ISO 16014-5:2019
Plastics — Determination of average molecular weight and molecular weight distribution of polymers using size-exclusion chromatography — Part 5: Light-scattering method
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.
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Symbols
5 Principle
5.1 SEC
5.2 Light-scattering SEC
6 Reagents
7 Apparatus
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
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
9.1.3 Calibration method B
9.1.4 Calibration method C
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
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
11.1.2 Method A
11.1.3 Method B
11.2 Calculation of average molecular weight
11.3 Differential molecular weight distribution curve
11.4 Cumulative molecular weight distribution curve
12 Precision
13 Test report
13.1 General
13.2 Apparatus and measurement parameters
13.3 Calibration of the system
13.4 Calibration curve
13.5 Results
Annex A (informative) Interlaboratory test
Annex B (informative) Information on light scattering
Annex C (informative) Calibration curve in low molecular weight range
Bibliography
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Foreword
1 Scope
2 Normative references
3 Terms and definitions
4 Symbols
5 Principle
5.1 SEC
5.2 Light-scattering SEC
6 Reagents
7 Apparatus
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
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
9.1.3 Calibration method B
9.1.4 Calibration method C
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
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
11.1.2 Method A
11.1.3 Method B
11.2 Calculation of average molecular weight
11.3 Differential molecular weight distribution curve
11.4 Cumulative molecular weight distribution curve
12 Precision
13 Test report
13.1 General
13.2 Apparatus and measurement parameters
13.3 Calibration of the system
13.4 Calibration curve
13.5 Results
Annex A (informative) Interlaboratory test
Annex B (informative) Information on light scattering
Annex C (informative) Calibration curve in low molecular weight range
Bibliography