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BS EN ISO 16014-5:2019

$142.49

Plastics. Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography – Light-scattering method

Published By Publication Date Number of Pages
BSI 2019 34
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This document specifies a general method for determining the average molecular weight and the molecular weight distribution of polymers using SEC-LS, i.e. size-exclusion chromatography coupled with light-scattering detection. The average molecular weight and the molecular weight distribution are calculated from molecular weight data and weight concentrations determined continuously with elution time. The molecular weight 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.

This method is applicable to linear homopolymers and to nonlinear homopolymers such as branched, star-shaped, comb-like, stereo-regular and stereo-irregular polymers. It can also be applied to heterophasic copolymers whose molecular composition cannot vary. However, SEC-LS is not applicable to block, graft or heterophasic copolymers whose molecular composition can vary. And the methods are applicable to molecular weights ranging from that of the monomer to 3 000 000, but are not intended for samples that contain > 30 % of components having a molecular weight < 1 000.

This document specifies a general method for determining the average molecular weight and the molecular weight distribution of polymers using SEC-LS, i.e. size-exclusion chromatography coupled with light-scattering detection. The average molecular weight and the molecular weight distribution are calculated from molecular weight data and weight concentrations determined continuously with elution time. The molecular weight 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.

This method is applicable to linear homopolymers and to nonlinear homopolymers such as branched, star-shaped, comb-like, stereo-regular and stereo-irregular polymers. It can also be applied to heterophasic copolymers whose molecular composition cannot vary. However, SEC-LS is not applicable to block, graft or heterophasic copolymers whose molecular composition can vary. And the methods are applicable to molecular weights ranging from that of the monomer to 3 000 000, but are not intended for samples that contain > 30 % of components having a molecular weight < 1 000.

PDF Catalog

PDF Pages PDF Title
2 National foreword
4 European foreword
7 Foreword
9 1 Scope
2 Normative references
3 Terms and definitions
10 4 Symbols
5 Principle
5.1 SEC
5.2 Light-scattering SEC
11 6 Reagents
6.1 Eluent.
6.2 Reagent for column evaluation
6.3 Calibration standards
7 Apparatus
7.1 General
12 7.5.1 General
13 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 solutions for column performance evaluation
8.5 Setting up the apparatus
8.6 Operating parameters
8.6.1 Flow rate
8.6.2 Injection masses and injection volumes
14 8.6.3 Column temperature
8.6.4 Detector sensitivity
8.7 Number of determinations
9 Calibration
9.1 Calibration of concentration-sensitive detector and light-scattering detector
9.1.1 General
9.1.2 Calibration method A
15 9.1.3 Calibration method B
9.1.4 Calibration method C
16 9.2 Determination of delay volume
9.3 Normalization of detector sensitivity
9.4 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
10.3.1 Baseline determination
17 10.3.2 Determination of calculation range
10.3.3 Calculation of signal intensity
10.3.4 Calculation of molecular weight
10.3.5 Second virial coefficient, A2
11 Expression of results
11.1 Calibration curve
11.1.1 General
18 11.1.2 Method A
11.1.3 Method B
20 11.2 Calculation of average molecular weight
11.3 Differential molecular weight distribution curve
11.4 Cumulative molecular weight distribution curve
21 12 Precision
13 Test report
13.1 General
13.2 Apparatus and measurement parameters
13.3 Calibration of the system
22 13.4 Calibration curve
13.5 Results
23 Annex A (informative) Interlaboratory test
25 Annex B (informative) Information on light scattering
29 Annex C (informative) Calibration curve in low molecular weight range
31 Bibliography
BS EN ISO 16014-5:2019
$142.49