DIN EN ISO 307-2013 Plastics - Polyamides - Determination of viscosity number (ISO 307 2007 + Amd 1 2013) German version EN ISO 307 2007 + A1 2013《塑料 聚酰胺 粘度值的测定(ISO 307-2007+Amd 1-.pdf

1、August 2013 Translation by DIN-Sprachendienst.English price group 17No 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!%i“2047098www.din.deDDIN EN ISO 307Plastics Polyamides Determination of viscosity number (ISO 307:2007 + Amd 1:2013);English version EN ISO 307:2007 + A1:2013,English translation of DIN EN ISO 307:2013-08Kunststoffe Polyamide Bestimmung der Viskosittszahl (ISO 307:2007 + Amd 1:2013);Engli

3、sche Fassung EN ISO 307:2007 + A1:2013,Englische bersetzung von DIN EN ISO 307:2013-08Plastiques Polyamides Dtermination de lindice de viscosit (ISO 307:2007 + Amd 1:2013);Version anglaise EN ISO 307:2007 + A1:2013,Traduction anglaise de DIN EN ISO 307:2013-08SupersedesDIN EN ISO 307:2007-08www.beut

4、h.deDocument comprises 41 pagesIn case of doubt, the German-language original shall be considered authoritative.08.13 DIN EN ISO 307:2013-08 2 A comma is used as the decimal marker. National foreword This document (EN ISO 307:2007 + A1:2013) has been prepared by Technical Committee ISO/TC 61 “Plasti

5、cs”, Subcommittee SC 9 “Thermoplastic materials” in collaboration with Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-02-10 AA

6、Thermoplast-Formmassen. This standard includes Amendment A1 approved by CEN on 02 April 2013. The start and finish of text introduced or altered by amendment is indicated in the text by tags !“. The DIN Standards corresponding to the International Standards referred to in this document are as follow

7、s: ISO 1042 DIN EN ISO 1042 ISO 1628-1 DIN EN ISO 1628-1 ISO 1874-1 DIN EN ISO 1874-1 ISO 3105 DIN 51562-1 (modified) ISO 3451-4 DIN EN ISO 3451-4 ISO 15512 DIN EN ISO 15512 Amendments This standard differs from DIN EN ISO 307:2007-08 as follows: a) in Clause 2, the reference to JIS K 6920-2:2000 ha

8、s been transferred to the Bibliography; b) in Subclause 5.1.7, the density of the orthophosphoric acid has been changed to g/ml; c) in Subclause 10.2.2, the first sentence “Weigh, to the nearest 0,2 mg, a test portion of (mc 5) mg” has been replaced by “Weigh, to the nearest 0,2 mg, a test portion o

9、f mass mt, where mtlies in the range (mc 5) mg”; d) in Subclauses 10.2.3 and 10.2.4, the first sentence “Weigh, to the nearest 0,2 mg, a test portion of (mc 10 %) mg” has been replaced by “Weigh, to the nearest 0,2 mg, a test portion of mass mt, where mtlies in the range (mc 10 %) mg”; e) in Subclau

10、se 10.2.4, EXAMPLE, “1,130 0 kg/m3” has been replaced by “1,130 0 kg/dm3” and “1,204 0 kg/m3” has been replaced by “1,204 0 kg/dm3”; f) in Clause 11, Equation (6), mchas been replaced by mtand in the definitions of the symbols used in the equations “mc” has been replaced by “mtis the mass of the tes

11、t portion taken in 10.2.2, 10.2.3 or 10.2.4, in milligrams”; g) the title of Figure B.1 has been corrected to read “Example of flow time/concentration relationship”; h) in Table D.1, heading and first line, the unit of density “kg/m3” has been replaced by “kg/dm3”; i) throughout the document, “JIS K

12、 6920-2:2000, Annex B” has been replaced by “JIS K 6920-2:2009, Annex JA”; j) the Bibliography in the National Annex NA (informative) has been updated. Previous editions DIN 53727: 1963-04, 1967-11, 1971-06, 1980-01 DIN EN ISO 307: 1998-03, 2003-12, 2007-08 DIN EN ISO 307:2013-08 3 National Annex NA

13、 (informative) Bibliography DIN 51562-1, Viscometry Measurement of kinematic viscosity by means of the Ubbelohde viscometer Part 1: Viscometer specification and measurement procedure DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN EN ISO 1628-1, Plastics Determination of the vis

14、cosity of polymers in dilute solution using capillary viscometer Part 1: General principles DIN EN ISO 1874-1, Plastics Polyamide (PA) moulding and extrusion materials Part 1: Designation system and basis for specification DIN EN ISO 3451-4, Plastics Determination of ash Part 4: Polyamides DIN EN IS

15、O 15512, Plastics Determination of water content DIN EN ISO 307:2013-08 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 307 May 2007 + A1 April 2013 ICS 83.080.01 Supersedes EN ISO 307:2003English Version Plastics - Polyamides - Determination of viscosity

16、number (ISO 307:2007 + Amd 1:2013) Plastiques - Polyamides - Dtermination de lindice de viscosit (ISO 307:2007 + Amd 1:2013) Kunststoffe - Polyamide - Bestimmung der Viskosittszahl (ISO 307:2007 + Amd 1:2013) EN ISO 307:2013 was approved by CEN on 2007-05-14 and Amendment A1:2013 on 2013-04-02. CEN

17、members are bound to comply 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 appli

18、cation to the CEN-CENELEC 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 Man

19、agement Centre has the same 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, Latv

20、ia, Lithuania, Luxembourg, 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 Management Centre: Avenue Marnix 17, B-100

21、0 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 307:2007 + A1:2013 EEN ISO 307:2007 + A1:2013 (E) 2 Contents Page Foreword to EN ISO 307:2007 3 !Foreword to EN ISO 307:2007/A1:2013 .3 Introduction .4 1 Scope 5 2

22、 Normative references 5 3 Terms and definitions .6 4 Principle 7 5 Reagents and materials 7 5.1 Solvents and reagents 7 5.2 Cleaning liquids .8 6 Apparatus .8 7 Preparation of test samples 9 7.1 General 9 7.2 Samples containing less than 98 % (by mass) polyamide 9 8 Calculation of test portion 10 9

23、Selection of solvent .10 10 Procedure .11 10.1 Cleaning of the viscometer .11 10.2 Preparation of test solution 11 10.3 Measurement of flow times .13 11 Expression of results 14 12 Repeatability and reproducibility .14 13 Relationship between the viscosity number determined in 96 % (by mass) sulfuri

24、c acid solution and the viscosity determined in various solvents 15 14 Test report 15 Annex A (informative) Determination of the concentration of commercial sulfuric acid (95 % to 98 %) and adjustment to 96 % by titration 17 Annex B (informative) Determination of the concentration of sulfuric acid (

25、95 % to 98 %) and adjustment to 96 % by flow time measurement in a small capillary viscometer 20 Annex C (informative) Determination of the concentration of commercial formic acid and adjustment to 90 % by titration 22 Annex D (informative) Determination of the concentration of commercial formic aci

26、d and adjustment to 90 % by density measurement .24 Annex E (informative) Relationship between the viscosity number determined in 96 % (by mass) sulfuric acid solution and the viscosity determined in various solvents 27 Bibliography 37 DIN EN ISO 307:2013-08 EN ISO 307:2007 + A1:2013 (E) 3Foreword t

27、o EN ISO 307:2007 This document (EN ISO 307:2007) 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 European Standard shall be given the status of a national standard, either by

28、 publication of an identical text or by endorsement, at the latest by November 2007, and conflicting national standards shall be withdrawn at the latest by November 2007. This document supersedes EN ISO 307:2003. According to the CEN/CENELEC Internal Regulations, the national standards organizations

29、 of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, S

30、lovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 307:2007 has been approved by CEN as EN ISO 307:2007 without any modifications. !Foreword to EN ISO 307:2007/A1:2013This document (EN ISO 307:2007/A1:2013) has been prepared by Technical Committee IS

31、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 October 2013, and confl

32、icting national standards shall be withdrawn at the latest by October 2013. 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

33、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 Macedonia, France, Germany, Gree

34、ce, 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 307:2007/Amd 1:2013 has been approved by CEN as EN ISO 307:200

35、7/A1:2013 without any modification.“ DIN EN ISO 307:2013-08 EN ISO 307:2007 + A1:2013 (E) 4 Introduction This International Standard specifies a method for the determination of the viscosity number of dilute solutions of polyamides in certain specified solvents. The determination of the viscosity nu

36、mber of a polyamide provides a value that depends on the molecular mass of the polymer, but does not strictly correlate with the molecular mass. Additives such as flame-retardants and modifiers often interfere with the viscosity measurement and may have an increasing effect on the viscosity number i

37、n one solvent and a decreasing effect in another solvent. The extent of the effect depends among others on the additive, the quantity of the additive, the presence of other additives and reactions. The viscosity number of a polyamide sample containing additives that interfere with the viscosity meas

38、urement, measured in a specific solvent, represents a specific viscosity number for the polyamide under investigation and the actual measurement conditions. The measured viscosity number cannot, in principle, be converted from one solvent to another and is only suitable for intra-product comparison.

39、 The viscosity number of pure polyamides or polyamides containing additives that do not interfere with the viscosity measurement can be converted from one solvent to another by a general relationship for that type of polyamide. Polyamide test samples for the determination of the viscosity number mus

40、t be completely soluble in the solvents mentioned. Additives contained in them, like glass and carbon fibres, must be separated from the solution. As it is not possible to distinguish between extractables such as caprolactam, its oligomers and other extractable additives, these are considered as an

41、essential part of the sample and therefore included in the sample mass. The test method is applicable for production control and intra-product comparison even if the polyamide contains additives that do interfere with the viscosity measurement. However, it should be realised that deviations of the v

42、iscosity number can be caused by either the polyamide itself, effects caused by the additives present, or a combination of these. The interference of additives with the viscosity determination can be checked by comparing the viscosity results of dry blend mixtures and regular production samples at s

43、everal concentrations of the additive under investigation and in the solvents concerned. It should be noted that the other additives present also could influence the viscosity result. The repeatability and reproducibility of the test method are strongly influenced by the correctness of the solvent c

44、oncentration, the use of the Hagenbach correction if applicable and the temperature of the solvent on diluting the sample solution. In this International Standard two specific viscometers are recommended. Furthermore, other types of viscometers listed in ISO 3105 may also be used, provided that the

45、results are demonstrated to be equivalent to those measured with the recommended viscometers. It is to be expected that in the next revision the use of the other types of viscometers will be excluded. DIN EN ISO 307:2013-08 EN ISO 307:2007 + A1:2013 (E) 51 Scope This International Standard specifies

46、 a method for the determination of the viscosity number of dilute solutions of polyamides in certain specified solvents. Polyamide samples must be completely soluble in the solvents mentioned. Additives such as flame-retardants and modifiers often interfere with the viscosity measurement, having an

47、increasing effect on the viscosity number in formic acid and a decreasing effect on the viscosity number in sulfuric acid. The extent of the effect for polyamide compounds depends on the additive, the quantity of the additive, the presence of other additives and the compounding conditions. For pure

48、polyamides or polyamides containing additives that do not interfere with the viscosity measurement, the determination of the viscosity number of a polyamide provides a measure of the molecular mass of the polymer. The viscosity number of pure polyamides or polyamides which contain additives that do not interfere with the viscosity measurement can be converted from one solvent to another. The viscosity number of polyamides containing additives that do interfere with the viscosity measurement is specific to the s