ASTM D4275-17
(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–Vinyl Acetate (EVA) Copolymers by Gas Chromatography
SIGNIFICANCE AND USE
5.1 Separation and identification of stabilizers used in the manufacture of polyethylene are necessary in order to correlate performance properties with polymer composition.
5.2 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 E260, E355, and E594.
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.
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: D4275 − 17
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* in Gas or Supercritical Fluid Chromatography
E691 Practice for Conducting an Interlaboratory Study to
1.1 This test method describes a procedure for the determi-
Determine the Precision of a Test Method
nation of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-
IEEE/ASTM SI-10 Practice for Use of the International
4-methyl-hydroxybenzene) in polymers of ethylene and
System of Units (SI) (the Modernized Metric System)
ethylene-vinyl acetate (EVA) copolymers by solvent extraction
followed by gas chromatographic analysis. Detection of the
3. Terminology
compound is achieved by flame ionization, and quantitative
analysis is obtained by use of internal or external standards, as
3.1 Definitions—Units and symbols used in this test method
described in Practices E260, E355, and E594.
are those recommended in Practice IEEE/ASTM SI-10. Chro-
matographic terms and relationships are as described in Prac-
1.2 The values stated in SI units are to be regarded as the
tice E355.
standard. The values given in parentheses are for information
only.
3.2 Abbreviations:
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
responsibility of the user of this standard to establish appro-
3.2.2 MM—Methyl myristate.
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.
2. Referenced Documents
4. Summary of Test Method
2
2.1 ASTM Standards:
4.1 The BHT from a finely ground polymer sample is
D883 Terminology Relating to Plastics
extracted by shaking or refluxing with cyclohexane or isopro-
D4968 Practice for Annual Review of Test Methods and
panol. A known volume of this extract is injected into a gas
Specifications for Plastics
chromatographic column packed with a liquid-coated solid
D7210 Practice for Extraction of Additives in Polyolefin
support. Passing through this column in a stream of carrier gas,
Plastics
BHT is separated from the extraction solvent and other
E260 Practice for Packed Column Gas Chromatography
components. Responses of BHT and any internal standard are
E355 Practice for Gas ChromatographyTerms and Relation-
measured by a flame ionization detector. This signal is re-
ships
corded to indicate the relative concentration and retention time
E594 Practice for Testing Flame Ionization Detectors Used
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 March 1, 2017. Published March 2017. Originally
manufacture of polyethylene are necessary in order to correlate
approved in 1983. Last previous edition approved in 2009 as D4275 - 09. DOI:
performance properties with polymer composition.
10.1520/D4275-17.
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.
*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 ----------------------
D4275 − 17
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.Pri
...
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: D4275 − 09 D4275 − 17
Standard Test Method for
Determination of Butylated Hydroxy Toluene (BHT) in
Polymers of Ethylene and Ethylene–Vinyl Acetate (EVA)
1
Copolymers Byby 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 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 E260, E355, and E594.
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.
2. Referenced Documents
2
2.1 ASTM Standards:
D883 Terminology Relating to Plastics
D4968 Practice for Annual Review of Test Methods and Specifications for Plastics
D7210 Practice for Extraction of Additives in Polyolefin Plastics
E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
E691 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 IEEE/ASTM SI-10.
Chromatographic terms and relationships are as described in Practice E355.
3.2 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. A
known volume of this extract is injected into a gas chromatographic column packed with a liquid-coated solid support. Passing
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. 1, 2009March 1, 2017. Published August 2009March 2017. Originally approved in 1983. Last previous edition approved in 20022009 as
D4275 - 02.D4275 - 09. DOI: 10.1520/D4275-09.10.1520/D4275-17.
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.
*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 ----------------------
D4275 − 17
through this column in a stream of carrier gas, BHT is separated from the extraction solvent and other components. Responses of
BHT and any internal standard are measured by a flame ionization detector. 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 used in the manufacture of polyethylene are necessary in order to correlate
performance properties with polymer composition.
5.2 The BHT extraction procedure is made effective by the insolubility of the polymer sample in solvents generally used for
gas chromatographic analysis.
6. Interferences
6.1 Any material eluting at or near the BHT or MM retention times will cause erron
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.