DIN EN ISO 16014-5-2012 Plastics - Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography - Part 5 Method using lig.pdf

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1、October 2012 Translation by DIN-Sprachendienst.English price group 14No 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).IC

2、S 83.080.01; 71.040.50!$|c“1918964www.din.deDDIN EN ISO 16014-5Plastics Determination of average molecular mass and molecular massdistribution of polymers using size-exclusion chromatography Part 5: Method using light-scattering detection (ISO 16014-5:2012);English version EN ISO 16014-5:2012,Englis

3、h translation of DIN EN ISO 16014-5:2012-10Kunststoffe Bestimmung der durchschnittlichen Molmasse und der Molmassenverteilung vonPolymeren mittels Gelpermeationschromatographie Teil 5: Lichtstreudetektionsverfahren (ISO 16014-5:2012);Englische Fassung EN ISO 16014-5:2012,Englische bersetzung von DIN

4、 EN ISO 16014-5:2012-10Plastiques Dtermination de la masse molculaire moyenne et de la distribution des massesmolculaires de polymres par chromatographie dexclusion strique Partie 5: Mthode utilisant la dtection par diffusion lumineuse (ISO 16014-5:2012);Version anglaise EN 16014-5:2012,Traduction a

5、nglaise de DIN EN ISO 16014-5:2012-10www.beuth.deDocument comprises 30 pagesIn case of doubt, the German-language original shall be considered authoritative.09.12 DIN EN ISO 16014-5:2012-10 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Commit

6、tee ISO/TC 61 “Plastics”, Subcommittee SC 5 “Physical-chemical properties” (Secretariat: DIN, Germany) in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Beschichtung

7、sstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee), Working Committee NA 002-00-02 AA Lackrohstoffe, Working Group NA 002-00-02-03 AK Gelpermeationschromatographie. The DIN Standards corresponding to the International Standards referred to in this document are as follows

8、: ISO 472 DIN EN ISO 472 ISO 5725-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabulary DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2

9、, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16014-5 July 2012 ICS 83.080.01 English Version Plastics -

10、Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography - Part 5: Method using light-scattering detection (ISO 16014-5:2012) Plastiques - Dtermination de la masse molculaire moyenne et de la distribution des masses molculaires de polymr

11、es par chromatographie dexclusion strique - Partie 5: Mthode utilisant la dtection par diffusion lumineuse (ISO 16014-5:2012) Kunststoffe - Bestimmung der durchschnittlichen Molmasse und der Molmassenverteilung von Polymeren mittels Gelpermeationschromatographie - Teil 5: Lichtstreudetektionsverfahr

12、en (ISO 16014-5:2012) This European Standard was approved by CEN on 30 June 2012. CEN 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

13、bibliographical references concerning such national standards may be obtained on application 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 re

14、sponsibility of a CEN member into its own language and notified to the CEN-CENELEC Management 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

15、Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE N

16、ORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 16014-5:2012: EContents PageForeword .1 Scope 2 Normative references .3 Terms

17、 and definitions .4 Symbols .5 Principle .5.1 SEC 5.2 Light-scattering SEC 6 Reagents 6.1 Eluent 6.2 Reagent for column evaluation .6.3 Calibration standards .6.4 Reagent for flow rate marker 6.5 Additives 7 Apparatus 7.1 General .7.2 Eluent reservoir .7.3 Pumping system 7.4 Injector .7.5 Columns .7

18、.6 Detector 7.7 Tubing .7.8 Temperature control .7.9 Recorder and plotter .7.10 Data-processing system 7.11 Other components 8 Procedure 8.1 Preparation of calibration solutions .8.2 Preparation of a solution for determining the L-point .8.3 Preparation of sample solutions .8.4 Preparation of soluti

19、ons for column performance evaluation 8.5 Setting up the apparatus 8.6 Operating parameters .8.7 Number of determinations .9 Calibration 9.1 Calibration of concentration-sensitive detector and light-scattering detector .9.2 Determination of delay volume 9.3 Normalization of detector sensitivity .9.4

20、 Determination of refractive index increment .10 Data acquisition and processing 10.1 Data acquisition .10.2 Evaluation of data and correction of chromatograms 10.3 Data processing .11 Expression of results .1411.1 Calibration curve .1411.2 Calculation of average molecular mass 1611.3 Differential m

21、olecular mass distribution curve .1611.4 Cumulative molecular mass distribution curve 1612 Precision 1713 Test report .17DIN EN ISO 16014-5:2012-10 EN ISO 16014-5:2012 (E) 24555666666777777888899999999991010101010101212121212121313.1 General .1713.2 Apparatus and measurement parameters 1713.3 Calibr

22、ation of the system 1713.4 Calibration curve .1813.5 Results .18Annex A (informative) Round-robin test .19Annex B (informative) Information on light scattering .Annex C (informative) Calibration curve in low molecular mass range 25Bibliography .27DIN EN ISO 16014-5:2012-10 EN ISO 16014-5:2012 (E) 32

23、1Foreword This document (EN ISO 16014-5:2012) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, ei

24、ther by publication of an identical text or by endorsement, at the latest by January 2013, and conflicting national standards shall be withdrawn at the latest by January 2013. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN an

25、d/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 organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Cze

26、ch Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, 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 Kingdo

27、m. Endorsement notice The text of ISO 16014-5:2012 has been approved by CEN as a EN ISO 16014-5:2012 without any modification. DIN EN ISO 16014-5:2012-10 EN ISO 16014-5:2012 (E) 41 ScopeThis part of ISO 16014 specifies a general method for determining the average molecular mass and the molecular mas

28、s distribution of polymers using SEC-LS, i.e. size-exclusion chromatography coupled with light-scattering detection. The average molecular mass and the molecular mass distribution are calculated from molecular mass data and mass concentrations determined continuously with elution time. The molecular

29、 mass at each elution time is determined absolutely by combining a light-scattering detector with a concentration-sensitive detector. Therefore, SEC-LS is classified as an absolute method.For the applicability of the method, see ISO 16014-1:2012, Clause A.1.2 Normative referencesThe following refere

30、nced 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 472, Plastics VocabularyISO 16014-1:2012, Plastics Determination o

31、f average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 1: General principlesISO 16014-2, Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 2: Universal calibrati

32、on methodISO 16014-3:2012, Plastics Determination of average molecular mass and molecular mass distribution of polymers using size-exclusion chromatography Part 3: Low-temperature methodISO 16014-4:2012, Plastics Determination of average molecular mass and molecular mass distribution of polymers usi

33、ng size-exclusion chromatography Part 4: High-temperature method3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and ISO 16014-1 and the following apply.3.1light-scattering detectionLS detectiona technique for determining the mass or size of polyme

34、r molecules in solution by measuring the light scattered by the polymer moleculesDIN EN ISO 16014-5:2012-10 EN ISO 16014-5:2012 (E) 5 3.2refractive index incrementdn/dcrate of change of the refractive index n of a polymer solution as a function of the mass concentration cNOTE 1 It is also called the

35、 “specific refractive index increment” in the literature.NOTE 2 The limiting value of dn/dc at zero concentration is commonly used in light scattering.3.3L-pointmeasured data point of a low molecular mass compound on the graph of molecular mass vs. elution time used for justification of the polynomi

36、nal fit of the calibration curve and/or construction of the calibration curve.NOTE In the lower molecular mass region, the LS signal is too low to calculate molecular mass. Therefore the measurement of the L-point is needed for justification or construction of the molecular mass calibration curve fo

37、r the whole range of molecular mass. The L-point is determined by measuring an oligomer of the polymer or an organic compound with a similar chemical structure to the oligomer.4 SymbolsRgradius of gyration of a polymer molecule in solution nmA2second virial coefficient for a polymer molecule in solu

38、tion cm3molg2c mass concentration of polymer in solution gcm3dn/dc refractive index increment cmg1Hiexcess signal intensity of a concentration detector at the ith elution time ILS,iexcess signal intensity of scattered light at the ith elution time Vevolume eluted during data acquisition time (interv

39、al) cm35 Principle5.1 SECFor a discussion of size-exclusion chromatography in general, see ISO 16014-1:2012, Clause 4.5.2 Light-scattering SECIn SEC-LS, polymer molecules eluted from the SEC columns are irradiated by a beam of monochromatic visible light. The light scattered by the molecules is cont

40、inuously detected by a light-scattering detector. Since the eluate is a dilute polymer solution, the intensity of the scattered light is approximately proportional to the product of the molecular mass and the mass concentration of the polymer molecules. The scattered-light intensity divided by the c

41、oncentration therefore gives the molecular mass at a particular elution time. The values of the molecular mass and the mass concentration or mass fraction at each elution time are used to calculate the molecular mass distribution and the average molecular mass of the polymer.6 Reagents6.1 EluentFor

42、a general discussion of eluents, see ISO 16014-1:2012, 5.1.For examples of eluents used for SEC measurements at temperatures below and above 60 C, see Annex B of ISO 16014-3:2012 and Annex B of ISO 16014-4:2012, respectively.DIN EN ISO 16014-5:2012-10 EN ISO 16014-5:2012 (E) 66.2 Reagent for column

43、evaluationFor examples of low molecular mass compounds used for column evaluation, see ISO 16014-3:2012, 5.2, for measurements at temperatures below 60 C and ISO 16014-4:2012, 5.2, for those above 60 C.6.3 Calibration standardsSince the Rayleigh ratios of toluene and benzene are well-known, these so

44、lvents are recommended for determining the calibration constant of the light-scattering detector (see Annex B, Clause B.2).Aqueous solutions of potassium chloride (KCl) or sodium chloride (NaCl) are used for determining the calibration constant of a refractive index detector. The concentration depen

45、dence of the differential refractive index of the solutions is used to calculate the constant.A low molecular mass, monodisperse polymer is used to determine the delay volume between the light-scattering and concentration-sensitive detectors. This polymer may also be used to calibrate the angular de

46、pendence of the detector sensitivity of a multiple-angle light-scattering detector. The radius of gyration Rgof the polymer molecule used to calibrate the detector sensitivity, should preferably be less than 10 nm. A radius of gyration less than 5 nm is desirable. Other compounds with a well-known R

47、gvalue may also be used.Polymer reference materials are used for molecular mass calibration ranges from 20 000 to 50 000.Low molecular mass organic compounds or oligomers of the polymer in the sample under investigation are used for determining the “L-point”.6.4 Reagent for flow rate markerSee ISO 1

48、6014-1:2012, 5.4.For examples of compounds suitable for use as a flow rate marker, see ISO 16014-3:2012, 5.4, for measurements at temperatures below 60 C and ISO 16014-4:2012, 5.4, for those above 60 C.6.5 AdditivesSee ISO 16014-1:2012, 5.5.Some examples of additives are given in ISO 16014-3:2012, 5.5, for measurements below 60 C and ISO 16014-4:2012, 5.5, for those above 60 C.7 Apparatus7.1 GeneralA typical schematic diagr