ASTM D4291-04

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An American National Standard
Designation:D4291–04
Standard Test Method for
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Trace Ethylene Glycol in Used Engine Oil
This standard is issued under the fixed designation D 4291; 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* detected by a flame ionization detector. The ethylene glycol
peak area is determined and compared with areas obtained
1.1 This test method covers the determination of ethylene
from the injection of freshly prepared known standards.
glycol as a contaminant in used engine oil. This test method is
designed to quantitate ethylene glycol in the range from 5 to
4. Significance and Use
200 mass ppm.
4.1 Leakage of aqueous engine coolant into the crank case
1.2 The values stated in SI units are to be regarded as the
weakens the ability of the oil to lubricate. If ethylene glycol is
standard. The values given in parentheses are for information
present, it promotes varnish and deposit formation. This test
only.
method is designed for early detection to prevent coolant from
1.3 This standard does not purport to address all of the
accumulating and seriously damaging the engine.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Gas Chromatograph—Any gas chromatograph
bilityofregulatorylimitationspriortouse.Forspecificwarning
equipped with the following:
statements, see Section 6.
5.1.1 Flame Ionization Detector, capable of operating con-
NOTE 1—A qualitative determination of glycol-base antifreeze is pro-
tinuously at a temperature equivalent to the maximum column
vided inTest Methods D 2982. ProcedureAis sensitive to about 100 ppm.
temperature employed, and connected to the column so as to
avoid any cold spots.
2. Referenced Documents
5.1.2 Sample Inlet System, providing for on-column injec-
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2.1 ASTM Standards:
tion and capable of operating continuously at a temperature
D 1193 Specification for Reagent Water
equivalent to the maximum column temperature employed.
D 2982 Test Methods for Detecting Glycol-BaseAntifreeze
5.2 Recorder—Recording potentiometer with a full-scale
in Used Lubricating Oils
response time of2sor less may be used.
D 4057 Practice for Manual Sampling of Petroleum and
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5.3 Columns—1.2-m (4-ft) by 6.4-mm ( ⁄4-in.) copper tube
Petroleum Products
packed with 5 mass % Carbowax 20-M liquid phase on 30/60
mesh Chromosorb T solid support. As an alternative, a fused
3. Summary of Test Method
silica capillary column, 15 m long with a 0.53–mm ID and
3.1 The sample of oil is extracted with water and the
2.0–micron film thickness of a bonded polyethylene glycol can
analysis is performed on the water extract. A reproducible
be used.
volume of the extract is injected into a gas chromatograph
5.4 Integrator—Manual, mechanical, or electronic integra-
using on-column injection and the eluting compounds are
tion is required to determine the peak area. However, best
precision and automated operation can be achieved with
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electronic integration.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
5.5 Centrifuge—RCF 600 minimum and centrifuge tubes
D02.04 on Hydrocarbon Analysis.
with stoppers.
Current edition approved Nov. 1, 2004. Published November 2004. Originally
5.6 Syringe—A microsyringe, 10 µL is needed for sample
approved in 1983. Last previous edition approved in 1998 as D 4291–93(1998).
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or introduction.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.7 Pasteur Pipets.
Standards volume information, refer to the standard’s Document Summary page on
5.8 Vials, 2 mL, with crimped septum caps.
the ASTM website.
*A Summary of Changes section appears at the end of this standard.
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D4291–04
6. Reagents and Materials 7.3 Column Conditioning—The column must be condi-
tioned at the operating temperature to reduce baseline shift due
6.1 Purity of Reagents—Reagent grade chemicals shall be
to bleeding of column substrate.
used in all tests. Unless otherwise indicated, it is intended that
7.4 Chromatograph—Place in service in accordance with
all reagents conform to the specifications of the Committee on
manufacturer’s instructions. Typical operating conditions are
Analyt
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