ASTM D4275-96

Designation: D 4275 – 96
Standard Test Method for
Determination of Butylated Hydroxy Toluene (BHT) in
Polymers of Ethylene and Ethylene–Vinyl Acetate (EVA)
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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 3. Terminology
1.1 This test method describes a procedure for the determi- 3.1 Definitions—Units and symbols used in this test method
nation of butylated hydroxy toluene (BHT) (2,6-di-t-butyl-4- are those recommended in Practice E 380. Chromatographic
methyl-hydroxybenzene) in polymers of ethylene and terms and relationships are as described in Practice E 355.
ethylene-vinyl acetate (EVA) copolymers by solvent extraction 3.2 Abbreviations:
followed by gas chromatographic analysis. Detection of the 3.2.1 BHT—Butylated hydroxy toluene (2,6-di-tert-butyl-4-
compound is achieved by flame ionization, and quantitative methyl-hydroxybenzene).
analysis is obtained by use of internal or external standards, as 3.2.2 MM—Methyl myristate.
described in Practices E 260, E 355, and E 594. 3.2.3 EVA—Ethylene-vinyl acetate copolymers.
1.2 The values stated in SI units are to be regarded as the 3.2.4 LDPE—Low-density polyethylene.
standard. The values given in parentheses are for information 3.2.5 HDPE—High-density polyethylene.
only.
4. Summary of Test Method
1.3 This standard does not purport to address all of the
4.1 The BHT from a finely ground polymer sample is
safety concerns, if any, associated with its use. It is the
extracted by shaking or refluxing with cyclohexane or isopro-
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- panol that may contain an internal standard. A known volume
of this extract is injected into a gas chromatographic column
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 9. packed with a liquid-coated solid support. Passing through this
column in a stream of carrier gas, BHT is separated from the
NOTE 1—There is no similar or equivalent ISO standard.
extraction solvent and other components. Responses of BHT
and any internal standard are measured by a flame ionization
2. Referenced Documents
detector. This signal is recorded to indicate the relative
2.1 ASTM Standards:
concentration and retention time of BHT.
D 4968 Guide to Using the Flow Chart for Annual Review
of Standards Including the Model Precision and Bias
5. Significance and Use
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Statement for Plastics
5.1 Separation and identification of stabilizers used in the
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E 260 Practice for Packed Column Gas Chromatography
manufacture of polyethylene are necessary in order to correlate
E 355 Practice for Gas Chromatography Terms and Rela-
performance properties with polymer composition.
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tionships
5.2 The BHT extraction procedure is made effective by the
E 380 Practice for Use of the International System of Units
insolubility of the polymer sample in solvents generally used
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(SI) (the Modernized Metric System)
for gas chromatographic analysis.
E 594 Practice for Testing Flame Ionization Detectors Used
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in Gas Chromatography
6. Interferences
E 691 Practice for Conducting an Interlaboratory Study to
6.1 Any material eluting at or near the BHT or MM
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Determine the Precision of a Test Method
retention times will cause erroneous results. Prior to extraction,
solvent blanks should be analyzed to confirm the absence of
interfering peaks.
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This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
7. Apparatus
Current edition approved Aug. 10, 1996. Published February 1997. Originally
published as D 4275 – 83. Last previous edition D 4275 – 91.
7.1 Reflux Extraction, consisting of 250-mL round-bottom
This test method has been updated to include an ISO statement, report section,
flask with condenser and heating mantle to fit.
and updated precision and bias statement to meet Practice E 691.
2
7.2 Wiley Mill, with 10 and 20-mesh screens.
Annual Book of ASTM Standards, Vol 08.03.
3
Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 4275
7.3 Wrist-Action Shaker. 11.4 Weigh and transfer 20 6 0.1 mg of BHT into a 500-mL
7.4 Gas Chromatograph, equipped with a flame ionization volumetric flask.
detector. 11.5 Dissolve BHT in the internal standard solution in
7.5 Chromatographic Column, 3.2-mm outside diameter accordance with 11.3 and dilute to volume using this same
times 1.8 m packed with 20 % UCW-98 on 80/100 mesh solution.
Chromosorb P, a similar p
...