ASTM D4291-04(2013)
(Test Method)Standard Test Method for Trace Ethylene Glycol in Used Engine Oil
Standard Test Method for Trace Ethylene Glycol in Used Engine Oil
SIGNIFICANCE AND USE
4.1 Leakage of aqueous engine coolant into the crank case weakens the ability of the oil to lubricate. If ethylene glycol is present, it promotes varnish and deposit formation. This test method is designed for early detection to prevent coolant from accumulating and seriously damaging the engine.
SCOPE
1.1 This test method covers the determination of ethylene glycol as a contaminant in used engine oil. This test method is designed to quantitate ethylene glycol in the range from 5 to 200 mass ppm.
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.For specific warning statements, see Section 6. Note 1—A qualitative determination of glycol-base antifreeze is provided in Test Methods D2982. Procedure A is sensitive to about 100 ppm.
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Designation: D4291 − 04 (Reapproved 2013)
Standard Test Method for
Trace Ethylene Glycol in Used Engine Oil
This standard is issued under the fixed designation D4291; 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 present, it promotes varnish and deposit formation. This test
method is designed for early detection to prevent coolant from
1.1 This test method covers the determination of ethylene
accumulating and seriously damaging the engine.
glycol as a contaminant in used engine oil. This test method is
designed to quantitate ethylene glycol in the range from 5 to
5. Apparatus
200 mass ppm.
1.2 This standard does not purport to address all of the
5.1 Gas Chromatograph—Any gas chromatograph
safety concerns, if any, associated with its use. It is the
equipped with the following:
responsibility of the user of this standard to establish appro-
5.1.1 Flame Ionization Detector, capable of operating con-
priate safety and health practices and determine the applica-
tinuously at a temperature equivalent to the maximum column
bility of regulatory limitations prior to use.FOR SPECIFIC WARNING
temperature employed, and connected to the column so as to
STATEMENTS, SEE SECTION 6.
avoid any cold spots.
NOTE 1—A qualitative determination of glycol-base antifreeze is
5.1.2 Sample Inlet System, providing for on-column injec-
provided in Test Methods D2982. Procedure A is sensitive to about 100
tion and capable of operating continuously at a temperature
ppm.
equivalent to the maximum column temperature employed.
2. Referenced Documents
5.2 Recorder—Recording potentiometer with a full-scale
2.1 ASTM Standards:
response time of2sor less may be used.
D1193 Specification for Reagent Water
D2982 Test Methods for Detecting Glycol-Base Antifreeze 5.3 Columns—1.2-m (4-ft) by 6.4-mm ( ⁄4-in.) copper tube
in Used Lubricating Oils packed with 5 mass % Carbowax 20-M liquid phase on 30/60
D4057 Practice for Manual Sampling of Petroleum and
mesh Chromosorb T solid support. As an alternative, a fused
Petroleum Products
silica capillary column, 15 m long with a 0.53–mm ID and
2.0–micron film thickness of a bonded polyethylene glycol can
3. Summary of Test Method
be used.
3.1 The sample of oil is extracted with water and the
5.4 Integrator—Manual, mechanical, or electronic integra-
analysis is performed on the water extract. A reproducible
tion is required to determine the peak area. However, best
volume of the extract is injected into a gas chromatograph
precision and automated operation can be achieved with
using on-column injection and the eluting compounds are
electronic integration.
detected by a flame ionization detector. The ethylene glycol
peak area is determined and compared with areas obtained
5.5 Centrifuge—RCF 600 minimum and centrifuge tubes
from the injection of freshly prepared known standards.
with stoppers.
4. Significance and Use
5.6 Syringe—A microsyringe, 10 µL is needed for sample
4.1 Leakage of aqueous engine coolant into the crank case
introduction.
weakens the ability of the oil to lubricate. If ethylene glycol is
5.7 Pasteur Pipets.
This test method is under the jurisdiction of ASTM Committee D02 on
5.8 Vials, 2 mL, with crimped septum caps.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0L on Gas Chromatography Methods.
Current edition approved Oct. 1, 2013. Published October 2013. Originally
6. Reagents and Materials
approved in 1983. Last previous edition approved in 2009 as D4291 – 04 (2009).
DOI: 10.1520/D4291-04R13.
6.1 Purity of Reagents—Reagent grade chemicals shall be
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
used in all tests. Unless otherwise indicated, it is intended that
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
all reagents conform to the specifications of the Committee on
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. Analytical Reagents of the American Chemical Society where
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4291 − 04 (2013)
TABLE 1 Typical Operating Conditions
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently Packed Column
Column: 1.2 m (4 ft) by 6.4 mm ( ⁄4 in.) OD copper
high purity to permit its use without lessening the accuracy of
Packing: 5 mass % Carbowax 20-M liquid phase on 30/60 mesh Chromosorb
the determination.
T solid support
Detector: FID
6.2 Purity of Water—Unless otherwise indicated, references
Detector Temperature: 200°C
to water shall be understood to mean reagent water as defined
Injection Port Temperature: 150°C
Column Oven Temperature: 130°C
by Type II of Specification D1193.
Carrier Gas Flow: 60 mL/min
6.3 Air and Hydrogen—(Warning—The air supply may be Sample Size: 5 µL
from a cylinder under high pressure. Hydrogen is an extremely
Capillary Column
flammable gas under pressure.)
Column: 15 m by 0.53–mm fused silica capillary with 2 µm of bonded
polyethylene glycol stationary phase
6.4 Calibration Mixtures—Aminimum of three mixtures of
Detector: FID
water and ethylene glycol are prepared to cover the range from
Detector Temperature: 300°C
Injection Port Temperature: 250°C
5 to 200 mass ppm. Prepare one blend of approximately 2000
Column Oven Initial Temperature: 150°C
mass ppm ethylene glycol in water to provide for accurate
Column Oven Initial Hold Time: 0 min
weighing; then, prepare dilutions of that solution.
Column Oven Temperature Program Rate: 10°C/min
Column Oven Program Final Temperature: 200°C
6.5 Carrier Gas, helium or nitrogen may be used with the
Column Oven Program Final Hold Time: 5 min
flame ionization detector. (Warning—Helium and nitrogen are Carrier Gas Flow: 22 mL/min
Sample Size: 1 µL
compressed gases under high pressure.)
6.6 Ethylene Glycol, 99 mass % pure.
6.7 n-Hexane, 99 mol % pure. (Warning—n-Hexane is
extremely flammable, harmful if inhaled, may produce nerve
7.4 Chromatograph—Place in service in accordance with
cell damage.)
manufacturer’s instructions. Typical operating conditions are
6.8 Liquid Phase and Solid Support, 5 mass % Carbowax shown in Table 1.
20-M liquid phase on 30/60 mesh ChromosorbTsolid support.
8. Calibration
6.9 Tubing, 6.4 mm ( ⁄4 in.) in outside diameter, 1.2 m (4 ft)
long of copper. 8.1 Analyze each of the calibration mix
...
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