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1、BRITISH STANDARD BS EN ISO 1599:1999 Plastics Cellulose acetate Determination of viscosity loss on moulding The European Standard EN ISO 1599:1999 has the status of a British Standard ICS 83.080.20 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c)
2、 BSI BS EN ISO 1599:1999 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 August 1999 BSI 03-2000 ISBN 0 580 32748 5 National foreword This Bri
3、tish Standard is the English language version of EN ISO 1599:1999. It is identical with ISO 1599:1990. The UK participation in its preparation was entrusted to Technical Committee PRI/82, Thermoplastic Materials, which has the responsibility to: aid enquirers to understand the text; present to the r
4、esponsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained o
5、n request to its secretary. 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 E
6、uropean publications 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 all the n
7、ecessary provisions 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, pages i and ii, th
8、e EN ISO title page, page 2, the ISO title page, pages ii to iv, pages 1 to 4, an inside back cover and a back cover. This standard 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. Amendments issu
9、ed since publication Amd. No.DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 1599:1999 BSI 03-2000i Contents Page National forewordInside front cover Foreword2 Forewordiii Text of ISO 15991 Licensed Copy: sheffieldun s
10、heffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii blank Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1599 May 1999 ICS 83.080.00 English version Plas
11、tics Cellulose acetate Determination of viscosity loss on moulding (ISO 1599:1990) Plastiques Actate de cellulose Dtermination de la perte de viscosit au moulage (ISO 1599:1990) Kunststoffe Celluloseacetat Bestimmung des Viskosittsverlustes beim Formen (ISO 1599:1990) This European Standard was appr
12、oved by CEN on 16 April 1999. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
13、standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notifie
14、d to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and
15、United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN
16、ISO 1599:1999 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 1599:1999 BSI 03-2000 2 Foreword The text of.the International Standard from Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardizatio
17、n (ISO) has been taken over as an European Standard by Technical Committee CEN/TC 249 “Plastics”, the secretariat of which is held by IBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November
18、1999, and conflicting national standards shall be withdrawn at the latest by November 1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Fin
19、land, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 1599:1990 has been approved by CEN as a European Standard without any modification. NOTE
20、Normative references to International Standards are listed in Annex ZA (normative). Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN
21、 ISO 1599:1999 ii BSI 03-2000 Contents Page Forewordiii 1Scope1 2Normative references1 3Principle1 4Reagents1 5Apparatus1 6Test sample2 7Procedure2 8Expression of results3 9Precision3 10Test report3 Annex ZA (normative) Normative references to international publications with their relevant European
22、publicationsInside back cover Figure 1 Suitable mould4 Descriptors: Plastics, cellulose derivatives, cellulose acetate, tests, determination, viscosity, plastic moulding. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 1599:1999 BSI 0
23、3-2000iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for
24、 which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on a
25、ll matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. International Standard IS
26、O 1599 was prepared by Technical Committee ISO/TC 61, Plastics. This second edition cancels and replaces the first edition (ISO 1599:1975), of which it constitutes a minor revision. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv blank Li
27、censed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 1599:1999 BSI 03-20001 WARNING The use of this International Standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety
28、 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 use. 1 Scope This International Standard specifies a method for the determination of the re
29、duction in viscosity which occurs when cellulose acetate is moulded. The viscosity loss on moulding is related to the depolymerization of cellulose acetate, which generally increases brittleness in the moulded product. This method is suitable for cellulose acetate which does not contain additives, f
30、illers, 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 provisions which, through reference in this text, constitute provisions of this International Sta
31、ndard. At the time of publication, the editions indicated were valid. All standards are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of
32、IEC and ISO maintain registers of currently valid International Standards. ISO 565:1990, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings. ISO 585:1990, Plastics Unplasticized cellulose acetate Determination of moisture content1). ISO 1157:1990,
33、Plastics Cellulose acetate in dilute solution Determination of viscosity number and viscosity ratio. 3 Principle Cellulose acetate plasticized with dimethyl phthalate is moulded under specified conditions of temperature, pressure and time. After cooling, the moulding is ground up. The viscosity rati
34、o of the ground material from the moulding and also that of the original cellulose acetate are determined in accordance with ISO 1157. The percentage viscosity loss is calculated from the values of viscosity before and after moulding. NOTE 1Since the moulded cellulose acetate contains dimethyl phtha
35、late, this is also present in the solution for viscosity measurement; the solution of original cellulose acetate does not contain dimethyl phthalate. However, the concentration of dimethyl phthalate in the solution for viscosity measurement is too small to have any significant effect on viscosity. 4
36、 Reagents During the determination, use only reagents of recognized analytical grade. 4.1 Dimethyl phthalate, analytical grade,1,191 to 1,195, purity more than 99 % (m/m). 4.2 Solvents for viscosity ratio determination, as specified in ISO 1157. 4.3 Propan-2-ol SAFETY PRECAUTIONS Propan-2-ol is high
37、ly flammable. Keep the container tightly closed and away from sources of ignition. Do not smoke. 5 Apparatus Ordinary laboratory apparatus, plus the following: 5.1 Hydraulic press, capable of exerting a pressure of at least 8 MN/m2 on the moulding surface, with means of heating to 200 C and with wat
38、er cooling. 5.2 Mould (see Figure 1 for a suitable type), with polished surfaces which are substantially flat and parallel, to produce mouldings of thickness within the range 1,5 mm to 5 mm. A particular thickness within this range may be specified. 5.3 Apparatus for viscosity ratio determination, a
39、s specified in ISO 1157. 5.4 Stainless-steel grinder, electrically operated. 5.5 Oven, capable of being thermostatically maintained at 60 C 2 C or 70 C 2 C. 1) To be published. d20 20 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:22:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN ISO 15
40、99:1999 2 BSI 03-2000 6 Test sample 6.1 If proceeding in accordance with 7.1.1 (first method of incorporating the plasticizer), the sample of cellulose acetate shall be in the form of powder passing entirely through a sieve of 710 4m mesh size (as defined in ISO 565); it shall be ground if necessary
41、, avoiding excessive heating of the sample. If proceeding in accordance with 7.1.2 (second method of incorporating the plasticizer), the cellulose acetate need not be ground. 6.2 Determine the moisture content of the sample in accordance with ISO 585. 7 Procedure 7.1 Either of the methods described
42、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 phthalate (4.1), to within 0,5 g. Slowly add the dimeth
43、yl phthalate to the cellulose acetate with constant stirring and continue to stir for at least 5 min after 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 in a 2 litre vessel. The
44、moisture content or the sample shall be less than 0,5 %; if not, there is a risk of bubbles forming in the moulding. Add about one-half of the following mixture: dimethyl phthalate (4.1): 75 ml 0,5 ml (90 g 0,6 g); propan-2-ol (4.3): 400 ml 0,5 ml. Homogenize by mixing briskly with a glass stirrer.
45、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 operating between 50 rpm and 70 rpm. After 2 h of mixing, tap the vessel with the palm of the hand in order to dislodge any powder which may have become
46、 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 maintained at 60 C 2 C, and leave for 3 h t
47、o 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 10 000 rpm. (This operation is to destroy any agglomerates that may have been produ
48、ced 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 2 C to remove moisture and complete the absorption or plasticizer. 7.3 Place a suitable quantity of the heated m
49、ixture in the mould (5.2), pre-heated to a temperature of 200 C 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 0,5 min for a moulding 1,5 mm thick. This time shall be increased by 0,5 min for each 0,5 mm above 1,5 mm thickness. 7.4 Release the pressure and start cooling immediately, continuing the cooling until the moulding is rigid enough to be ejected without being deformed. The rate of cooling shall be such that the m