1、BRITISH STANDARD Plastics - Cellulose acetate - Determination of viscosity loss on moulding The European Standard EN IS0 1599:1999 has the status of a British Standard ICs 83.080.20 BS EN IS0 1599: 1999 U- NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGH LAW STD-BSI BS EN IS0 L599-E
2、NGL 3777 E lb2Libb7 0830342 323 D direction of the Sector Committee for Materiais and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 August 1999 Amd. No. O BSI 08-1999 BS EN IS0 15991999 Date Comments National foreword This British Standard is the
3、 English language version of EN IS0 1599:1999. It is identical with IS0 1599 1990. The UK participation in its preparation was entrusted to Technical Committee PRl/“, Thermoplastic Materials, which has the responsibiliy to: - aid enquirers to understand the text; - present to the responsible interna
4、tionalEuropean committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed - monitor related intemational and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its se
5、cretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publication
6、s referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index“, or by using the “Find“ facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include ail the necessary provisions
7、 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 front cover, an inside front cover, the EN IS0 title page, the EN IS0 for
8、ward page, the IS0 title page, page ii, pages 1 to 4, the annex ZA page and a back cover. The BSI copyright notice displayed throughout this document indicates when this document was updated. ISBN O 680 32748 5 STDDBSI BS EN IS0 L577-ENGL 1997 W Lb24bb7 0830343 2bT EUROPEANSTANDARD NORME EUROgENNE E
9、UROPISCHE NORM EN Is0 1599 May 1999 ICs 83.080.00 English version Plastics - Cellulose acetate - Determination of viscosity loss on moulding (IS0 1 599: 1990) plasdique8 - Acetate de cellulose - Determination de la pette de vi the solution of original cellulose acetate does not contain dimethyl phth
10、alate. However, the concentration of dimethyl phthalate in the solution for viscosity measurement is too small to have any significant effect on viscosity. 4 Reagents During the determination, use only reagents of rec- ognized analytical grade. 4.1 Dimethyl phthalate, analytical grade, it shall be g
11、round if necessary, avoiding excessive heating of the sam- ple. If proceeding in accordance with 7.1.2 (second method of incorporating the plasticizer), the cellu- lose acetate need not be ground. 6.2 Determine the moisture content of the sample in accordance with IS0 585. 7 Procedure 7.1 Either of
12、the methods described below may be used for the incorporation of plasticizer. 7.1.1 Flrst method Weigh into a glass bottle, to within f 0,s g, the quantity of the sample corresponding to 100 g of dry cellulose acetate. Into another glass bottle, weigh 45 g of dimethyl phthalate (4.1), to within f 0,
13、s g. Slowly add the dimethyl phthalate to the cellulose acetate with constant stirring and continue to stir for at least 5 min afler all the dimethyl phthalate has been added. Proceed in accordance with 7.2 to 7.8. 7.1.2 Second method Place 200 g, weighed to the nearest 1 g, of the cellulose acetate
14、 in a 2 litre vessel. The moisture content of the sample shall be less than 0,s %; if not, there is a risk of bubbles forming in the mould- ing. Add about one-half of the following mixture: - dimethyl phthalate (4.1): 75 ml f 0,s ml (90 g 0,6 9); - propan-2-01 (4.3): 400 ml f 0,s ml. Homogenize by m
15、ixing briskly with a glass stirrer. Pour in the rest of the solvent/piasticizer mixture, and, after having mixed again and stoppered the vessel, place it immediately on a roller mixer oper- ating between 50 rpm and 70 rpm. After 2 h of mix- ing, tap the vessel with the palm of the hand in order to d
16、islodge any powder which may have become stuck to the sides. Place on the roller mixer again and mix for a further 4 h. Pour the product into a porcelain dish, cover with a sheet of filter paper and let it stand in the open, at room temperature, overnight. Then place in an oven, thermostatically mai
17、ntained at 60 OC f 2 OC, and leave for 3 h to eliminate part of the solvent. At the end of this time, place the product in the original clean vessel again. Homogenize it for one or two minutes, by rapid mixing with a mixing rod equipped with a blade turning at IO000 rpm. (This operation is to destro
18、y any agglomerates that may have been produced during the stoving.) Stopper the vessel, then let it stand again at room temperature for about 20 h. Proceed in accordance with 7.2 to 7.8. 7.2 Heat the mixed material for 2 h at 70 “C f 2 “C to remove moisture and complete the absorption of plasticizer
19、. 7.3 Place a suitable quantity of the heated mixture in the mould (5.2), pre-heated to a temperature of 200 “C 2 OC. Apply contact pressure for 2 min, then full pressure (at least 8 MN/m2 at the moulding surface) for a further 10 min f 0,5 min for a mould- ing 1,5 mrn thick. This time shall be incr
20、eased by 0,5 min for each 0.5 mm above 1,5 mm thickness. 7.4 Release the pressure and start cooling im- mediately, continuing the cooling until the moulding is rigid enough to be ejected without being de- formed. The rate of cooling shall be such that the mould temperature 2 min aier the start of co
21、oling is at least 30 “C below the moulding temperature. 7.5 Grind the moulded cellulose acetate to a size less than 0.9 mm, avoiding excessive heating, and dry it at 70 “C f 2 “C for 2 h. 2 STD.BSI BS EN IS0 1599-ENGL 1799 Lb24bb9 0810349 788 EN IS0 1599:1999 7.6 Prepare a solution of the ground mat
22、erial in dichloromethane/methanol mixture as speclied in IS0 1157, but containing 0,725 g of material (.e. 0,500 g of cellulose acetate) in 100 ml of solution, and determine the viscosity ratio in accordance with IS0 1157. 7.7 Determine the viscosity ratio of a 5 g/l solution of the original cellulo
23、se acetate in accordance with IS0 1157. 7.8 Make two complete determinations in accord- ance with 7.1 to 7.7. If the difference between the determinations is more than 10 % of their mean value, two further determinations shall be made, 8 Expression of results 8.1 lhe viscosity loss on moulding, expr
24、essed as a percentage of the viscosity ratio of the original cellulose acetate. is calculated from the formula %,a - %,b %.a where vr,a is the viscosity ratio of the original cellu- lose acetate; If,b is the viscosity ratio of the cellulose acetate after moulding. NOTE 2 If the same viscometer is us
25、ed in the two de- terminations, it is sufficient to determine the flow time of each solution. In that case, the viscosity loss on moulding is calculated from the formula 8 - b 100 x - r. where 8 Ib is the flow time of the original cellulose acet- ate solution, in seconds; is the flow time of the sol
26、ution of moulded cellulose acetate, in seconds. 8.2 The result is the mean of two valid determi- nations (see 7.8). 9 Precision The precision of this test method is not known be- cause inter-laboratory data are not available. This method may not be suitable for use in specifications or in cace of di
27、sputed results as long as these data are not available. 10 Test report The test report shall include the following particu- lars: a) a reference to this International Standard; b) all details necessary for the complete identifi- cation of the product tested, including type, manufacturers code number
28、, source, trade name, etc.; c) the viscosity loss on moulding (see 8.2); d) the date of the test. 3 EN IS0 1599:1999 Dimensions in millimetres la Flat plate, 1.5 rnrn thick, of stainless steel or nickel-plated steel polished on the lower surface lb Stainless-steel moulding template, 1,5 mrn to 5 mrn
29、 thick IC Flat plate, 1,5 rnrn thick, of stainless steel or nickel-plated steel polished on the upper surface Figure 1 - Suitable mould (see 5.2) 4 STD.BS1 BS EN IS0 1599-ENGL 1999 Lb24bb9 01310351 33b EN IS0 1699:1999 Annex ZA (normative) Normative references to international publications with thei
30、r relevant European publications This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to
31、 or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies. Publication Year - EN - Year EN IS0 585 1990 Plastics - Unplasticized cellulose EN IS0 5
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