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1、INTERNATIONAL STANDARD IS0 1599 Second edition 1990-12-01 Plastics - Cellulose acetate - Determination of viscosity loss on moulding Plas tiques - Acetate de cellulose - L36termination de la perte de viscosik! au moulage Reference number IS0 1599:1990(E) Copyright International Organization for Stan
2、dardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/27/2007 04:23:21 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 1599:1990(E) Foreword IS0 (the International Organization for Standardization) is a worl
3、dwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 technical committees. Each member body interested In a subject for which a technical committee has been established has the right to be represented on
4、that committee. International organizations, govern- mental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with th.e International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adop
5、ted by the technical committees are circulated to the member bodies for voting. Publication as an Inter- national Standard requires approval by at least 75% of the member bodies casting a vote. International Standard IS0 1599 was prepared by Technical Committee ISO/TC 61, Plastics. This second editi
6、on cancels and replaces the first edition (IS0 1599:1975), of which it constitutes a minor revision. 0 IS0 1990 All rights reserved. No part of thls publication may be reproduced or utilized in any form or by any means, electronic or mechanical, Including photocopying and microfilm, without permlssl
7、on In writing from the publlsher. lnternatlonal Organlzatlon for Standardlzatlon Case Postale 56 l CH-1211 Geneve 20 * Switzerland Prlnted In Switzerland II Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001
8、Not for Resale, 04/27/2007 04:23:21 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD IS0 1599:1990(E) Plastics - Cellulose acetate - Determination of viscosity loss on moulding WARNING - The use of this International Standard may involve hazardous mate
9、rials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to
10、 use, 1 Scope This International Standard specifies a method for the determination of the reduction in viscosity which occurs when cellulose acetate is moulded. The vis- cosity loss on moulding is related to the depolymerization of cellulose acetate, which gener- ally Increases brittleness in the mo
11、ulded product. This method is suitable for cellulose acetate which does not contain additives, fillers, etc., which may interfere with the determination of viscosity. It is suitable for cellulose acetate having an acetic acid yield above 50 %. 2 Normative references The following standards contain p
12、rovisions which, through reference in this text, constitute provisions of this International Standard. At the time of publi- cation, the editions indicated were valid. All stan- dards are subject to revision, and pat-ties to agreements based on this International Standard are encouraged to investiga
13、te the possibility of ap- plying the most recent editions of the standards in- dicated below. Members of IEC and IS0 maintain registers of currently valid International Standards. IS0 565:1990, Test sieves - Metal wire cloth, perfo- rated metal plate and electroformed sheet-Nominal sizes of openings
14、. IS0 585:19901), Plastics - Unplasticized cellulose acetate - Determination of moisture content. IS0 1157:1990, Plastics - Cellulose acetate in dilute solution - Determination of viscosity number and viscosity ratio. 3 Principle Cellulose acetate plasticized with dimethyl phthalate is moulded under
15、 specified conditions of tempera- ture, pressure and time. After cooling, the moulding is ground up. The viscosity ratio of the ground ma- terial from the moulding and also that of the original cellulose acetate are determined in accordance with IS0 1157. The percentage viscosity loss is calcu- late
16、d from the values of viscosity before and after moulding. NOTE 1 Since the moulded cellulose acetate contains dimethyl phthalate, this is also present in the solution for viscosity measurement; the solution of original cellulose acetate does not contain dimethyl phthalate. However, the concentration
17、 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, if not, there is a risk of bubbles forming in
18、the mould- ing. Add about one-half of the following mixture: 5.1 Hydraulic press, capable of exerting a pressure of at least 8 MN/m* on the mouldlng surface, with means of heating to 200 “C and with water cooling. 5.2 Mould (see figure 1 for a suitable type), with polished surfaces which are substan
19、tially flat and parallel, to produce mouldings of thickness within the range I,5 mm to 5 mm. A particular thickness within this range may be specified. - dimethyl phthalate (4.1): 75 ml ) 0,5 ml (90 g + 0,6 g): - propan-2-01 (4.3): 400 ml + 0,5 ml. Homogenize by mixing briskly with a glass stirrer.
20、Pour in the rest of the solvent/plasticizer 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 dislodge any powder which may have be
21、come stuck to the sides. Place on the roller mixer again and mix for a further 4 h. 5.3 Apparatus for viscosity ratio determination, as specified in IS0 1157. $4 Stainless-steel grinder, electrically operated. 55 Oven, capable of being thermostatically main- tained at 60 “C If: 2 “C or 70 “C + 2 “C.
22、 6 Test sample 6.1 If proceeding in accordance with 7.1.1 (first method of incorporating the plasticizer), the sample of celluldse acetate shall be in the form of powder passing entirely through a sieve of 710 pm mesh size (as defined in IS0 565); it shall be ground if necessary, avoiding excessive
23、heating of the sam- ple. Pour the product into a porcelain dish, cover with a sheet of filter paper and let it stand in the open, at room temperature, overnight. Then place in an oven, thermostatically maintained at 60 “C + 2 “C, and leave for 3 h to eliminate part of the solvent. At the end of this
24、 time, place the product in the original clean vessel again. Homogenize it for one or two minutes, by rapid mixing with a mixing rod equipped with a blade turning at 10000 rpm. (This operation is to destroy any agglomerates that may have been produced during the stoving.) Stopper the vessel, then le
25、t it stand again at room temperature for about 20 h. Proceed in accordance with 7.2 to 7.8. If proceeding in accordance with 7.1.2 (second method of incorporating the plasticizer), the cellu- lose acetate need not be ground. 6.2 Determine the moisture content of the sample in accordance with IS0 585
26、. 7 Procedure 7.1 Either of the methods described below may be used for the Incorporation of plasticizer. 7.1.1 First method Weigh into a glass bottle, to within + 0,5 g, the quantity of the sample corresponding to 100 g of dry cellulose acetate. Into another glass bottle, weigh 45 g of dimethyl pht
27、halate (4.1), to within I): 0,5 g. Slowly add the dimethyl phthalate to the cellulose acetate with constant stirring and continue to stir for 7.2 Heat the mixed material for 2 h at 70 “C -I- 2 “C to remove moisture and complete the absor$ion of plasticizer. 7.3 Place a suitable quantity of the heate
28、d mixture In the mould (5.2), pre-heated to a temperature of 200 “C f 2 “C. Apply contact pressure for 2 min, then full pressure (at least 8 MN/m2 at the moulding surface) for a further 10 min %,b is the viscosity ratio of the cellulose acetate after moulding. NOTE 2 If the same viscometer is used i
29、n 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 1ooxq a where t a is the flow time of the original cellulose acet- ate solution, in seconds: tb is the flow time of the solution of mo
30、ulded 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 case of disputed resu
31、lts 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, manufacturer s code number, source,
32、trade name, etc.; c) the viscosity loss on moulding (see 8.2); d) the date of the test. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/27/2007 04:23:21 MDTNo reproduction or networking
33、permitted without license from IHS -,-,- IS0 1599:1990(E) Dimensions in millimetres la Flat plate, 1,5 mm thick, of stainless steel or nickel-plated steel polished on the lower surface lb Stainless-steel moulding template, 1,5 mm to 5 mm thick Ic Flat plate, 1,5 mm thick, of stainless steel or nicke
34、l-plated steel polished on the upper surface Figure 1 - Suitable mould (see 5.2) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/27/2007 04:23:21 MDTNo reproduction or networking permitt
35、ed without license from IHS -,-,- IS0 1599:1990(E) UDC 678.544.4532.13 Descriptors: plastics, cellulose derivatives, cellulose acetate, tests, determination, vlscoslty, plastic moulding. Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/27/2007 04:23:21 MDTNo reproduction or networking permitted without license from IHS -,-,-