ASTM D4275-09
(Test Method)Standard Test Method for Determination of Butylated Hydroxy Toluene (BHT) in Polymers of Ethylene and Ethylene–Vinyl Acetate (EVA) Copolymers By Gas Chromatography
Standard Test Method for Determination of Butylated Hydroxy Toluene (BHT) in Polymers of Ethylene and Ethylene<span class='unicode'>–</span>Vinyl Acetate (EVA) Copolymers By Gas Chromatography
SIGNIFICANCE AND USE
Separation and identification of stabilizers used in the manufacture of polyethylene are necessary in order to correlate performance properties with polymer composition.
The BHT extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for gas chromatographic analysis.
SCOPE
1.1 This test method describes a procedure for the determination of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-4-methyl-hydroxybenzene) in polymers of ethylene and ethylene-vinyl acetate (EVA) copolymers by solvent extraction followed by gas chromatographic analysis. Detection of the compound is achieved by flame ionization, and quantitative analysis is obtained by use of internal or external standards, as described in Practices E 260, E 355, and E 594.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 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 for this test method.
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Designation: D4275 − 09
Standard Test Method for
Determination of Butylated Hydroxy Toluene (BHT) in
Polymers of Ethylene and Ethylene–Vinyl Acetate (EVA)
1
Copolymers By Gas Chromatography
This standard is issued under the fixed designation D4275; 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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This test method describes a procedure for the determi-
IEEE/ASTM SI-10 Practice for Use of the International
nation of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-
System of Units (SI) (the Modernized Metric System)
4-methyl-hydroxybenzene) in polymers of ethylene and
ethylene-vinyl acetate (EVA) copolymers by solvent extraction
3. Terminology
followed by gas chromatographic analysis. Detection of the
compound is achieved by flame ionization, and quantitative
3.1 Definitions—Units and symbols used in this test method
analysis is obtained by use of internal or external standards, as
are those recommended in Practice IEEE/ASTM SI-10. Chro-
described in Practices E260, E355, and E594.
matographic terms and relationships are as described in Prac-
tice E355.
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
3.2 Abbreviations:
only.
3.2.1 BHT—Butylated hydroxy toluene (2,6-di-tert-butyl-4-
1.3 This standard does not purport to address all of the
methyl-hydroxybenzene).
safety concerns, if any, associated with its use. It is the
3.2.2 MM—Methyl myristate.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.2.3 EVA—Ethylene-vinyl acetate copolymers.
bility of regulatory limitations prior to use. Specific precau-
3.2.4 LDPE—Low-density polyethylene.
tionary statements are given in Section 9.
3.2.5 HDPE—High-density polyethylene.
NOTE 1—There is no known ISO equivalent for this test method.
4. Summary of Test Method
2. Referenced Documents
2
2.1 ASTM Standards: 4.1 The BHT from a finely ground polymer sample is
D4968 Guide for Annual Review of Test Methods and extracted by shaking or refluxing with cyclohexane or isopro-
Specifications for Plastics panol. A known volume of this extract is injected into a gas
D7210 Practice for Extraction of Additives in Polyolefin chromatographic column packed with a liquid-coated solid
Plastics support. Passing through this column in a stream of carrier gas,
E260 Practice for Packed Column Gas Chromatography BHT is separated from the extraction solvent and other
E355 Practice for Gas ChromatographyTerms and Relation- components. Responses of BHT and any internal standard are
ships measured by a flame ionization detector. This signal is re-
corded to indicate the relative concentration and retention time
E594 Practice for Testing Flame Ionization Detectors Used
in Gas or Supercritical Fluid Chromatography of BHT.
5. Significance and Use
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods. 5.1 Separation and identification of stabilizers used in the
Current edition approved Aug. 1, 2009. Published August 2009. Originally
manufacture of polyethylene are necessary in order to correlate
approved in 1983. Last previous edition approved in 2002 as D4275 - 02. DOI:
performance properties with polymer composition.
10.1520/D4275-09.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.2 The BHT extraction procedure is made effective by the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
insolubility of the polymer sample in solvents generally used
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. for gas chromatographic analysis.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
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D4275 − 09
6. Interferences not connect the exit end of the column to the detector during
this conditioning period.Turn off hydrogen and air flows to the
6.1 Any material eluting at or near the BHT or MM
detector while the column is disconnected.
retentiontimeswillcauseerroneousresults.Priortoextraction,
solvent blanks shall be analyzed to confirm the absence of 10.2 Connect the exit end of the column to the detector. Set
interfering peaks. optimum hydrogen and air flow rates for the detector as
specified for the chromatograph model in use, or as deter
...
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:D4275–02 Designation:D4275–09
Standard Test Method for
Determination of Butylated Hydroxy Toluene (BHT) in
Polymers of Ethylene and Ethylene–Vinyl Acetate (EVA)
1
Copolymers By Gas Chromatography
This standard is issued under the fixed designation D 4275; 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 describes a procedure for the determination of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-4-
methyl-hydroxybenzene) in polymers of ethylene and ethylene-vinyl acetate (EVA) copolymers by solvent extraction followed
by gas chromatographic analysis. Detection of the compound is achieved by flame ionization, and quantitative analysis is obtained
by use of internal or external standards, as described in Practices E 260, E 355, and E 594.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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 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 for this test method.
2. Referenced Documents
2
2.1 ASTM Standards:
D 4968 Guide for Annual Review of Test Methods and Specifications for Plastics Guide for Annual Review of Test Methods
and Specifications for Plastics
D 7210 Practice for Extraction of Additives in Polyolefin Plastics
E 260 Practice for Packed Column Gas Chromatography
E 355 Practice for Gas Chromatography Terms and Relationships
E380Practice for Use of the International System of Units (SI) (the Modernized Metric System) Practice for Gas
Chromatography Terms and Relationships
E 594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3
E 691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method Practice for Conducting
an Interlaboratory Study to Determine the Precision of a Test Method
IEEE/ASTM SI-10 Practice for Use of the International System of Units (SI) (the Modernized Metric System)
3. Terminology
3.1 Definitions—Units and symbols used in this test method are those recommended in Practice E380IEEE/ASTM SI-10.
Chromatographic terms and relationships are as described in Practice E 355.
3.2 Abbreviations:Abbreviations:
3.2.1 BHT—Butylated hydroxy toluene (2,6-di-tert-butyl-4-methyl-hydroxybenzene).
3.2.2 MM—Methyl myristate.
3.2.3 EVA—Ethylene-vinyl acetate copolymers.
3.2.4 LDPE—Low-density polyethylene.
3.2.5 HDPE—High-density polyethylene.
4. Summary of Test Method
4.1 The BHT from a finely ground polymer sample is extracted by shaking or refluxing with cyclohexane or isopropanol that
may contain an internal standard.isopropanol. A known volume of this extract is injected into a gas 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 Aug. 10, 2002. Published October 2002. Originally published as D4275–83. Last previous edition D4275–96.
Current edition approved Aug. 1, 2009. Published August 2009. Originally approved in 1983. Last previous edition approved in 2002 as D 4275 - 02.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 08.03.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
D4275–09
packed with a liquid-coated solid support. Passing through this column in a stream of carrier gas, BHT is separated from the
extractionsolventandothercomponents.ResponsesofBHTandanyinternalstandardaremeasuredbyaflameionizationdetector.
This signal is recorded to indicate the relative concentration and retention time of BHT.
5. Significance and Use
5.1 Separation and identification of stabilizers us
...
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