ASTM D6953-18
(Test Method)Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatography (LC)
Standard Test Method for Determination of Antioxidants and Erucamide Slip Additives in Polyethylene Using Liquid Chromatography (LC)
SIGNIFICANCE AND USE
5.1 Separation and identification of stabilizers used in the manufacture of polyethylene resins are necessary in order to correlate performance properties with polymer composition. This test method provides a means to determine the polymer additives listed in Table 1 in polyethylene samples. This test method is capable of the determination of other antioxidants, but the stability of these during extraction has not been investigated.
5.2 The additive extraction procedure is made effective by the relatively low solubility of the polymer sample in solvents generally used for liquid chromatographic analysis. In this method, isopropanol and cyclohexane were chosen because of their excellent extraction efficiencies as well as for safety reasons. Other solvents including ethylacetate, isobutanol, chloroform and methylene chloride can also be used.
5.3 Methods other than refluxing that have been used to remove additives from the polymer matrix including pressurized liquid, microwave, ultrasonic, and supercritical fluid extractions. For the separation of the extracted additives, SFC and GC have been used successfully for several of the additives.
5.4 Under optimum conditions, the lowest level of detection for an antioxidant is approximately 2 ppm.
SCOPE
1.1 This test method covers a liquid-chromatographic procedure for the separation of primary and secondary antioxidant and slip additives currently used in polyethylene plastics. These additives are extracted with either isopropanol (resin densities 3) or cyclohexane (resin densities > 0.94 g/cm3) prior to liquid-chromatographic separation. The ultraviolet absorbance of the eluting compound(s) is measured and quantitation is performed using external calibration.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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
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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:D6953 −18
Standard Test Method for
Determination of Antioxidants and Erucamide Slip Additives
1
in Polyethylene Using Liquid Chromatography (LC)
This standard is issued under the fixed designation D6953; 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.
3
1. Scope* Laboratory (Withdrawn 2009)
E131 Terminology Relating to Molecular Spectroscopy
1.1 This test method covers a liquid-chromatographic pro-
E169 PracticesforGeneralTechniquesofUltraviolet-Visible
cedure for the separation of primary and secondary antioxidant
Quantitative Analysis
and slip additives currently used in polyethylene plastics.
E275 Practice for Describing and Measuring Performance of
These additives are extracted with either isopropanol (resin
3 Ultraviolet and Visible Spectrophotometers
densities < 0.94 g/cm ) or cyclohexane (resin densities > 0.94
3 E691 Practice for Conducting an Interlaboratory Study to
g/cm ) prior to liquid-chromatographic separation. The ultra-
Determine the Precision of a Test Method
violet absorbance of the eluting compound(s) is measured and
E1657 Practice for Testing Variable-Wavelength Photomet-
quantitation is performed using external calibration.
ric Detectors Used in Liquid Chromatography
1.2 The values stated in SI units are to be regarded as
IEEE/ASTM SI 10 Standard for Use of the International
standard. No other units of measurement are included in this
System of Units (SI): The Modern Metric System
standard.
3. Terminology
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3.1 Definitions:
responsibility of the user of this standard to establish appro-
3.1.1 For definitions of plastic terms and detector terminol-
priate safety, health, and environmental practices and deter-
ogy used in this test method, see Terminologies D883, D1600,
mine the applicability of regulatory limitations prior to use.
and E1657.
Specific precautionary statements are given in Section 9.
3.1.2 Forunitsandsymbolsusedinthistestmethod,referto
Terminology E131 or IEEE/ASTM SI 10.
NOTE 1—There is no known ISO equivalent to this standard.
1.4 This international standard was developed in accor-
4. Summary of Test Method
dance with internationally recognized principles on standard-
4.1 The polyethylene sample is ground to a 1-mm (~20
ization established in the Decision on Principles for the
mesh) or 0.5-mm (~40 mesh) particle size and extracted by
Development of International Standards, Guides and Recom-
refluxing with either isopropanol or cyclohexane.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
4.2 The solvent extract is analyzed by liquid chromatogra-
phy.
2. Referenced Documents
4.3 Additive concentrations are determined from external
2
2.1 ASTM Standards:
calibration curves using reverse phase chromatography (C-8 or
D883 Terminology Relating to Plastics
C-18 column) with ultraviolet (UV) detection at wavelengths
D1600 Terminology forAbbreviatedTerms Relating to Plas-
corresponding to the wavelengths of an absorption apex of
tics
each additive (except erucamide which does not have an
D4697 Guide for Maintaining Test Methods in the User’s
absorption maximum in the accessible UV region).
5. Significance and Use
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
5.1 Separation and identification of stabilizers used in the
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Nov. 1, 2018. Published November 2018. Originally
manufacture of polyethylene resins are necessary in order to
approved in 2003. Last previous edition approved in 2011 as D6953 - 11.
correlate performance properties with polymer composition.
DOI:10.1520/D6953-18.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
*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
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D6953−18
TABLE 1 Common Polyolefin Additives
Chemical Name Chemical Classificatio
...
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: D6953 − 11 D6953 − 18
Standard Test Method for
Determination of Antioxidants and Erucamide Slip Additives
1
in Polyethylene Using Liquid Chromatography (LC)
This standard is issued under the fixed designation D6953; 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 a liquid-chromatographic procedure for the separation of primary and secondary antioxidant and
slip additives currently used in polyethylene plastics. These additives are extracted with either isopropanol (resin densities < 0.94
3 3
g/cm ) or cyclohexane (resin densities > 0.94 g/cm ) prior to liquid-chromatographic separation. The ultraviolet absorbance of the
eluting compound(s) is measured and quantitation is performed using external calibration.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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.
1.4 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
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D1600 Terminology for Abbreviated Terms Relating to Plastics
3
D4697 Guide for Maintaining Test Methods in the User’s Laboratory (Withdrawn 2009)
E131 Terminology Relating to Molecular Spectroscopy
E169 Practices for General Techniques of Ultraviolet-Visible Quantitative Analysis
E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1657 Practice for Testing Variable-Wavelength Photometric Detectors Used in Liquid Chromatography
IEEE/ASTM SI 10 Standard for Use of the International System of Units (SI): The Modern Metric System
3. Terminology
3.1 Definitions:
3.1.1 For definitions of plastic terms and detector terminology used in this test method, see Terminologies D883, D1600, and
E1657.
3.1.2 For units and symbols used in this test method, refer to Terminology E131 or IEEE/ASTM SI 10.
4. Summary of Test Method
4.1 The polyethylene sample is ground to a 1-mm (~20 mesh) or 0.5-mm (~40 mesh) particle size and extracted by refluxing
with either isopropanol or cyclohexane.
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, 2018. Published September 2011November 2018. Originally approved in 2003. Last previous edition approved in 20032011
as D6953 - 03.D6953 - 11. DOI:10.1520/D6953-11.DOI:10.1520/D6953-18.
2
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.
3
The last approved version of this historical standard is referenced on www.astm.org.
*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 ----------------------
D6953 − 18
TABLE 1 Common Polyolefin Additives
Chemical Name Chemical Classification CAS Number
Formula
BHEB, 2,6-di-t-butyl-4-ethylphenol or butylated hydroxyethyl C H O 1º Antioxidant 4130-42-1
16 26
benzene
BHT, 2,6-di-t-butylcresol or butylated hydroxy toluene C H O 1º Antioxidant 128-37-0
15 24
Tris (2,4-di-t-butylphenyl)-phosphite C H O P 2º Antioxidant 31570-04-4
42 63 3
Tris(2,4-di-t-butylphenyl)-phosphate C H O P Degradation product 78-33-1
30 39 4
Tetrakis[methylene
...
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