Standard Test Method for Molecular Weight Averages and Molecular Weight Distribution of Polystyrene by High Performance Size-Exclusion Chromatography

SIGNIFICANCE AND USE
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.
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). 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 and health 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.

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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5296 − 11
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* 2. Referenced Documents
3
1.1 This test method covers the determination of molecular 2.1 ASTM Standards:
weight (MW) averages and the distribution of molecular D883Terminology Relating to Plastics
weights for linear, soluble polystyrene by high-performance D2857Practice for Dilute Solution Viscosity of Polymers
size-exclusion chromatography (HPSEC). This test method is D3016Practice for Use of Liquid Exclusion Chromatogra-
not absolute and requires the use of commercially available phy Terms and Relationships
narrow molecular weight distribution (MWD) polystyrene E685Practice for Testing Fixed-Wavelength Photometric
standards for calibration. This test method is applicable for Detectors Used in Liquid Chromatography
samples containing molecular weight components that have E691Practice for Conducting an Interlaboratory Study to
elution volumes falling within the elution volume range Determine the Precision of a Test Method
defined by polystyrene standards (that is, molecular weights
−1
3. Terminology
generally from 2000 to 2000000 g·mol ).
3.1 Definitions—For definitions of technical terms pertain-
1.2 The HPSEC is differentiated from traditional size-
ing to plastics used in this test method see Terminology D883.
exclusion chromatography SEC (also referred to as gel perme-
ation chromatography (GPC)) in that the number of theoretical
4. Summary of Test Method
plates per metre with an HPSEC system is at least ten times
4.1 In this test method a dilute solution of a polystyrene
greater than that for traditional SEC (see Terminology D883
2
sample is injected into a liquid mobile phase containing the
and Practice D3016). The HPSEC systems employ low-
samesolventusedtopreparethepolymersolution.Themobile
volume liquid chromatography components and columns
phase transports the polymer into and through a chromato-
packed with relatively small (generally 3 to 20 µm) micropo-
graphic column (or set of columns connected in series) packed
rous particles. High-performance liquid chromatography in-
with a solid or semirigid, porous substrate which separates the
strumentation and automated data handling systems for data
polymer molecules according to their size in solution. Starting
acquisition and processing are required.
frominjection,adetectorcontinuouslymonitorstheeluateasa
1.3 The values stated in SI units are to be regarded as the
function of elution volume (or time). Upon emerging from the
standard.
column(s), the size-separated molecules are detected and
1.4 This standard does not purport to address all of the
recordedaccordingtotheirconcentration.Throughcalibration,
safety concerns, if any, associated with its use. It is the
the elution volumes (or times) are converted to molecular
responsibility of the user of this standard to establish appro-
weights, and various molecular weight parameters for the
priate safety and health practices and determine the applica-
samplearecalculatedfromthemolecularweight/concentration
bility of regulatory limitations prior to use. Specific precau-
data.
tionary statements are given in Section 9.
5. Significance and Use
NOTE 1—There is no known ISO equivalent to this standard.
5.1 General Utility—The molecular weight (MW) and mo-
lecular weight distribution (MWD) are fundamental character-
1 istics of a polymer sample.They are used for a wide variety of
ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Sept. 1, 2011. Published September 2011. Originally
3
approved in 1992. Last previous edition approved in 2005 as D5296-05. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D5296-11. 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
and40-S3onSizeExclusionChromatography, availablefromASTMHeadquarters. 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 − 11
co
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:D5296–05 Designation:D5296–11
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*
1.1 This test method covers the determination of molecular weight (MW) averages and the distribution of molecular weights
for linear, soluble polystyrene by liquid 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 2000000
−1
g·mol ).
1.2 The HPSEC is differentiated from traditional size-exclusion chromatography SEC (also referred to as gel permeation
chromatography(GPC))inthatthenumberoftheoreticalplatespermetrewithanHPSECsystemisaboutatleasttentimesgreater
2
than 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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 9.
NOTE1—There is no similar or equivalent ISO standard. 1—There is no known ISO equivalent to this standard.
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
solventusedtopreparethepolymersolution.Themobilephasetransportsthepolymerintoandthroughachromatographiccolumn
(or set of columns connected in series) packed with a solid or semirigid, porous substrate which separates the polymer molecules
according to their size in solution. Starting from injection, a detector continuously monitors the eluate as a function of elution
volume (or time). Upon emerging from the column(s), the size-separated molecules are detected and recorded according to their
concentration. Through calibration, the elution volumes (or times) are converted to molecular weights, and various molecular
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 MarchSept. 1, 2005.2011. Published March 2005.September 2011. Originally approved in 1992. Last previous edition approved in 19972005 as
D5296-97.D5296-05. DOI: 10.1520/D5296-05.10.1520/D5296-11.
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
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@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 1942
...

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