ASTM D4275-02

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4275–02
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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 691 Practice for Conducting an Interlaboratory Study to
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Determine the Precision of a Test Method
1.1 This test method describes a procedure for the determi-
nation of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-4-
3. Terminology
methyl-hydroxybenzene) in polymers of ethylene and
3.1 Definitions—Units and symbols used in this test method
ethylene-vinyl acetate (EVA) copolymers by solvent extraction
are those recommended in Practice E 380. Chromatographic
followed by gas chromatographic analysis. Detection of the
terms and relationships are as described in Practice E 355.
compound is achieved by flame ionization, and quantitative
3.2 Abbreviations:Abbreviations:
analysis is obtained by use of internal or external standards, as
3.2.1 BHT—Butylated hydroxy toluene (2,6-di-tert-butyl-4-
described in Practices E 260, E 355, and E 594.
methyl-hydroxybenzene).
1.2 The values stated in SI units are to be regarded as the
3.2.2 MM—Methyl myristate.
standard. The values given in parentheses are for information
3.2.3 EVA—Ethylene-vinyl acetate copolymers.
only.
3.2.4 LDPE—Low-density polyethylene.
1.3 This standard does not purport to address all of the
3.2.5 HDPE—High-density polyethylene.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Method
priate safety and health practices and determine the applica-
4.1 The BHT from a finely ground polymer sample is
bility of regulatory limitations prior to use. Specific precau-
extracted by shaking or refluxing with cyclohexane or isopro-
tionary statements are given in Section 9.
panol that may contain an internal standard. A known volume
NOTE 1—There is no similar or equivalent ISO standard.
of this extract is injected into a gas chromatographic column
packed with a liquid-coated solid support. Passing through this
2. Referenced Documents
column in a stream of carrier gas, BHT is separated from the
2.1 ASTM Standards:
extraction solvent and other components. Responses of BHT
D 4968 Guide for Annual Review of Test Methods and
and any internal standard are measured by a flame ionization
2
Specifications for Plastics
detector. This signal is recorded to indicate the relative
2
E 260 Practice for Packed Column Gas Chromatography
concentration and retention time of BHT.
E 355 Practice for Gas Chromatography Terms and Rela-
3
tionships 5. Significance and Use
E 380 Practice for Use of the International System of Units
5.1 Separation and identification of stabilizers used in the
4
(SI) (the Modernized Metric System)
manufacture of polyethylene are necessary in order to correlate
E 594 Practice for Testing Flame Ionization Detectors Used
performance properties with polymer composition.
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in Gas Chromatography
5.2 The BHT extraction procedure is made effective by the
insolubility of the polymer sample in solvents generally used
for gas chromatographic analysis.
1
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
6. Interferences
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
Current edition approved Aug. 10, 2002. Published October 2002. Originally
6.1 Any material eluting at or near the BHT or MM
published as D 4275 – 83. Last previous edition D 4275 – 96.
retentiontimeswillcauseerroneousresults.Priortoextraction,
2
Annual Book of ASTM Standards, Vol 08.03.
3 solvent blanks should be analyzed to confirm the absence of
Annual Book of ASTM Standards, Vol 14.02.
4
interfering peaks.
Discontinued; see 1997 Annual Book of ASTM Standards , Vol 14.02.
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D4275–02
7. Apparatus 11.2 Transfer syringe contents to a 2-Lvolumetric flask and
immediately reweigh the syringe (60.1 mg).
7.1 Reflux Extraction, consisting of 250-mL round-bottom
11.3 Dilute to volume with extraction solvent (cyclohexane
flask with condenser and heating mantle to fit.
or isopropyl alcohol) and store in a tightly stoppered flask.
7.2 Wiley Mill, with 10 and 20-mesh screens.
11.4 Weighandtransfer20 60.1mgofBHTintoa500-mL
7.3 Wrist-Action Shaker.
volumetric flask.
7.4 Gas Chromatograph, equipped with a flam
...