1、BRITISH STANDARD BS3090:1978 Incorporating Amendment No.1 Method of test for The determination of the cuprammonium fluidity of linen materials UDC 677.11.07:532.132:546.562.39145BS3090:1978 This British Standard, having been prepared under the directionof the Fibres, Yarns andFabrics Standards Commi
2、ttee, was published underthe authority of the Executive Board on 31January1978 BSI11-1999 First published February1959 First revision January1978 The following BSI references relate to the work on this standard: Committee referenceTCM/26 Draft for comment76/35805DC ISBN 0 580 09538 X Cooperating org
3、anizations 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 organizations: Association of Jute Spinners and Manufacturers British Man-made F
4、ibres Federation* British Nonwovens Manufacturers Association British Railways Board British Textile Employers Association* Central Council of the Irish Linen Industry Consumers Standards Advisory Committee of BSI Department of Industry, Chemicals and Textiles International Wool Secretariat* Knittin
5、g Industries Federation Ltd* Manchester Chamber of Commerce and Industry Ministry of Defence* Narrow Fabrics Federation Retail Trading Standards Association Textile Institute* Warp Knitters Association Ltd. The organizations marked with an asterisk in the above list, together with the following, wer
6、e 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, Laboratory of the Government Chemist Manchester Chamber of Commerce
7、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 Comments 4964 November 1985 Indicated by a sideline in the marginBS3090:1978 BSI 11-1999 i Contents Page Cooperating org
8、anizations Inside front cover Foreword ii 1 Scope 1 2 References 1 3 Principle 1 4 Definitions 1 5 Reagents 1 6 Apparatus 1 7 Conditioning and testing atmosphere 1 8 Calibration of solution bottle 2 9 Test specimens 2 10 Test procedure 2 11 Calculation and expression of results 3 12 Test report 3 Ap
9、pendix A Cleansing of apparatus 4 Appendix B Preparation of the solvent 4 Appendix C Determination of copper 4 Appendix D Determination of ammonia 4 Appendix E Determination of nitrite 4 Figure 1 Polyethylene bottle and accessories 1 Figure 2 Filling the viscometer 3 Publications referred to Inside
10、back coverBS3090:1978 ii BSI 11-1999 Foreword The first edition of this standard was based on Tentative Textile Standard No.45 which was adopted from the method used by the Linen Industry Research Association (now the Lambeg Industrial Research Association) as described in the Journal of the Textile
11、 Institute, September1957,P675. Unbleached or partially bleached linen materials usually contain fragments of lignified tissues insoluble in a cuprammonium hydroxide solution. These have to be removed by a preliminary treatment before reliable measurements of fluidity can be made with a capillary ou
12、tflow viscometer. This revision, although similar in principle to the first edition, specifies a simplified procedure and apparatus for preparation of the cellulose solution, making the test more appropriate for use in quality control, where it has its greatest application. Experience has shown that
13、 this simplified method is as reproducible as that described in the first edition of this standard. As in that edition, reference is made to BS2610 for a detailed description of the viscometer and its calibration, and the standard cuprammonium solvent. Guidance on the cleansing of apparatus is given
14、 in Appendix A and the other appendices contain information on the preparation of the cuprammonium hydroxide solution. NOTECuprammonium fluidity is the reciprocal of the dynamic viscosity of a solution of cellulose of prescribed concentration in a cuprammonium solvent of prescribed composition measu
15、red under precisely defined conditions. These solutions commonly exhibit non-newtonian flow behaviour. Cuprammonium fluidity does not, therefore, have absolute physical significances as does the fluidity of a newtonian liquid, although it has been expressed in reciprocal poises. It is considered tha
16、t it should be regarded as an empirical quantity and because of this, the results are given in “units of cuprammonium fluidity”. 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. Compli
17、ance 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 standard has been updated (see copyright date) and may have had
18、 amendments incorporated. This will be indicated in the amendment table on the inside front cover.BS3090:1978 BSI 11-1999 1 1 Scope This British Standard specifies a method for the determination of cuprammonium fluidity of linen materials. 2 References The titles of the publications referred to in t
19、his standard are listed on the inside back cover. 3 Principle The material under test is first pretreated in sodium hydroxide to remove non-cellulosic matter and soluble modified cellulose. A specimen is then dissolved in the standard cuprammonium solution and the cuprammonium fluidity of the result
20、ing solution is determined. 4 Definitions For the purposes of this British Standard the following definitions apply. 4.1 kinematic fluidity (of a solution) the reciprocal of the kinematic viscosity of the solution 4.2 cuprammonium fluidity (of a specimen of linen) the kinematic fluidity (expressed i
21、n “units of cuprammonium fluidity”) of a solution in the standard cuprammonium solvent containing0.5g of the dry pretreated material per100ml of solution divided by the density of the solution. A value of0.94g/m 3for the density is sufficiently accurate 5 Reagents The reagents used shall be of analy
22、tical grade and the following are required. 5.1 Sodium hydroxide solution,20g/l. 5.2 Sulphuric acid solution,2.5g/l. 5.3 Sodium bicarbonate solution,1g/l. 5.4 Standard cuprammonium solution, prepared as described in BS2610 and consisting of15 0.1g/l copper,200 5g/l ammonia and less than0.5g/l nitrou
23、s acid 1) . Guidance on the preparation of the solution is given in Appendix B, Appendix C, Appendix D and Appendix E. If a stock solution is used, it shall be free from any deposit. 5.5 Bromocresol purple indicator (see BS4123) 6 Apparatus 6.1 Solution bottle, (see Figure 1) of polyethylene with a
24、plug insert and cap and a separate filter cap fitted with a polyurethane foam filter disc and of approximate volume34ml. Alternatively, equivalent apparatus capable of dissolving, filtering and transferring the solution with minimum exposure to air and light may be used. 6.2 Four stainless steel bal
25、ls, of6mm diameter. 6.3 Stainless steel rod, about300mm long. 6.4 Calibrated viscometer, complete with glass jacket, brass supports, blackened glass container, rotating device, glass thermostat and stopwatch, all as specified in BS2610. 7 Conditioning and testing atmosphere Conditioning shall be car
26、ried out in the standard temperate atmosphere for conditioning and testing textiles defined in BS1051. Since testing is carried out in a temperature controlled water bath, it is not necessary to use this atmosphere for testing. 1) For details of the source of a suitable solution write to Enquiry Sec
27、tion (London), BSI,2 Park Street, London W1A2BS, sending a stamped addressed envelope for a reply. Figure 1 Polyethylene bottle and accessoriesBS3090:1978 2 BSI 11-1999 8 Calibration of solution bottle Place the stainless steel balls in the solution bottle and fill it with distilled water at20 C, ta
28、king care to tap out any entrapped air bubbles. Push the plug insert half-way into the neck of the bottle and then push fully home by screwing on the cap. To prevent inadvertent squeezing of the bottle while screwing on the cap, the bottle may be placed in a closely fitting hole bored in a block of
29、wood. Carefully remove the screw cap without squeezing the bottle and dry any excess water with filter paper. The difference between the mass, measured to an accuracy of 0.1mg, of the bottle, containing the steel balls when empty and when full of water gives the volume of the liquid it holds. 9 Test
30、 specimens From the volume of the solution bottle, calculate the mass of boiled and conditioned linen cellulose required to give an0.5% m/v solution in the cuprammonium solvent, assuming a moisture content of7%. Samples should be sufficiently larger than this to allow for loss during removal of non-
31、fibrous matter and pretreatment. 10 Test procedure 10.1 Removal of non-fibrous matter. The material under examination shall be free from appreciable amounts of non-cellulosic substances that are not removed by the pretreatment described in10.2. Some methods for the removal of non-fibrous matter are
32、given in Handbook No.11. Attention is drawn to the fact that some of these methods may cause degradation of the cellulose. 10.2 Pretreatment. Using a liquor specimen ratio of approximately250:1, boil the specimen for6h in sodium hydroxide solution in a500ml conical flask under a reflux condenser wit
33、h ground glass joints, thus removing any remaining non-cellulosic matter and soluble modified cellulose. Boil vat-dyed materials away from direct sunlight. After boiling, wash the material in hot water until it is as free as possible from alkali, immerse it for5min in the sulphuric acid solution and
34、 again wash it with water. Then immerse it for5min in the sodium bicarbonate solution and, finally, wash with water until a purple colour is obtained on spotting the material with bromocresol purple indicator. Allow it to dry at room temperature and cut it into fine shreds,1mm to2mm in length. If he
35、avy or closely woven cloths are being tested, separate the warp and weft yarns before the pretreatment and test them separately. 10.3 Conditioning. Expose the shredded material to the conditioning atmosphere for2h. 10.4 Preparation of the cellulose solution. Take sufficient of the pretreated sample
36、weighed to the nearest milligram to give an0.5% m/v solution in the cuprammonium hydroxide solvent, assuming a7% moisture content of the specimen. Place the specimen in the solution bottle with the four steel balis. Half-fill the bottle with the cuprammonium solvent and gently shake until the specim
37、en is completely wetted out. When the material is difficult to wet, this process may be assisted by dispersing the shredded linen with the stainless steel rod. Wash down the rod with cuprammonium solvent while it is being withdrawn from the bottle. Then completely fill the bottle with solvent using
38、the technique described in clause8 for its calibration. Revolve it overnight excluding light. Remove the screw cap from the bottle and ease out the plug insert. Fit a small filter disc of polyurethane foam cut out with a cork borer inside the filter cap and screw this assembly on to the bottle. Inve
39、rt the bottle over the open end of the viscometer, the capillary end of which is closed by a clipped rubber tube. Squeeze the solution through the filter disc and into the viscometer as shown in Figure 2. Close the top of the viscometer with a suitable stopper. In most cases the bottle will need to
40、be squeezed twice in order to fill the viscometer and shall be returned to its upright position between squeezes to avoid passing air bubbles through the solution. As a check on the mixing and filtering, squeeze the first few drops of filtrate on to a clean glass plate and immediately examine for un
41、dissolved cellulose by holding the plate up to the light and looking through it; this may also be done with a few drops after filling the viscometer. Examine the residue in the bottle for undissolved cellulose. If undissolved cellulose is present in excessive amounts the test is not valid and reason
42、s for non-dissolution should be sought e.g.resin treatment and use of reactive dyestuffs. Protect the solution from direct sunlight during its transfer to the viscometer and until measurement is completed. BS3090:1978 BSI 11-1999 3 10.5 Measurement of viscosity. Remove the clipped rubber tube from t
43、he capillary end of the viscometer, mount the viscometer vertically in a jacket within the water bath and allow the temperature to reach equilibrium. Remove the upper closure so as to allow the solution to flow freely through the capillary into a reservoir attached to the jacket. Observe the meniscu
44、s against the light from the vertical striplight, and measure by means of the stopwatch the times, in seconds, for the meniscus to fall from the top to the intermediate, and from the top to the bottom marks. Only the time from the top mark to the bottom mark is required for calculating the fluidity.
45、 The intermediate reading serves to detect any considerable irregularity that would indicate a partial choking of the capillary. Information on the use of the middle timing mark is given in BS2610. 11 Calculation and expression of results Calculate and express the cuprammonium fluidity of the soluti
46、on as follows: The values of C and K are derived from the calibration of the viscometer and are stated on the calibration certificate. NOTEThese values are customarily expressed in c.g.s. units on the calibration certificates supplied with the viscometer in accordance with BS2610. If they are given
47、in SI units the calculated result (ins/mm 2 ) may be converted to “units of cuprammonium fluidity” by multiplying it by100. 12 Test report The report shall state the following: a) that the test was carried out in accordance with BS3090; b) the cuprammonium fluidity of the linen as calculated in clau
48、se11; c) any factors that may have an effect on the test result. Figure 2 Filling the viscometer where F is the cuprammonium fluidity in “units of cuprammonium fluidity” t is the time of outflow in seconds between the top and bottom marks is the density of the solution taken to be0.94g/cm 2 C is the
49、 viscometer constant in reciprocal poises per second K is the kinetic energy correction constant of the viscometer in s 2 F C tK/t - =BS3090:1978 4 BSI 11-1999 Appendix A Cleansing of apparatus Empty the viscometer and rinse with water immediately after the determination is complete to remove the cuprammonium solution. Immerse in a cold acidified solution of potassium dichromate or sodium dichromate for2h, thoroughly rinse with water and dry at room temperature. CAUTION. The cleansing agent is a corrosive oxidizing agent and should be handle
