EN ISO 1628-5-2015 en Plastics - Determination of the viscosity of polymers in dilute solution using capillary viscometers - Part 5 Thermoplastic polyester (TP) homopolymers and co.pdf

1、BRITISH STANDARDBS ISO1628-5:1998BS 2782-7: Method732E:1998Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 5: Thermoplastic polyester (TP) homopolymers and copolymersICS 83.080.20BS EN ISO 1628-5:2015BS EN ISO 1628-5:2015ISBN 978 0 580 87203 7A

2、mendments/corrigenda issued since publicationDate Comments31 March 2015 This corrigendum renumbers BS ISO 1628-5:1998 as BS EN ISO 1628-5:2015This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Stan

3、dards Board and comes into effect on 15 June 1998 The British Standards Institution 2015. Published by BSI Standards Limited 2015National forewordThis British Standard is the UK implementation of EN ISO 1628-5:2015. It is identical to ISO 1628-5:1998. It supersedes BS ISO 1628-5:1998, which is withd

4、rawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Use

5、rs are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1628-5 March 2015 ICS 83.080.20 English Version Plastics - Determination of the viscosity of polymers in dilute so

6、lution using capillary viscometers - Part 5: Thermoplastic polyester (TP) homopolymers and copolymers (ISO 1628-5:1998) Plastiques - Dtermination de la viscosit des polymres en solution dilue laide de viscosimtres capillaires - Partie 5: Homopolymres et copolymres des polyesters thermoplastiques (TP

7、) (ISO 1628-5:1998) Kunststoffe - Bestimmung der Viskositt von Polymeren in verdnnter Lsung durch ein Kapillarviscosimeter - Teil 5: Thermoplastische Polyester(TP) Homopolymere und Copolymere (ISO 1628-5:1998) This European Standard was approved by CEN on 1 March 2015. CEN members are bound to compl

8、y 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 standards may be obtained on application to the CEN-CENELEC

9、Management Centre 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 notified to the CEN-CENELEC Management Centre has the sam

10、e status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg,

11、 Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 201

12、5 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 1628-5:2015 EEN ISO 1628-5:2015 (E) 3 Foreword The text of ISO 1628-5:1998 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for St

13、andardization (ISO) and has been taken over as EN ISO 1628-5:2015 by Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. 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

14、 by September 2015, and conflicting national standards shall be withdrawn at the latest by September 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all

15、 such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of M

16、acedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 1628-5:1998 has been approved b

17、y CEN as EN ISO 1628-5:2015 without any modification. ii The British Standards Institution 2015BS EN ISO 1628-5:2015EN ISO 1628-5:2015 (E)BS ISO 1628-5:1998 BSI 04-1999 iContentsPageNational foreword Inside front coverForeword iii1 Scope 12 Normative references 13 Principle 14 Solvents 15 Apparatus

18、26 Solvent and solution 27 Procedure 38 Expression of results 49 Test report 4Annex A (informative) Round-robin testing 5Figure A.1 Viscosity number of PET inphenol/1,2-dichlorobenzene (50/50) relative to that in other solvents 6Figure A.2 Viscosity number of PBT in m-cresolrelative to that in other

19、 solvents 7Table A.1 5BS ISO 1628-5:1998 BSI 04-1999 iContentsPageNational foreword Inside front coverForeword iii1 Scope 12 Normative references3 Principle4 Solvents5 Apparatus 26 Solvent and solution7 Procedure 38 Expression of results 49 Test reportAnnex A (informative) Round-robin testing 5Figur

20、e A.1 Viscosity number of PET inphenol/1,2-dichlorobenzene (50/50) relative to that in other solvents 6Figure A.2 Viscosity number of PBT in m-cresolrelative to that in other solvents 7Table A.1 5BS EN ISO 1628-5:2015ISO 1628-5:1998iii The British Standards Institution 2015blankBS ISO 1628-5:1998 BS

21、I 04-1999 11 ScopeThis part of ISO 1628 specifies a method for the determination of the viscosity number (also referred to as “reduced viscosity”) of dilute solutions of thermoplastic polyesters (TPs) in certain specified solvents. The method is applicable to poly(ethylene terephthalate) (PET), poly

22、(butylene terephthalate) (PBT), poly-(cyclohexylenedimethylene terephthalate) (PCT), and poly(ethylene naphthalate) (PEN), as well as to copolyesters and other polyesters, defined in ISO 7792-1, that are soluble in one of the specified solvents under the specified conditions.The viscosity number is

23、determined by the general procedure specified in ISO 1628-1, observing the particular conditions specified in this part of ISO 1628.The determination of the viscosity number of a thermoplastic polyester provides a measure of the relative molecular mass of the polymer.2 Normative referencesThe follow

24、ing 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 inv

25、estigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of current valid International Standards.ISO 1628-1:, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 1: G

26、eneral principles1). ISO 3105:1994, Glass capillary kinematic viscometers Specifications and operating instructions. ISO 3451-2:1984, Plastics Determination of ash Part 2: Polyalkylene terephthalates. ISO 7792-1:1997, Plastics Thermoplastic polyester (TP) moulding and extrusion materials Part 1: Des

27、ignation system and basis for specifications. 3 PrincipleThe times of flow of a solvent and a solution of resin in the solvent at a concentration of 0,005 g/ml are measured at 25 C by conventional methods. The viscosity number is calculated from these measurements and from the known concentration of

28、 the solution. Specific gravity difference and kinetic energy corrections are small in this method and are not applied.4 SolventsWARNING The solvents used are hazardous. Avoid contact with the skin and inhalation of the vapours.4.1 Phenol/1,2-dichlorobenzeneWeigh out 1 part by mass of phenol (analyt

29、ical grade) and dissolve in 1 part by massof 1,2-dichlorobenzene (analytical grade). Work to an accuracy of1% or better in the weighings.4.2 Phenol/1,1,2,2-tetrachloroethaneWeigh out 6 parts by mass of phenol (analytical grade) and dissolve in 4 parts by massof 1,1,2,2-tetrachloroethane (analytical

30、grade), or weigh out 1 part by mass of phenol and dissolve in 1 part by mass of 1,1,2,2-tetrachloroethane. Work to an accuracy of1% or better in the weighings.4.3 o-Chlorophenol, analytical grade.4.4 m-Cresol, meeting the following specifications:appearance: clear and colorless;m-cresol content: 99%

31、(m/m) min.;o-cresol content: 0,3%(m/m) max.;water content: 0,1%(m/m) max.NOTE A solvent of the required purity can be obtained by distillation of chemically pure m-cresol, preferably in vacuo, pressure compensation being effected with nitrogen in order to avoid oxidation. The purity of the solvent m

32、ay be checked by gas chromatography.4.5 Dichloroacetic acid, analytical grade.4.6 Phenol/2,4,6-trichlorophenolWeight out 6 parts by mass of phenol (analytical grade) and dissolve in 4 parts by massof 2,4,6-trichlorophenol (analytical grade).NOTE 2,4,6-trichlorophenol of the required purity can be ob

33、tained by distillation of chemically pure 2,4,6-trichlorophenol.4.7 Storage of the solventsProtect the solvents from light by storing them, for example, in stoppered brown-glass bottles.1) To be published. (Revision of ISO 1628-1:1984)BS EN ISO 1628-5:2015ISO 1628-5:19981 The British Standards Insti

34、tution 2015BS ISO 1628-5:19982 BSI 04-19995 Apparatus5.1 Mill, to reduce the sample to a grain size of about 0,5 mm.5.2 Volumetric flask, of capacity 100 ml, fitted with a ground-glass stopper.5.3 Conical flask, of capacity 150 ml, fitted with a ground-glass stopper.5.4 Burette, graduated in divisio

35、ns of 0,1 ml.5.5 Steam bath, or other means to heat the contents of a flask to 90 to 100 C.5.6 Oil bath, capable of being controlled at 135 to 140 C, or other means to heat the contents of a flask to that temperature range.5.7 Magnetic stirrer, or other equipment to continuously agitate the contents

36、 of a stoppered flask.5.8 Thermostatic bath, capable of being maintained at 25 0,05 C.5.9 Viscometer, suspended-level Ubbelohde type, size No. 1B, 1C or 2, in accordance with ISO 3105.Other types of viscometer listed in ISO 3105 may be used, provided that the results are equivalent to those of the U

37、bbelohde viscometers specified above. However, in cases of dispute, Ubbelohde viscometers shall be used.5.10 Stainless-steel sieve, with a nominal aperture size of 63 to 90 4m, or sintered-glass filter funnel with 40 to 100 4m pore diameter.5.11 Analytical balance, accurate to 0,1 mg.5.12 Stopwatch,

38、 accurate to 0,1 s.5.13 Vacuum dryer, capable of being maintained at about 130 C under vacuum.6 Solvent and solution6.1 Selection of the solvent6.1.1 The value of the viscosity number of a saturated polyester depends on the solvent used. Six different solvents are described in this part of ISO 1628:

39、 phenol/1,2-dichlorobenzene (4.1),phenol/1,1,2,2-tetrachloroethane (4.2),o-chlorophenol (4.3), m-cresol (4.4), dichloroacetic acid (4.5) and phenol/2,4,6-trichlorophenol (4.6).The flow times of the solvents shall be determined at least once each day that they are used (see 7.2). If the flow time of

40、a solvent differs by more than1% from the initial value at the time of preparation, the solvents shall be discarded and fresh solvent prepared.The solvent or solvents to be used for a particular saturated polyester are specified below.6.1.2 For PET, use phenol/1,2-dichlorobenzene(50/50), phenol/1,1,

41、2,2-tetrachloroethane(50/50 or 60/40), o-chlorophenol or dichloroacetic acid as solvent.NOTE Equations for the interconversion of viscosity number determined in these four solvents are presented in Annex A, subclause A.3.1.6.1.3 For PBT and corresponding copolyesters, use phenol/1,1,2,2-tetrachloroe

42、thane (50/50 or 60/40),o-chlorophenol, m-cresol,phenol/1,2-dichlorobenzene (50/50) or dichloroacetic acid as solvent.NOTE Equations for the interconversion of viscosity number determined in these four solvents are presented in Annex A, subclause A.3.2.6.1.4 For PCT, usephenol/1,1,2,2-tetrachloroetha

43、ne (60/40) as solvent.6.1.5 For amorphous PEN, usephenol/1,1,2,2-tetrachloroethane (60/40) as solvent and for crystalline PEN usephenol/2,4,6-trichlorophenol (60/40).6.1.6 For other TP homopolymers and copolymers, m-cresol is the recommended solvent.6.2 Determination of inorganic materials or other

44、additives in the sampleContents of inorganic materials or other additives exceeding 0,5%(m/m) each shall be taken into account in the preparation of the test solution (6.4).6.2.1 Determination of the content of inorganic materialsIf the sample contains inorganic materials, such as fillers or glass f

45、ibres, determine the content in accordance with ISO 3451-2.6.2.2 Determination of the content of other additivesIf the sample contains other additives, such as polyalkenes or flame retardants, determine the content in an appropriate way. Report the procedure(s) used.NOTE When a polyester is a compou

46、nd consisting of many components (flame retardants, fillers, antioxidants, impact modifiers), the analysis of the polyester content is more specific. This can be achieved by hydrolysis of the polyester and subsequent analysis of the monomer(s).6.3 SampleThe sample shall be representative of the mate

47、rial to be tested. Predry the sample at 120 C under vacuum for3h to avoid a decrease in VN by hydrolysis with residual water.BS EN ISO 1628-5:2015ISO 1628-5:1998 The British Standards Institution 2015BS ISO 1628-5:1998 BSI 04-1999 36.4 Preparation of solutionUse one of the following procedures:6.4.1

48、 Procedure AWeigh out, to the nearest 0,2 mg, a test portion m1in the rangewherei is the content of inorganic materials, expressed as a percentage by mass, in the sample, determined in accordance with 6.2.1o is the content of other additives, expressed as a percentage by mass, in the sample, determi

49、ned in accordance with 6.2.2.The corrections for i and o need only be applied if they exceed 0,5%(m/m) each.Transfer the test portion to the volumetric flask (5.2), add 60 ml of solvent, stopper the flask and warm on the steam bath (5.5), with occasional stirring, until the polymer has dissolved completely. On the steam bath, no degradation of the polymer occurs. If, however, long waiting times are undesirable for other reasons, the dissolution may be accelerated by agitating the flask continuously, for example with the ma