ASTM D4768-96

Standard Test Method for Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-Ditertiary- Butyl Phenol in Insulating Liquids by Gas Chromatography

SCOPE
1.1 This test method covers the determination by gas chromatography of 2,6-ditertiary-butyl para-cresol and 2,6-ditertiary-butyl phenol in new and used insulating liquids at concentrations up to 0.5%. It includes the determination in Type I and II insulating mineral oils as specified in Specification D3487, but has also been used to measure these inhibitors in other insulating liquids, such as esters and high fire-point hydrocarbons.  
1.2 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.

General Information

• Status: Historical
• Publication Date: 31-Dec-1995
• ICS: 29.040.10 - Insulating oils
• Technical Committee: D27 - Electrical Insulating Liquids and Gases
• Drafting Committee: D27.03 - Analytical Tests

Relations

• Replaced By: ASTM D4768-03 - Standard Test Method for Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-Ditertiary- Butyl Phenol in Insulating Liquids by Gas Chromatography
• Effective Date: 10-Mar-2003

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn. Contact
ASTM International (www.astm.org) for the latest information.
Designation: D 4768 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Analysis of 2,6-Ditertiary-Butyl Para-Cresol and 2,6-
Ditertiary-Butyl Phenol in Insulating Liquids by Gas
1
Chromatography
This standard is issued under the fixed designation D 4768; 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 a quantitative measure of the amounts of 2,6-ditertiary-butyl
para-cresol and 2,6-ditertiary-butyl phenol that have been
1.1 This test method covers the determination by gas
added to the oil. In a used oil, the test measures the amount of
chromatography of 2,6-ditertiary-butyl para-cresol and 2,6-
these inhibitors remaining in the oil. This test method is
ditertiary-butyl phenol in new and used insulating liquids at
suitable for manufacturing control, specification acceptance,
concentrations up to 0.5 %. It includes the determination in
and service evaluation.
Type I and II insulating mineral oils as specified in Specifica-
4.2 This test method is used to separate, identify, and
tion D 3487, but has also been used to measure these inhibitors
quantify the inhibitors with minimal interference and matrix
in other insulating liquids, such as esters and high fire-point
effects.
hydrocarbons.
4.3 This test method has also been used successfully to
1.2 This standard does not purport to address all of the
determine the inhibitor concentrations in other insulating
safety concerns, if any, associated with its use. It is the
liquids such as esters and high-temperature hydrocarbons.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use.
5.1 Gas Chromatograph, equipped with oven temperature
control constant to 1°C and with heated injector port.
2. Referenced Documents
5.1.1 Means to Record the Chromatogram, such as a pen
2.1 ASTM Standards:
recorder or a digital integrator to determine peak areas, is
D 923 Test Method for Sampling Electrical Insulating Liq-
recommended. An automated sample injector may be used.
2
uids
5.2 Flame Ionization Detector, with appropriate hydrogen/
D 3487 Specification for Mineral Insulating Oil Used in
air gas flows, is preferred over a thermal conductivity detector
2
Electrical Apparatus
to provide maximum sensitivity.
D 5222 Guide for High-Fire Point Electrical Insulating Oils
5.3 Column, a suitable stainless steel or glass column
2
of Petroleum Origin
packed with a nonpolar silicone on an appropriate support.
3
E 260 Practice for Packed Column Gas Chromatography
4 5
NOTE 1—A 3 % OV-1 on 100/120 Mesh Supelcoport, 1.83 m (6 ft)
3. Summary of Test Method
long, 3.2 mm (0.125 in.) in outside diameter has been used successfully.
3.1 The test specimen is placed onto a column containing
5.3.1 Condition columns in accordance with manufacturer’s
activated alumina and extracted to remove interfering sub-
recommendations. Disconnect columns from detector prior to
stances. The inhibitors are then eluted from the column with
conditioning and reconnect after conditioning.
suitable solvent and analyzed by gas chromatography. The
5.4 Precision Syringe, glass, 10.0 μL.
inhibitor type and quantity are determined by comparison of
5.5 Volumetric Glassware, appropriate for making dilutions.
each component with a working standard tested under similar
5.6 Pipets, Pasteur, disposable, 146 by 7.5 mm.
conditions.
5.7 Analytical Balance.
5.8 Automatic Pipetter, 1 mL calibrated, adjustable.
4. Significance and Use
5.9 Oven, capable of maintaining a temperature of 275 6
4.1 In new electrical insulating oil, this test method provides
5°C for conditioning extraction columns.
5.10 Desiccator.
1
6. Reagents and Materials
This test method is under the jurisdiction of ASTM Committee D-27 on
Electrical Insulating Liquids and Gasesand is the direct responsibility of Subcom-
6.1 Purity of Reagents—Use reagent grade chemicals in all
mittee D27.01on Physical Tests.
Current edition approved March 10, 1996. Published May 1996. Originally
published as D 4768 – 88. Last previous edition D 4768 – 95.
2 4
Annual Book of ASTM Standards, Vol 10.03. Registered trademark of Ohio Valley Specialty Co.
3 5
Annual Book of ASTM Standards, Vol 14.01. Registered trademark of Supelco, Inc.
1

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NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.
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