1、BS EN ISO1628-3:2010ICS 83.080.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Determination of theviscosity of polymersin dilute solution usingcapillary viscometersPart 3: Polyethylenes andpolypropylenes (ISO 1628-3:2010)This British Standardwas publ
2、ished under theauthority of the StandardsPolicy and StrategyCommittee on 30 June2010 BSI 2010ISBN 978 0 580 57208 1Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 1628-3:2010National forewordThis British Standard is the UK implementation of EN ISO 1628-3:2010.It supersedes BS EN
3、 ISO 1628-3:2003 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PRI/82, Thermoplastic materials.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necess
4、ary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1628-3 May 2010 ICS 83.080.20 Supersedes EN ISO 1628-3:2003English Version Plastics
5、- Determination of 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 - Partie 3: Polythylnes et polypropylnes
6、(ISO 1628-3:2010) Kunststoffe - Bestimmung der Viskositt von Polymeren in verdnnter 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
7、 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 Management Centre or to any CEN member.
8、 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 Management Centre has the same status as the official versions. CEN members
9、are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Swe
10、den, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION 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.
11、 Ref. No. EN ISO 1628-3:2010: EBS EN ISO 1628-3:2010EN ISO 1628-3:2010 (E) 3 Foreword This document (EN ISO 1628-3:2010) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This Europea
12、n 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 conflicting national standards shall be withdrawn at the latest by November 2010. Attention is drawn to the possibility that some of the elem
13、ents 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 document supersedes EN ISO 1628-3:2003. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the follo
14、wing countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slova
15、kia, 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 without any modification. BS EN ISO 1628-3:2010ISO 1628-3:2010(E) ISO 2010 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Nor
16、mative references1 3 Principle1 4 Solvent2 5 Apparatus.2 6 Test sample4 7 Procedure.4 7.1 Cleaning the viscometer.4 7.2 Measurement of efflux time of solvent4 7.3 Choice of polymer solution concentration .4 7.4 Preparation of the solution.5 7.5 Measurement of efflux time of solution 5 8 Expression o
17、f results6 8.1 Reduced viscosity, I6 8.2 Intrinsic viscosity, h6 8.3 Precision.7 9 Test report7 BS EN ISO 1628-3:2010ISO 1628-3:2010(E) iv ISO 2010 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member
18、bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each 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
19、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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directive
20、s, Part 2. The main task of technical committees is to prepare International Standards. 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 least 75 % of the member bodies c
21、asting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 1628-3 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9,
22、 Thermoplastic materials. This third edition cancels and replaces the second edition (ISO 1628-3:2001), which has been technically revised. The main changes relate to the way in which the solution of the polymer under test is prepared and introduced into the viscometer. ISO 1628 consists of the foll
23、owing parts, under the general title Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers: Part 1: General principles Part 2: Poly(vinyl chloride) resins Part 3: Polyethylenes and polypropylenes Part 4: Polycarbonate (PC) moulding and extrusion materials
24、 Part 5: Thermoplastic polyester (TP) homopolymers and copolymers Part 6: Methyl methacrylate polymers BS EN ISO 1628-3:2010INTERNATIONAL STANDARD ISO 1628-3:2010(E) ISO 2010 All rights reserved 1Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part
25、3: Polyethylenes and polypropylenes 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 viscosity of polymer solutions may be af
26、fected 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 viscosity as the Staudinger index (J
27、g). 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 amendments) applies. ISO 1628-1:2009, Plast
28、ics 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 a solution of polymer at a specified
29、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 temperature in any known solvents. Precau
30、tions must therefore be taken during the test to avoid any precipitation of polymer, which would give an incorrect solution concentration. BS EN ISO 1628-3:2010ISO 1628-3:2010(E) 2 ISO 2010 All rights reserved4 Solvent 4.1 Decahydronaphthalene, analytical-reagent grade, redistilled at a temperature
31、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 inhibit oxidation d
32、uring 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-butyl-4-hydroxyph
33、enyl)-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 Table B.4 of ISO 3105
34、: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 3105:1994 may be
35、 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 of bulb C Inside
36、 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 as those of the t
37、ype 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 bath, maintained
38、 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. BS EN ISO 1628-3:2010ISO 1628-3:2010(E) IS
39、O 2010 All rights reserved 35.7 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
40、 of 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 filte
41、r stick BS EN ISO 1628-3:2010ISO 1628-3:2010(E) 4 ISO 2010 All rights reserved6 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 gr
42、inding in the presence 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 red
43、uced viscosity for the 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, grind
44、ing and homogenizing them 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 Bet
45、ween two successive determinations, 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-
46、free air or nitrogen. 7.2 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 solu
47、tion 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 the approximate value of the reduced viscosity of the polymer is known, choose the concentration from Table 2. Table 2 C
48、oncentration c to be used as a function of the reduced viscosity to be measured Reduced viscosity Concentration, c ml/g g/ml W 40 but 1 000 but u 5 000 0,000 2 BS EN ISO 1628-3:2010ISO 1628-3:2010(E) ISO 2010 All rights reserved 57.3.3 If the approximate value of the reduced viscosity of the polymer
49、 is not known, test a solution of concentration 0,001 g/ml. If the reduced viscosity so obtained is not in the range prescribed in Table 2 for that concentration, repeat the test with the concentration in Table 2 corresponding to the value of the viscosity obtained. 7.4 Preparation of the solution 7.4.1 Calculate, to the nearest 1 mg, the mass m, in grams, of sample to be dissolved, using the equation: mcV= where c is the concentration, in grams per millilitre, o
