malaysian standard
Transcription
malaysian standard
MALAYSIAN STANDARD MS ISO 1628-6:2008 PLASTICS - DETERMINATION OF VISCOSITY NUMBER AND LIMITING VISCOSITY NUMBER PART 6: METHYL METHACRYLATE POLYMERS (ISO 1628-6:1990, IDT) ISO 1628-6:1990 is endorsed as Malaysian Standard with the reference number MS ISO 1628-6:2008. ICS: 83.080.20 Descriptors: viscosity, polymers, capillary viscometers, methyl methacrylate polymers © Copyright 2008 DEPARTMENT OF STANDARDS MALAYSIA © STANDARDS MALAYSIA 2008 – All rights reserved DEVELOPMENT OF MALAYSIAN STANDARDS The Department of Standards Malaysia (STANDARDS MALAYSIA) is the national standardisation and accreditation body. The main function of the Department is to foster and promote standards, standardisation and accreditation as a means of advancing the national economy, promoting industrial efficiency and development, benefiting the health and safety of the public, protecting the consumers, facilitating domestic and international trade and furthering international cooperation in relation to standards and standardisation. Malaysian Standards are developed through consensus by committees which comprise of balanced representation of producers, users, consumers and others with relevant interests, as may be appropriate to the subject in hand. To the greatest extent possible, Malaysian Standards are aligned to or are adoption of international standards. Approval of a standard as a Malaysian Standard is governed by the Standards of Malaysia Act 1996 (Act 549). Malaysian Standards are reviewed periodically. The use of Malaysian Standards is voluntary except in so far as they are made mandatory by regulatory authorities by means of regulations, local by-laws or any other similar ways. The Department of Standards appoints SIRIM Berhad as the agent to develop Malaysian Standards. The Department also appoints SIRIM Berhad as the agent for distribution and sale of Malaysian Standards. For further information on Malaysian Standards, please contact: Department of Standards Malaysia Century Square, Level 1 & 2 Blok 2300, Jalan Usahawan 63000 Cyberjaya Selangor D.E. MALAYSIA OR SIRIM Berhad (Company No. 367474 - V) 1, Persiaran Dato’ Menteri P.O. Box 7035, Section 2 40911 Shah Alam Selangor D.E. Tel: 60 3 8318 0002 Fax: 60 3 8319 3131 Tel: 60 3 5544 6000 Fax: 60 3 5510 8095 http://www.standardsmalaysia.gov.my http://www.sirim.my E-mail: [email protected] © STANDARDS MALAYSIA 2008 – All rights reserved MS ISO 1628-6:2008 CONTENTS Page Committee representation..................................................................................................... ii National foreword .................................................................................................................. iii 1 Scope ....................................................................................................................... 1 2 Normative references............................................................................................... 1 3 Definitions and units................................................................................................. 1 4 Principle ................................................................................................................... 1 5 Measurements ......................................................................................................... 1 6 Apparatus................................................................................................................. 2 7 Solvent and test solution.......................................................................................... 2 8 Temperature of measurement ................................................................................. 2 9 Procedure ................................................................................................................ 2 10 Expression of results................................................................................................ 3 11 Test report................................................................................................................ 3 Annexes A Calibration of the viscometer ................................................................................... 4 B Determination of the limiting viscosity number ........................................................ 6 C Bibliography ............................................................................................................. 6 © STANDARDS MALAYSIA 2008 – All rights reserved i MS ISO 1628-6:2008 Committee representation The Plastics and Plastics Products Industry Standards Committee (ISC J) under whose authority this Malaysian Standard was adopted, comprises representatives from the following organisations: Department of Standards Malaysia Federation of Malaysian Manufacturers Jabatan Kerja Raya Malaysia Malaysian Association of Standards Users Malaysian Institute of Chemistry Malaysian Petrochemical Association Malaysian Plastics Manufacturers Association Malaysian Rubber Board Ministry of Domestic Trade and Consumers Affairs Ministry of Health Malaysia Ministry of International Trade and Industry Malaysia Plastics and Rubber Institute of Malaysia SIRIM Berhad (Advanced Polymer and Composites Programme) SIRIM QAS International Sdn Bhd The Institution of Engineers, Malaysia Universiti Kebangsaan Malaysia Universiti Sains Malaysia Universiti Teknologi Malaysia The Technical Committee on General and Raw Materials for Plastics which recommends adoption of the ISO Standard consists of representatives from the following organisations: Federation of Malaysian Manufacturers (Hercules Sdn Bhd) Malaysian Petrochemical Association (Dow Chemical (Malaysia) Sdn Bhd) Malaysian Plastics Manufacturers Association (Industrial Resins (Malaysia) Berhad) Petronas Polymer Technology Centre SIRIM Berhad (Advanced Polymer and Composites Programme) SIRIM Berhad (Secretariat) SIRIM QAS International Sdn Bhd (Civil and Construction Section) Universiti Malaya Vinyl Chloride (Malaysia) Sdn Bhd ii © STANDARDS MALAYSIA 2008 – All rights reserved MS ISO 1628-6:2008 NATIONAL FOREWORD The adoption of the ISO Standard as a Malaysian Standard was recommended by the Technical Committee on General and Raw Materials for Plastics under the authority of the Plastics and Plastics Products Industry Standards Committee. This Malaysian Standard is identical with ISO 1628-6:1990, Plastics - Determination of viscosity number and limiting viscosity number - Part 6: Methyl methacrylate polymers, published by the International Organization for Standardization (ISO). However, for the purposes of this Malaysian Standard, the following apply: a) in the source text, “this International Standard” should read “this Malaysian Standard”; b) the comma which is used as a decimal sign (if any), to read as a point; and c) reference(s) to International Standard(s) should be replaced by equivalent Malaysian Standard(s) as follows: Referenced International Standard Corresponding Malaysian Standard ISO 1628-1:1984, Plastics - Determination of the viscosity of polymers in dilute solution using capillary viscometers - Part 1: General Principles MS ISO 1628-1:2004, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 1: General Principles Compliance with a Malaysian Standard does not of itself confer immunity from legal obligations. NOTE. IDT on the front cover indicates an identical standard i.e. a standard where the technical content, structure, and wording (or is an identical translation) of a Malaysian Standard is exactly the same as in an International Standard or is identical in technical content and structure although it may contain the minimal editorial changes specified in clause 4.2 of ISO/IEC Guide 21-1. © STANDARDS MALAYSIA 2008 – All rights reserved iii INTERNATIONAL STANDARD . ISO 1628-6. First edition 1990-02-01 Plastics - Determination of viscosity and limiting viscosity number - number Part 6: Methyl methacrylate polymers Hastiques - Dt2termination de l’indice de viscosittS et de l’indice limite de viscositb Partie 6: Polymkres de mbhacrylate de m&h yle Reference number ISO 1628-6 : 1990 (El ISOl628-6:199O(E) Foreword ISO (the International Organization for Standardization) is a worldwide federation of national Standards bodies (ISO member bedies). The work of preparing International Standards is normally carried out through ISO technical committees. Esch member body interested in a subject for 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 all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the ISO Council. They are approved in accordance with ISO procedures requiring at least 75 % approval by the member bodies voting. International Standard ISO 1628-6 was prepared by Technical Committee ISO/TC 61, Plastics. lt cancels and replaces International Standard ISO 1233 : 1975, of which it constitutes a technical revision. ISO 1628 consists of the following Parts, under the general title Plastics - Determination of viscosity number and limiting viscosity number 1): - Part 1: General conditions - Part 2: Polyfvinyl chloride) resins - Part 3: Polyeth ylenes and polyprop ylenes - Part 4: Polycarbonate (PC) moulding and extrusion materials - Part 5: Poly(alkylene tereph thala tes) - Part 6: Methyl methacrylate polymers Annexes A and B form an integral part of this part of ISO 1628. Annex C is for information only. 1) The general title of ISO 1628-1 is Guide/i.es for the Standardkation of methods for the determination of viscosity number and limiting viscosity number of polymers in dilute solution. 0 ISO 1990 All rights reserved. No patt of this publication may be reproduced or utilized in any form or by any means, electronie or mechanical, including photocopying and microfilm, without Permission in writing from the publisher. International Organization for Standardization Case postale 56 l CH-1211 Geneve 20 l Switzerland Printed in Switzerland ii INTERNATIONAL Plastics viscosity - STANDARD ISO 1628-6 : 1990 (E) Determination number - Part 6: Methyl methacrylate of viscosity number and limiting Polymers 1 Scope 3 This patt of ISO 1628 specifies the conditions to be used for the determination of the viscosity number of methyl methacrylate polymer moulding and extrusion materials in dilute solution. For the purposes of this part of ISO 1628, the following definition applies, in addition to those in clause 3 of ISO 1628-1 : 1984. lt applies to methyl methacrylate (MMA) copolymers, and mixtures of the two with (mlm) of MMA and up to 20 % (mlm) with and without additives, as defined in homopolymers and a minimum of 80 % of other monomers, ISO 8257-1. Definitions viscosity number, V.N. = - 1 C and units V. N. : r - f-70 ( VO > . . . (1) where NOTE - The dilute-Solution viscosity of Polymers tan be also expressed as a limiting viscosity number [VI (sec annex 6). V. N. is the viscosity number, in millilitres per gram; q is the dynamic millipascal seconds; 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions of this part of ISO 1628. At the time of publication, the editions indicated were valid. All Standards are subject to revision, and Parties to agreements based on this part of ISO 1628 are encouraged to investigate 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. viscosity of the test Solution, in q. is the dynamic viscosity of the solvent, in millipascal seconds; c is the concentration, the Solution. in grams per millilitre, of polymer in NOTE - If the solvent and Solution densities eo and Q are substantially equal, q in equation (1) may be replaced by v and ylo by vo, where v and v. are the kinematic viscosities, in Square millimetres per second, of the solution and the solvent, respectively (sec clause IO). ISO 1628-1 : 1984, Guidelines for the standardization of methods for the determination of viscosity number and limiting viscosity number of Polymers in dilute Solution - Part 7: General conditions. 4 IS 0 3105 : 1976, Glass capillary kinema tic Specifica tion and Opera ting instructions. Calculation of the viscosity number and the limiting viscosity number from the above measurements and the known concentration of the Solution. viscometers - ISO 4793 : 1980, Laboratory sintered (fritted) filters - Porosity grading, classifica tion and designa tion. ISO 8257-1: 1987, (PMMA) moulding na tion. Plastics Polyfmethyl and extrusion materials - methacrylate) Part 1: Desig- Principle Determination of the efflux time at 25 OC + 0,05 OC of a solvent and of a polymer Solution, having a specified concentration, in that solvent. 5 Measurements The data needed to calculate the function defined in clause 3 are obtained by means of a capillary tube viscometer, as explained in clause 4 of ISO 1628-1 : 1984. 1 ISO 1628-6 : 1990 (E) The efflux time of a liquid is related to its viscosity Poiseuille-Hagenbach-Couette equation : = !!- = k(t - At) = kt - -A t e V k is the viscometer second squared; constant, by the . . . in Square millimetres 7.1 Per Chloroform, recognized analytical grade, stabilized with less than 1 % (V/ V) of ethanol, kept in a brown bottle and stored in the dark. (Hagenbach Q is the density, in grams per cubic centimetre, liquid; of the A is a kinetic energy correction Parameter, as defined in ISO 1628-1. NOTE - The kinetic energy correction At becomes insignificant if it is less than 0,2 % of t. For Ubbelohde type OC apparatus, At tan be neglected if the efflux time t is greater than 270 s; for micro-Ubbelohde type MI apparatus, At tan be neglected if f is greater than 70 s. 6 Apparatus (see also ISO 1628-1 : 1984, clause 5) 6.1 Capillary viscometer : suspended-level Ubbelohde type OC apparatus with a capillary diameter of 0,36 mm and measuring bulb of volume 2 ml, in accordance with ISO 3105, or micro-Ubbelohde type MI viscometer, with a capillary diameter of 040 mm and measuring bulb of volume 0,75 ml. The calibration of the viscometer used shall be checked by the method specified in annex A. 6.2 Timing device, with an accuracy of 0,l s for the Ubbelohde type OC viscometer and 0,02 s for the type MI viscometer . 65. Balance, 2 Shaking of 100 ml capacity, fitted accurate to 0,l mg. 6.6 Sintered-glass diameter of 40 Fm ISO 4793). 6.7 flask, filter funnel, with a maximum pore (porosity grade P 40 as defined in machine. Solvent Sample lt is important that the Sample is representative of the material to be tested. 7.3 Test solution concentration The Solution concentration Solution. 7.4 Preparation be 2,6 g of polymer per litre of of the test solution Weigh, to the nearest 0,l mg, 0,26 g + 0,005 g of the Sample into the volumetric flask (6.4). Add 50 ml of chloroform (7.1) and dissolve the Sample completely with shaking. Then make up to the mark with chloroform at 20 OC + 1 OC and Shake once more briefly. With polymers containing viscosity-increasing additives requiring modifications to the Solution preparation process, such modifications shall be agreed upon by the interested Parties. For materials containing Pigments and/or special additives, the quantity weighed into the volumetric flask shall be increased so that the test Solution contains 0,26 g of MMA homopolymers and copolymers per 100 ml. 8 Temperature of measurement The temperature of measurement shall be 25 OC ?I 0,05 OC. 9 6.3 Thermostatic bath, capable of being maintained at a temperature of 25 OC + 0,05 OC. 6.4 One mark volumetric with a ground-glass stopper. (sec also (2) 7.2 correction Solvent and test solution ISO 1628-1 : 1984, clause 6) t is the efflux time, in seconds; At .is the kinetic energy correction), in seconds; 7 Procedure (see also 1628-1 : 1984, clause 8) Using the sintered-glass filter (6.6), introduce the chloroform solvent or the test Solution directly into the tube of the viscometer . Determine the efflux times of the solvent and the test Solution at 25 OC + 0,05 OC in three to five passages through the same viscometer. If the maximum differente between the efflux times exceeds 0,2 s for a Ubbelohde type OC viscometer or 0,03 s for a type MI viscometer, repeat the test with the Same test Solution after cleaning the viscometer with the solvent and drying it. The above procedure may be suitably modified if a viscometer other than the Ubbelohde as described in ISO 3105 is used. ISO 1628-6 : 1990 (EI 10 Expression of resuks (sec also ISO 1628-1 : 1984, clause 9) Calculate the viscosity number V.N., expressed in millilitres per gram, by means of the following equation (this equation is in accordance with ISO 1628-1, but includes the kinetic energy correction, which is necessary in Order to obtain accurate results with the viscometer sizes specified) : t, is the arithmetic mean of the values obtained for the efflux time, in seconds, of the solvent; c is the concentration, the test Solution; At At, expressed in grams per millilitre, of is the kinetic energy correction for t (see annex A); is the kinetic energy correction for t0 (see annex A). The equation for the viscosity number given in ISO 1628-1: V.N. = +(;- l)=f(t;+;;O - 1) lmm (9) VN = t _ t, . . . . . (4) tOc v vO is the viscosity of the test Solution; may be used to give results of similar accuracy if a viscometer with a smaller capillary diameter is used so that the kinetic energy correction is less than 0,2 % of the efflux time. is the viscosity of the solvent; t is the arithmetic mean of the values obtained for the efflux time, in seconds, of the test Solution; 11 Test report See ISO 1628-1 : 1984, clause 10. 3 ISO 1628-6 : 1990 (EI Annex A (normative) Calibration of the viscometer A.l Experience has shown that the required high accuracy of the viscosity number determination of MMA homopolymer and copolymer solutions cannot always be achieved with commercially available U bbelohde viscometers because of minor irregularities in the capillary. lt is therefore advisable to check the accuracy of the viscometer by means of calibrating liquids whose kinematic viscosity ~1 is known. A.2 Viscometer constant k k =- ’ . . . (A.1) where v for n-undecane at 25 OC is 1,467 5 mm2/s. NOTE - The density Q of n-undecane at 25 OC is 0,736 5 g/ml. Kinetic energy corrections At, and At The energy correction tan be neglected if it is less than 0,2 % of the efflux time. The Ubbelohde type OC viscometer camplies with this requirement if the efflux time is greater than 270 s (ASTM viscometer) . Measure the efflux time of each Standard liquid in three to five passages and determine the kinetic energy correction Atsi for each liquid using the equation If the efflux time is less than specified above, a kinetic energy correction shall be made for the viscometer, using the following low-viscosity liquids as Standards : (recognized V25oc @25OC 2. Trichloroethylene analytical grade) 4 0,314 2 mm2ls = 1,316 3 g/ml = (recognized vBoc = 0,369 3 mm2/s @25OC = 1,455 5 g/ml . . . (A.2) where t SI* is the efflux time, in seconds, of the ith Standard liquid; is the kinema tic viscos Iity, in vi second, of the ith Standard liquid; k is the viscometer second squared. constant, millimetres Per in Square millimetres Per Linear interpolation, using the following equations, between the two efflux times ts, and te for the Standard liquids i = 1 and i = 2 (see figure A. 1) gives the kinematic energy correction At, for the efflux time t, of the solvent (chloroform) : At,= 42= The micro-Ubbelohde type MI viscometer camplies if the efflux time is greater than 70 s. 1. Dichloromethane analytical grade) v250c = 0,525 7 mm2/s @25OC = 1,614 4 g/ml Atsi = tsi - 2 Using n-undecane of recognized analytical grade at 25 OC, make three to five passages with the same viscometer and determine the mean efflux time t in accordance with ISO 3105 : 1976, clause 5. Calculate the viscometer constant k from the equation: A.3 3. Tetrachloroethylene (recognized analytical grade) At,, - K,, (y-) At,1 1 - At, -- t sl . . . (A.3) At,, - At, 1 -- 1 1 h2 t SI t0 =------- . . . (A.4) In the same manner, linear interpolation, using the following equations, between tB and ta gives At for the efflux time t of the test Solution: At=Atd-K23(&-+) FD= At, 1 -k2 . . . (A-5) - At, 1 h3 = At, - At 1 1 --P h2 t . . . (A-6) hl Ata Ah At Afs3 111 fs- f& Figure A.1 - Kinetic 11 5 G Reciprocal of eff lux time energy correction as a function of efflux time of the reciprocal 5 ISO 1628-6 I 1990 (i, Annex B (normative) Determination of the limiting The limiting viscosity number [VI for methyl methacrylate polymer solutions may be calculated, in millilitres per gram, from values obtained at a Single concentration by use of the following equation [Zl : viscosity number where y~ is the dynamic viscosity, in millipascal seconds, of the Solution; Q is the dynamic viscosity, in millipascal seconds, of the solvent; [q] = f-f] . . . (B.l) csol;,i,n~ IS the concentration of polymer, in grams per millilitre of Annex C (informative) Bibliography Hl BAUER, H., and MEERENDER, G., Precise viscosity measurements of Newtonian liquids with v < 1 mm% suitable Standards. Rheologica Acta 23: 514-521 (1984). M BILLMEYER,F.W., Jr., Journal of Polymer Science 4: 83 (1949). UDC 678.744.335 : 532.13.08 Descriptors : plastics, Price based on 6 pages 6 polymers, methylmethacrylate, tests, physical tests, determination, viscosity, viscosity index. for the selection of Acknowledgements Members of Technical Committee on General and Raw Materials for Plastics Mr Ahmad Khairuddin Sha’aban (Chairman) Dow Chemical (Malaysia) Sdn Bhd Ms Noraslina Mat Zain (Secretary) SIRIM Berhad Mr Chu Tam Sang Federation of Malaysian Manufacturers Mr Umat Lokman Ahmad Johari Petronas Polymer Technology Centre Ms Zarina Rasmin SIRIM Berhad (Advanced Polymer and Composites Programme) Ms Kamaliah Ahmad SIRIM QAS International Sdn Bhd (Civil and Construction Section) Mr Mohd Helmee Mat Jenan Vinyl Chloride (Malaysia) Sdn Bhd © STANDARDS MALAYSIA 2008 – All rights reserved