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

1、May 2015 Translation by DIN-Sprachendienst.English price group 10No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 83

2、.080.20!%B“2315890www.din.deDDIN EN ISO 1628-5Plastics Determination of the viscosity of polymers in dilute solution usingcapillary viscometers Part 5: Thermoplastic polyester (TP) homopolymers and copolymers(ISO 1628-5:1998);English version EN ISO 1628-5:2015,English translation of DIN EN ISO 1628-

3、5:2015-05Kunststoffe Bestimmung der Viskositt von Polymeren in verdnnter Lsung durch einKapillarviscosimeter Teil 5: Thermoplastische Polyester (TP) Homopolymere und Copolymere(ISO 1628-5:1998);Englische Fassung EN ISO 1628-5:2015,Englische bersetzung von DIN EN ISO 1628-5:2015-05Plastiques Dtermina

4、tion de la viscosit des polymres en solution dilue laide de viscosimtres capillaires Partie 5: Homopolymres et copolymres des polyesters thermoplastiques (TP)(ISO 1628-5:1998);Version anglaise EN ISO 1628-5:2015,Traduction anglaise de DIN EN ISO 1628-5:2015-05SupersedesDIN 53728-3:1985-01, withdrawn

5、2014-04www.beuth.deDocument comprises 16 pagesIn case of doubt, the German-language original shall be considered authoritative.04.15 DIN EN ISO 1628-5:2015-05 2 A comma is used as the decimal marker. National foreword The text of ISO 1628-5:1998 has been prepared by Technical Committee ISO/TC 61 “Pl

6、astics” and has been taken over as EN ISO 1628-5:2015 by Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the DIN-Normenausschuss Kunststoffe (DIN Standards Committee Plastics), Working Committee NA 054-02-10 AA Thermo

7、plast-Formmassen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 1628-1 DIN EN ISO 1628-1 ISO 3451-2 DIN ISO 3451-2 ISO 7792-1 DIN EN ISO 7792-1 Amendments This standard differs from DIN 53728-3:1985-01 (withdrawn 2014-04) as follows:

8、a) specifications relating to solvents and the selection of solvents have been extended and completely revised; b) two procedures can be used for the preparation of the solution; c) the determination of the viscosity number has been modified. Previous editions DIN 53728-3: 1973-08, 1985-01 National

9、Annex NA (informative) Bibliography DIN EN ISO 1628-1, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometer Part 1: General principles DIN ISO 3451-2, Plastics Determination of ash Part 2: Poly(alkyleneterephthalates) DIN EN ISO 7792-1, Plastics Thermopla

10、stic polyester (TP) moulding and extrusion materials Part 1: Designation system and basis for specifications 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 solution using capilla

11、ry 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) (ISO 1628-5:1998) K

12、unststoffe - 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 comply with the CEN/CENEL

13、EC 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 Management Centre or

14、 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 same status as the offi

15、cial 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, Malta, Netherlands,

16、 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 2015 CEN All rights of

17、exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 1628-5:2015 EDIN EN ISO 1628-5:2015-05 EN ISO 1628-5:2015 (E) 2Contents Page Foreword . 3 1 Scope 4 2 Normative references 4 3 Principle 5 4 Solvents 5 4.1 Phenol/1,2-dichlorobenzene .5 4.2 Phenol/

18、1,1,2,2-tetrachloroethane .5 4.3 o-Chlorophenol, analytical grade . 5 4.4 m-Cresol, meeting the following specifications . 5 4.5 Dichloroacetic acid, analytical grade 5 4.6 Phenol/2,4,6-trichlorophenol 5 4.7 Storage of the solvents . 5 5 Apparatus . 6 6 Solvent and solution . 6 6.1 Selection of the

19、solvent 6 6.2 Determination of inorganic materials or other additives in the sample 7 6.2.1 Determination of the content of inorganic materials . 7 6.2.2 Determination of the content of other additives 7 6.3 Sample 7 6.4 Preparation of solution . 7 6.4.1 Procedure A . 76.4.2 Procedure B .8 7 Procedu

20、re .9 7.1 Preparatory operations .9 7.2 Measurement of flow time 9 8 Expression of results 9 9 Test report 10 Annex A (informative) Round-robin testing.11 A.1 General .11 A.2 Repeatability and reproducibility .11 A.3 Interconversion of the viscosity numbers determined in different solvents 11 A.3.1

21、Viscosity number of PET 11 A.3.2 Viscosity number of PBT 12 Foreword The text of ISO 1628-5:1998 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 1628-5:2015 by Technical Committee CEN/TC 249 “

22、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 by September 2015, and conflicting national standards shall be withdrawn at the latest by September

23、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 such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organi

24、zations 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 Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, M

25、alta, 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 by CEN as EN ISO 1628-5:2015 without any modification. DIN EN ISO 1628-5:2015-05 EN ISO 1628-5:2015 (E

26、) 3 1 ScopeThis part of ISO 1628 specifies a method for the determination of the viscosity number (also referred toas “reduced viscosity”) of dilute solutions of thermoplastic polyesters (TPs) in certain specified solvents.The method is applicable to poly(ethylene terephthalate) (PET), poly(butylene

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

28、by the general procedure specified in ISO 1628-1, observing theparticular conditions specified in this part of ISO 1628.The determination of the viscosity number of a thermoplastic polyester provides a measure of therelative molecular mass of the polymer.2 Normative referencesThe following standards

29、 contain provisions which, through reference in this text, constitute provisionsof this part of ISO 1628. At the time of publication, the editions indicated were valid. All standards aresubject to revision, and parties to agreements based on this part of ISO 1628 are encouraged toinvestigate the pos

30、sibility of applying the most recent editions of the standards indicated below.Members of IEC and ISO maintain registers of current valid International Standards.ISO 1628-1:1), Plastics - Determination of the viscosity of polymers in dilute solution using capillaryviscometers - Part 1: General princ

31、iples.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:Designation

32、 system and basis for specifications._1) To be published. (Revision of ISO 1628-1:1984)DIN EN ISO 1628-5:2015-05 EN ISO 1628-5:2015 (E) 4 3 PrincipleThe times of flow of a solvent and a solution of resin in the solvent at a concentration of 0,005 g/ml aremeasured at 25 C by conventional methods. The

33、 viscosity number is calculated from thesemeasurements and from the known concentration of the solution. Specific gravity difference and kineticenergy corrections are small in this method and are not applied.4 SolventsWARNING - The solvents used are hazardous. Avoid contact with the skin and inhalat

34、ion of thevapours.4.1 Phenol/1,2-dichlorobenzeneWeigh out 1 part by mass of phenol (analytical grade) and dissolve in 1 part by mass of 1,2-dichlorobenzene (analytical grade). Work to an accuracy of 1 % or better in the weighings.4.2 Phenol/1,1,2,2-tetrachloroethaneWeigh out 6 parts by mass of pheno

35、l (analytical grade) and dissolve in 4 parts by mass of 1,1,2,2-tetrachloroethane (analytical grade), or weigh out 1 part by mass of phenol and dissolve in 1 part bymass of 1,1,2,2-tetrachloroethane. Work to an accuracy of 1 % or better in the weighings.4.3 o-Chlorophenol, analytical grade.4.4 m-Cre

36、sol, meeting the following specifications:appearance: clear and colorless;m-cresol content: 99 % (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, press

37、ure compensation being effected with nitrogen in order to avoid oxidation.The purity of the solvent may 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 mass o

38、f 2,4,6-trichlorophenol (analytical grade).NOTE - 2,4,6-trichlorophenol of the required purity can be obtained by distillation of chemically pure2,4,6-trichlorophenol.4.7 Storage of the solventsProtect the solvents from light by storing them, for example, in stoppered brown-glass bottles.DIN EN ISO

39、1628-5:2015-05 EN ISO 1628-5:2015 (E) 5 5 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 divisions

40、 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 flaskto that temperature range.5.7 Magnetic stirrer, or other equipment to continuously agitate the contents of

41、 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 tothose of the Ubb

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

43、ate 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. Sixdifferent solvents are described in this part of ISO 1628: phenol

44、/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) andphenol/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). Ifthe flow time of a solven

45、t differs by more than 1 % from the initial value at the time of preparation, thesolvents 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/1,1,2,2-te

46、trachloroethane (50/50 or60/40), o-chlorophenol or dichloroacetic acid as solvent.DIN EN ISO 1628-5:2015-05 EN ISO 1628-5:2015 (E) 6 NOTE - Equations for the interconversion of viscosity number determined in these four solvents arepresented in annex A, subclause A.3.1.6.1.3 For PBT and corresponding

47、 copolyesters, use phenol/1,1,2,2-tetrachloroethane (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 arepresented in annex A, subclause A.3.2.6.1.4 For PCT, use phenol/1,1,2,2-tetrachloroethane (60/40) as solvent.6.1.5 For amorphous PEN, use phenol/1,1,2,2-tetrachloroethane (60/40) as solvent and for crystallinePEN use p