DIN EN ISO 1628-3-2010 Plastics - Determination of the viscosity of polymers in dilute solution using capillary viscometers - Part 3 Polyethylenes and polypropylenes (ISO 1628-3 20.pdf

1、October 2010 Translation by DIN-Sprachendienst.English price group 9No 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

2、 83.080.20!$kUV“1725051www.din.deDDIN EN ISO 1628-3Plastics Determination of the viscosity of polymers in dilute solution usingcapillary viscometers Part 3: Polyethylenes and polypropylenes (ISO 1628-3:2010)English translation of DIN EN ISO 1628-3:2010-10Kunststoffe Bestimmung der Viskositt von Poly

3、meren in verdnnter Lsung durch einKapillarviskosimeter Teil 3: Polyethylen und Polypropylen (ISO 1628-3:2010)Englische bersetzung von DIN EN ISO 1628-3:2010-10Plastiques Dtermination de la viscosit des polymres en solution dilue laide de viscosimtres capillaires Partie 3: Polythylnes et polypropylne

4、s (ISO 1628-3:2010)Traduction anglaise de DIN EN ISO 1628-3:2010-10SupersedesDIN EN ISO 1628-3:2003-06www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 14 pages10.10 DIN EN ISO 1628-3:2010-10 2 A comma is used as the decimal marker. Natio

5、nal foreword This standard has been prepared by Technical Committee ISO/TC 61 “Plastics” (Secretariat: ANSI, USA) in collaboration with Technical Committee CEN/TC 249 “Plastics”, (Secretariat: NBN, Belgium) The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (

6、Plastics Standards Committee), Working Committee NA 054-02-06 AA Formmassen aus Polyolefinen. DIN EN ISO 1628 consists of the following parts, under the general title Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers: Part 1: General principles Part 2

7、: Poly(vinyl chloride) resins Part 3: Polyethylenes and polypropylenes In addition, ISO 1628 consists of the following parts, under the above-mentioned general title: Part 4: Polycarbonate (PC) moulding and extrusion materials Part 5: Thermoplastic polyester (TP) homopolymers and copolymers Part 6:

8、Methyl methacrylate polymers 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 1628-2 DIN EN ISO 1628-2 ISO 3105 DIN 51366, DIN 51562-1 Amendments This standard differs from DIN EN ISO 1628-3:2003-06 as follow

9、s: a) the standard has been editorially revised; b) the dated reference ISO 1628-1:1998 has been changed to read ISO 1628-1:2009; c) Subclause 5.1 “Ubbelohde viscometer” has been revised and Table 1 “Ubbelohde viscometers recommended for the determination of the dilute-solution viscosity of polymers

10、” has been included; d) Subclause 5.8 “Drying oven” has been replaced by “Shaker”; e) Subclause 5.11 “Filter funnel” has been included; f) Figure 1 has been revised; DIN EN ISO 1628-3:2010-10 3 g) in Subclause 7.1 “Cleaning the viscometer”, Subclause 7.1.2 has been reformulated; h) Subclause 7.3 “Ch

11、oice of polymer solution concentration” has been restructured; i) in Table 2 “Concentration c to be used as a function of the reduced voscosity to be measured” (former Table 1), column “Reduced viscosity”, the value “40” has been changed to read “ 40”; j) Subclause 7.4.2 in Subclause 7.4 “Preparatio

12、n of the solution” has been reformulated; k) Subclause 7.5 “Measurement of efflux time of solution” has been reformulated and now includes a description of the filtration of the solution; l) Clause 9 “Test report” now includes the information whether or not the solution was filtered. Previous editio

13、ns DIN 53728-4: 1973-08, 1975-03 DIN EN ISO 1628-3: 1999-12, 2003-06 DIN EN ISO 1628-3:2010-10 4 National Annex NA (informative) Bibliography DIN 51366, Testing of mineral oil hydrocarbons Measurement of kinematic viscosity by means of the Cannon-Fenske viscometer, for opaque liquids DIN 51562-1, Vi

14、scometry Measurement of kinematic viscosity by means of the Ubbelohde viscometer Part 1: Viscometer specification and measurement procedure DIN EN ISO 1628-1, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 1: General principles DIN EN ISO 1628

15、-2, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscosimeters Part 2: Poly(vinyl chloride) resins EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1628-3 May 2010 ICS 83.080.20 Supersedes EN ISO 1628-3:2003English Version Plastics - Determination of

16、 the viscosity of polymers in dilute solution using capillary viscometers - Part 3: Polyethylenes and polypropylenes (ISO 1628-3:2010) Plastiques - Dtermination de la viscosit des polymres en solution dilue laide de viscosimtres capillaires - Kunststoffe - Bestimmung der Viskositt von Polymeren in v

17、erdnnter Lsung durch ein Kapillarviskosimeter - Teil 3: Polyethylen und Polypropylen (ISO 1628-3:2010) This European Standard was approved by CEN on 29 April 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standa

18、rd 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 Management Centre or to any CEN member. This European Standard exists in three official versions (English, French,

19、 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, C

20、yprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION

21、 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 1628-3:2010: EPartie 3: Polythylnes et polypropylnes(ISO 1

22、628-3:2010) 2 DIN EN ISO 1628-3:2010-10 EN ISO 1628-3:2010 (E) Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Solvent 4 5 Apparatus .5 6 Test sample 6 7 Procedure .7 7.1 Cleaning the viscometer .7 7.2 Measurement of efflux time of solvent 7 7.3 Choice of polymer solution c

23、oncentration .7 7.4 Preparation of the solution .7 7.5 Measurement of efflux time of solution.8 8 Expression of results 9 8.1 Reduced viscosity, I 9 8.2 Intrinsic viscosity, 9 8.3 Precision.9 9 Test report . 10 3 Foreword This document (EN ISO 1628-3:2010) has been prepared by Technical Committee IS

24、O/TC 61 “Plastics“ in collaboration with 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 by November 2010, and confl

25、icting national standards shall be withdrawn at the latest by November 2010. 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. This docu

26、ment supersedes EN ISO 1628-3:2003. 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, France, German

27、y, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 1628-3:2010 has been approved by CEN as a EN ISO 1628-3:2010 wi

28、thout any modification. DIN EN ISO 1628-3:2010-10 EN ISO 1628-3:2010 (E) 1 Scope This part of ISO 1628 defines particular conditions for determining the reduced viscosity (also known as viscosity number) and intrinsic viscosity of polyethylenes and polypropylenes at 135 C in dilute solution. The vis

29、cosity of polymer solutions may be affected by additives present in the sample. The value of a reduced viscosity determined by this method may therefore be unreliable if the sample contains fillers or other additives. NOTE Reduced viscosity is also known as the Staudinger function (Jv) and intrinsic

30、 viscosity as the Staudinger index (Jg). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendm

31、ents) applies. ISO 1628-1:2009, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 1: General principles ISO 3105:1994, Glass capillary kinematic viscometers Specifications and operating instructions 3 Principle The times of flow of a solvent and

32、a solution of polymer at a specified concentration in that solvent are measured at 135 C. The reduced viscosity and intrinsic viscosity are calculated from these measurements and from the known concentration of the solution. Ethylene polymers and isotactic polypropylenes are not soluble at room temp

33、erature in any known solvents. Precautions must therefore be taken during the test to avoid any precipitation of polymer, which would give an incorrect solution concentration. DIN EN ISO 1628-3:2010-10 EN ISO 1628-3:2010 (E) 44 Solvent 4.1 Decahydronaphthalene, analytical-reagent grade, redistilled

34、at a temperature not higher than 65 C and a pressure of approximately 500 Pa; its peroxidation shall be prevented by suitable means, for example distilling in the presence of hydroquinone. Immediately after redistillation of the decahydronaphthalene, 0,2 % by mass of antioxidant shall be added to in

35、hibit oxidation during the viscosity determination. Antioxidants which have been found satisfactory include: 4,4-thio-bis-(6-tert-butyl-3-methyl)phenol; bis-(2-hydroxy-3-tert-butyl-5-methyl)phenylmethane; octadecyl-3-(3,5-di-tert-butyl-4-hydroxyphenyl)-n-propionate; tetrakismethylene 3-(3,5-di-tert-

36、butyl-4-hydroxyphenyl)-n-propionatemethane. Filter the solvent through a P100 sintered-glass funnel. Solvent stabilized in this way gives polymer solutions that are resistant to oxidation at 135 C for several hours. 5 Apparatus 5.1 Ubbelohde viscometer, preferably either type 0B as specified in Tabl

37、e B.4 of ISO 3105:1994 or type 0a as specified in Table B.9 of ISO 3105:1994, having a nominal viscometer constant of 0,005 (mm2/s)/s. These viscometers are shown in Figure 1 and Figure 2 of ISO 1628-1:2009 and the principal parameters are given in Table 1. Other types of viscometer described in ISO

38、 3105:1994 may be used provided they give equivalent results. However, in cases of dispute, an Ubbelohde viscometer shall be used. Table 1 Ubbelohde viscometers recommended for the determination of the dilute-solution viscosity of polymers Nominal viscometer constant Inside diameter of tube R Volume

39、 of bulb C Inside diameter of tube P Type (mm2/s)/s mm (2 ) ml (5 %) mm (5 ) 0B 0,005 0,46 3,0 6,0 0a 0,005 0,53 5,7 6,0 If the polymer solution needs to be filtered, the modified Ubbelohde viscometer design shown in Figure 1 may be used (the essential dimensions of the modified design are the same

40、as those of the type 0B and type 0a viscometers, but tube L has been modified to include a filter). 5.2 Viscometer holder, to hold the viscometer firmly in the correct position in the thermostatic bath. 5.3 Thermostatic bath, maintained at 135 C 0,2 C, in accordance with ISO 1628-1. 5.4 Thermostatic

41、 bath, maintained at 20 C 0,1 C. 5.5 Temperature-measuring device, in accordance with ISO 1628-1 (scale division 0,1 C). 5.6 Timer, of any kind provided that it can be read to the nearest 0,1 s or better and that it operates at a rate which is constant to 0,1 % over 15 min. DIN EN ISO 1628-3:2010-10

42、 EN ISO 1628-3:2010 (E) 55.7 Analytical balance, accurate to 0,1 mg. 5.8 Shaker, fitted in a heating bath capable of maintaining a temperature of 150 C 2 C, for dissolving the polymer in the solvent. The shaker may be of the rotating, the reciprocating or another suitable type. NOTE Certain types of

43、 shaker are not suitable for preparation of PE-UHMW solutions. 5.9 Glass-stoppered flask, capacity 100 ml. 5.10 Graduated pipette, capacity 50 ml. 5.11 Filter funnel, with a P100 sintered-glass disc. Dimensions in millimetres Key 1 P100 sintered-glass disc Figure 1 Ubbelohde viscometer with filter s

44、tick DIN EN ISO 1628-3:2010-10 EN ISO 1628-3:2010 (E) 66 Test sample 6.1 The test sample shall be in the form of dry powder or very small pieces to facilitate dissolution. 6.2 If the sample is a manufactured article, cut it into very small pieces (for example by cutting and grinding in the presence

45、of solid carbon dioxide). If the sample is in the form of granules, reduce the particle size by grinding in the same way. Since the reduced viscosity of material from the surface of a manufactured article could differ from that from the interior, one can either measure the reduced viscosity for the

46、whole article by grinding it, homogenizing the ground material, dissolving a portion and taking a test sample from the solution; or measure the reduced viscosities for the surface and the interior separately by cutting small pieces from the surface and from the interior, grinding and homogenizing th

47、em separately and testing a sample taken from each. 7 Procedure 7.1 Cleaning the viscometer 7.1.1 Before its utilization, or when inconsistent results are obtained, and in any case at regular intervals, clean the viscometer as specified in Annex A of ISO 1628-1:2009. 7.1.2 Between two successive det

48、erminations, clean the viscometer with the solvent being used for the determinations. During the cleaning procedure, maintain the viscometer, as well as the solvent, at 135 C in thermostatic bath 5.3. Remove the solvent by suction and dry the viscometer with dust-free and oil-free air or nitrogen. 7

49、.2 Measurement of efflux time of solvent Determine the efflux time of the solvent by the procedure given in 7.5 for the solution. Use the average value of three consecutive readings agreeing to within 0,2 s in the calculation of the viscosity number. 7.3 Choice of polymer solution concentration 7.3.1 The polymer concentration shall be such that the ratio between the solution efflux time t and the solvent efflux time t0lies between 1,2 and 2,0. 7.3.2 If th