ASTM D5296-19
(Test Method)Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography
Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography
SIGNIFICANCE AND USE
5.1 General Utility—The molecular weight (MW) and molecular weight distribution (MWD) are fundamental characteristics of a polymer sample. They are used for a wide variety of correlations for fundamental studies, processing, or product applications. For example, the observed MWD is compared to one predicted from assumed kinetics or mechanisms for a polymerization reaction. Differences between the values will allow alteration of theory or experimental design. Similarly, the strength, melt flow, and other properties of a polymer sample usually are dependent on MW and MWD. Determinations of MW and MWD are used for quality control of polymers.
5.2 Limitations—Because of the need for specific calibration of the polymer type under study, and because of the specific nature of polymer/solvent/column-packing interactions, this test method is valid only for polystyrene and non-exclusion effects are to be avoided. However, many of the principles of the method have been applied in generating HPSEC methods for other polymer systems, for example, using the principles of universal calibration. (see Practice D3016).
SCOPE
1.1 This test method covers the determination of molecular weight (MW) averages and the distribution of molecular weights for linear, soluble polystyrene by high-performance size-exclusion chromatography (HPSEC). This test method is not absolute and requires the use of commercially available narrow molecular weight distribution (MWD) polystyrene standards for calibration. This test method is applicable for samples containing molecular weight components that have elution volumes falling within the elution volume range defined by polystyrene standards (that is, molecular weights generally from 2000 to 2 000 000 g·mol−1).
1.2 The HPSEC is differentiated from traditional size-exclusion chromatography SEC (also referred to as gel permeation chromatography (GPC)) in that the number of theoretical plates per metre with an HPSEC system is at least ten times greater than that for traditional SEC (see Terminology D883 and Practice D3016).2 The HPSEC systems employ low-volume liquid chromatography components and columns packed with relatively small (generally 3 to 20 μm) microporous particles. High-performance liquid chromatography instrumentation and automated data handling systems for data acquisition and processing are required.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.
Note 1: There is no known ISO equivalent to this standard.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Buy Standard
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D5296 − 19
Standard Test Method for
Molecular Weight Averages and Molecular Weight
Distribution of Polystyrene by High Performance Size-
1
Exclusion Chromatography
This standard is issued under the fixed designation D5296; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope* 1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the determination of molecular
ization established in the Decision on Principles for the
weight (MW) averages and the distribution of molecular
Development of International Standards, Guides and Recom-
weights for linear, soluble polystyrene by high-performance
mendations issued by the World Trade Organization Technical
size-exclusion chromatography (HPSEC). This test method is
Barriers to Trade (TBT) Committee.
not absolute and requires the use of commercially available
narrow molecular weight distribution (MWD) polystyrene
2. Referenced Documents
standards for calibration. This test method is applicable for
3
samples containing molecular weight components that have 2.1 ASTM Standards:
elution volumes falling within the elution volume range D883Terminology Relating to Plastics
D2857Practice for Dilute Solution Viscosity of Polymers
defined by polystyrene standards (that is, molecular weights
−1
generally from 2000 to 2000000 g·mol ). D3016Practice for Use of Liquid Exclusion Chromatogra-
phy Terms and Relationships
1.2 The HPSEC is differentiated from traditional size-
E685Practice for Testing Fixed-Wavelength Photometric
exclusion chromatography SEC (also referred to as gel perme-
Detectors Used in Liquid Chromatography
ation chromatography (GPC)) in that the number of theoretical
E691Practice for Conducting an Interlaboratory Study to
plates per metre with an HPSEC system is at least ten times
Determine the Precision of a Test Method
greater than that for traditional SEC (see Terminology D883
2
and Practice D3016). The HPSEC systems employ low-
3. Terminology
volume liquid chromatography components and columns
packed with relatively small (generally 3 to 20 µm) micropo- 3.1 Definitions—For definitions of technical terms pertain-
rous particles. High-performance liquid chromatography in- ing to plastics used in this test method see Terminology D883.
strumentation and automated data handling systems for data
acquisition and processing are required. 4. Summary of Test Method
4.1 In this test method a dilute solution of a polystyrene
1.3 The values stated in SI units are to be regarded as the
standard. sample is injected into a liquid mobile phase containing the
samesolventusedtopreparethepolymersolution.Themobile
1.4 This standard does not purport to address all of the
phase transports the polymer into and through a chromato-
safety concerns, if any, associated with its use. It is the
graphic column (or set of columns connected in series) packed
responsibility of the user of this standard to establish appro-
with a solid or semirigid, porous substrate which separates the
priate safety, health, and environmental practices and deter-
polymer molecules according to their size in solution. Starting
mine the applicability of regulatory limitations prior to use.
frominjection,adetectorcontinuouslymonitorstheeluateasa
Specific precautionary statements are given in Section 9.
function of elution volume (or time). Upon emerging from the
NOTE 1—There is no known ISO equivalent to this standard.
column(s), the size-separated molecules are detected and
recordedaccordingtotheirconcentration.Throughcalibration,
the elution volumes (or times) are converted to molecular
1
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Nov. 1, 2019. Published December 2019. Originally
3
approved in 1992. Last previous edition approved in 2011 as D5296–11. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D5296-19. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2
Seealso AMD Bibliography and Bibliography SupplementsAMD 40-S1, 40-S2, Standards volume information, refer to the standard’s Document Summary page on
and 40-S3 on Size Exclusion Chromatography, availablefromASTMHeadquarters. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyri
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5296 − 11 D5296 − 19
Standard Test Method for
Molecular Weight Averages and Molecular Weight
Distribution of Polystyrene by High Performance Size-
1
Exclusion Chromatography
This standard is issued under the fixed designation D5296; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the determination of molecular weight (MW) averages and the distribution of molecular weights
for linear, soluble polystyrene by high-performance size-exclusion chromatography (HPSEC). This test method is not absolute and
requires the use of commercially available narrow molecular weight distribution (MWD) polystyrene standards for calibration.
This test method is applicable for samples containing molecular weight components that have elution volumes falling within the
−1
elution volume range defined by polystyrene standards (that is, molecular weights generally from 2000 to 2 000 000 g·mol ).
1.2 The HPSEC is differentiated from traditional size-exclusion chromatography SEC (also referred to as gel permeation
chromatography (GPC)) in that the number of theoretical plates per metre with an HPSEC system is at least ten times greater than
2
that for traditional SEC (see Terminology D883 and Practice D3016). The HPSEC systems employ low-volume liquid
chromatography components and columns packed with relatively small (generally 3 to 20 μm) microporous particles.
High-performance liquid chromatography instrumentation and automated data handling systems for data acquisition and
processing are required.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.
NOTE 1—There is no known ISO equivalent to this standard.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
3
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D2857 Practice for Dilute Solution Viscosity of Polymers
D3016 Practice for Use of Liquid Exclusion Chromatography Terms and Relationships
E685 Practice for Testing Fixed-Wavelength Photometric Detectors Used in Liquid Chromatography
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
3. Terminology
3.1 Definitions—For definitions of technical terms pertaining to plastics used in this test method see Terminology D883.
4. Summary of Test Method
4.1 In this test method a dilute solution of a polystyrene sample is injected into a liquid mobile phase containing the same
solvent used to prepare the polymer solution. The mobile phase transports the polymer into and through a chromatographic column
1
This test method is under the jurisdiction of ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Sept. 1, 2011Nov. 1, 2019. Published September 2011December 2019. Originally approved in 1992. Last previous edition approved in 20052011
as D5296 - 05.D5296 – 11. DOI: 10.1520/D5296-11.10.1520/D5296-19.
2
See also AMD Bibliography and Bibliography Supplements AMD 40-S1, 40-S2, and 40-S3 on Size Exclusion Chromatography, available from ASTM Headquarters.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D5296 − 19
(or set of columns connected in series) packed with a solid or se
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.