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of standards. Buying standards Orders for all BSI, international and foreign standards publications should be addressed to Customer Services. Tel:02089969001. Fax:02089967001.
