1、BRITISH STANDARD BS EN ISO 1599:1999 Plastics Cellulose acetate Determination of viscosityloss on moulding The European Standard EN ISO 1599:1999 has the status of a British Standard ICS 83.080.20BSENISO1599:1999 This British Standard, having been prepared under the directionof the Sector Committeef
2、or 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 British Standard is the English language version of ENISO1599:1999. Itis identical with ISO1599:1990. The UK particip
3、ation 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 responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the
4、 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 on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally in
5、clude an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitl
6、ed “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 necessary provisions of a contract. Users of British Standards are responsible for their correct application. Complianc
7、e 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, theEN ISO title page, page 2, the ISO title page, pages ii to iv,pages 1 to 4, aninside back cover and a back cover. Thi
8、s 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 issued since publication Amd. No. Date CommentsBSENISO1599:1999 BSI 03-2000 i Contents Page National foreword Inside front co
9、ver Foreword 2 Foreword iii Text of ISO 1599 1ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM ENISO1599 May 1999 ICS 83.080.00 English version Plastics Cellulose acetate Determination of viscosity loss on moulding (ISO 1599:1990) Plastiques Actate de cellulose Dtermination de la perte de v
10、iscosit aumoulage (ISO 1599:1990) Kunststoffe Celluloseacetat Bestimmung des Viskosittsverlustes beim Formen (ISO 1599:1990) This European Standard was approved by CEN on 16 April 1999. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for givin
11、g this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versio
12、ns (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Cz
13、ech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue
14、 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 ISO 1599:1999 EENISO1599:1999 BSI 03-2000 2 Foreword The text of.the International Standard from Technical Committee ISO/TC 61“Plastics” of the I
15、nternational Organization for Standardization (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 ofa national standard, either by publication of an identical text or
16、by endorsement, at the latest by November1999, and conflicting national standards shall be withdrawn at the latest by November1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austri
17、a, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. Endorsement notice The text of the International Standard ISO1599:1990 has been approved by CEN as aEuropean St
18、andard without any modification. NOTENormative references to International Standards arelisted inAnnex ZA (normative).ENISO1599:1999 ii BSI 03-2000 Contents Page Foreword iii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Reagents 1 5 Apparatus 1 6 Test sample 2 7 Procedure 2 8 Expression of res
19、ults 3 9 Precision 3 10 Test report 3 Annex ZA (normative) Normative references to international publicationswiththeir relevant European publications Inside back cover Figure 1 Suitable mould 4 Descriptors: Plastics, cellulose derivatives, cellulose acetate, tests, determination, viscosity, plastic
20、moulding.ENISO1599:1999 BSI 03-2000 iii 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 technicalcommittees. Each member bod
21、y interested in a subject for which atechnical committee has been established has the right to be represented onthatcommittee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaboratesclosely with the International Electrotechni
22、cal Commission (IEC)on all 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 least75% of the member bodies casting a vote. Int
23、ernational Standard ISO 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.iv blankENISO1599:1999 BSI 03-2000 1 WARNING The use of this International Standard may involve h
24、azardous materials, 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 limitat
25、ions prior to use. 1 Scope This International Standard specifies a method for the determination of the reduction in viscosity which occurs when cellulose acetate is moulded. Theviscosity loss on moulding is related to the depolymerization of cellulose acetate, which generally increases brittleness i
26、n the moulded 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 aceticacid yield above50%. 2 Normative references The following standards cont
27、ain provisions which, through reference in this text, constitute provisions of this International Standard. 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 investiga
28、te the possibility of applying the most recent editions of the standards indicated below. Members of 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 58
29、5:1990, Plastics Unplasticized cellulose acetate Determination of moisture content 1) . ISO 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 specified con
30、ditions of temperature, pressure and time. After cooling, the moulding is ground up. The viscosity ratio of the ground material from the moulding and also that ofthe original cellulose acetate are determined in accordance with ISO1157. The percentage viscosity loss is calculated from the values of v
31、iscosity before and after moulding. NOTE 1Since the moulded cellulose acetate contains dimethyl phthalate, this is also present in the solution for viscosity measurement; the solution of original cellulose acetate does notcontain dimethyl phthalate. However, the concentration of dimethyl phthalate i
32、n the solution for viscosity measurement is too small to have any significant effect on viscosity. 4 Reagents During the determination, use only reagents of recognized analytical grade. 4.1 Dimethyl phthalate, analytical grade,1,191 to 1,195, purity more than99% (m/m). 4.2 Solvents for viscosity rat
33、io determination, asspecified in ISO 1157. 4.3 Propan-2-ol SAFETY PRECAUTIONS Propan-2-ol is highly 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
34、pressure of at least 8 MN/m 2on the moulding surface, with means of heating to200 C and with water cooling. 5.2 Mould (seeFigure 1 for a suitable type), with polished surfaces which are substantially flat and parallel, to produce mouldings of thickness within the range1,5mm to5mm. A particular thick
35、ness within this range may be specified. 5.3 Apparatus for viscosity ratio determination, as specified in ISO1157. 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. d 20 20ENISO1599:1999 2 BSI 03-20
36、00 6 Test sample 6.1 If proceeding in accordance with7.1.1 (firstmethod ofincorporating the plasticizer), the sample of cellulose acetate shall be in the form of powder passing entirely through a sieve of710 4m mesh size (as defined in ISO 565); it shall be ground if necessary, avoiding excessive he
37、ating of the sample. If proceeding in accordance with7.1.2 (secondmethod of incorporating the plasticizer), thecellulose acetate need not be ground. 6.2 Determine the moisture content of the sample inaccordance with ISO585. 7 Procedure 7.1 Either of the methods described below may be used for the in
38、corporation of plasticizer. 7.1.1 First method Weigh into a glass bottle, to within 0,5g, the quantity of the sample corresponding to100g ofdrycellulose acetate. Into another glass bottle,weigh45g of dimethyl phthalate (4.1), to within 0,5g. Slowly add the dimethyl phthalate tothe cellulose acetate
39、with constant stirring andcontinue to stir for at least5min after all the dimethyl phthalate has been added. Proceed in accordance with7.2 to7.8. 7.1.2 Second method Place 200 g, weighed to the nearest 1 g, of the cellulose acetate in a 2 litre vessel. The moisture content or the sample shall be les
40、s than0,5%; 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. Pour in the rest of the solvent/plasticizer m
41、ixture, and, after having mixed again and stoppered the vessel, place it immediately on a roller mixer operating between50rpm and70rpm. After2h ofmixing, tap the vessel with the palm of the hand in order to dislodge any powder which may have become stuck to the sides. Place on the roller mixer again
42、 and mix for a further4h. Pour the product into a porcelain dish, cover with asheet of filter paper and let it stand in the open, atroom temperature, overnight. Then place in an oven, thermostatically maintained at60 C 2 C, and leave for3h to eliminate part of the solvent. Atthe end of this time, pl
43、ace the product in the original clean vessel again. Homogenize it for one ortwo minutes, by rapid mixing with a mixing rodequipped with a blade turning at 10 000 rpm. (Thisoperation is to destroy any agglomerates thatmay have been produced during the stoving.) Stopper the vessel, then let it stand a
44、gain at room temperature for about20h. Proceed in accordance with7.2 to7.8. 7.2 Heat the mixed material for 2h at 70 C 2 C to remove moisture and complete the absorption or plasticizer. 7.3 Place a suitable quantity of the heated mixturein the mould (5.2), pre-heated to a temperature of 200 C 2 C. A
45、pply contact pressure for2min, then full pressure (atleast8MN/m 2at the moulding surface) for afurther10min 0,5min for a moulding 1,5 mm thick. This time shall be increased by 0,5min for each0,5mm above 1,5mm thickness. 7.4 Release the pressure and start cooling immediately, continuing the cooling u
46、ntil the moulding is rigid enough to be ejected without being deformed. The rate of cooling shall be such that the mould temperature2min after the start of cooling is at least30 C below the moulding temperature. 7.5 Grind the moulded cellulose acetate to a size less than0,9mm, avoiding excessive hea
47、ting, and dry it at70 C 2 C for 2h. 7.6 Prepare a solution of the ground material in dichloromethane/methanol mixture as specified in ISO1157, but containing0,725g of material (i.e.0,500g of cellulose acetate) in 100ml of solution, and determine the viscosity ratio in accordance with ISO1157. 7.7 De
48、termine the viscosity ratio of a5g/l solution ofthe original cellulose acetate in accordance with ISO1157. 7.8 Make two complete determinations in accordance with7.1 to7.7. If the difference between the determinations is more than 10% of their mean value, two further determinations shall be made.ENI
49、SO1599:1999 BSI 03-2000 3 8 Expression of results 8.1 The viscosity loss on moulding, expressed as a percentage of the viscosity ratio of the original cellulose acetate, is calculated from the formula where NOTE 2If the same viscometer is used in the two determinations, it is sufficient to determine the flow timeofeachsolution. In that case, the viscosity loss on mouldingiscalculated from the formula where 8.2 The result is the mean of two valid determinations (see7.8). 9 Prec
