ASTM D4291-93(1998)

Standard Test Method for Trace Ethylene Glycol in Used Engine Oil

SCOPE
1.1 This test method provides for 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 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3 This standard does not purport to address all of the safety problems, 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 hazard statements see Notes 2 through 5.  Note 1-A qualitative determination of glycol-base antifreeze is provided in Test Method D2982. Procedure A is sensitive to about 100 ppm.

General Information

• Status: Historical
• Publication Date: 31-Dec-1992
• ICS: 75.100 - Lubricants, industrial oils and related products
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.04.0L - Gas Chromatography Methods

Relations

• Replaced By: ASTM D4291-04 - Standard Test Method for Trace Ethylene Glycol in Used Engine Oil
• Effective Date: 01-Nov-2004
• Referred By: ASTM D6074-15(2022) - Standard Guide for Characterizing Hydrocarbon Lubricant Base Oils
• Effective Date: 01-Jan-1993
• Referred By: ASTM D7922-21 - Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography
• Effective Date: 01-Jan-1993

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
An American National Standard
Designation:D4291–93 (Reapproved 1998)
Standard Test Method for
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 4. Significance and Use
1.1 This test method provides for the determination of 4.1 Leakage of aqueous engine coolant into the crank case
ethylene glycol as a contaminant in used engine oil. This test weakens the ability of the oil to lubricate. If ethylene glycol is
method is designed to quantitate ethylene glycol in the range present, it promotes varnish and deposit formation. This test
from 5 to 200 mass ppm. method is designed for early detection to prevent coolant from
1.2 The values stated in SI units are to be regarded as the accumulating and seriously damaging the engine.
standard. The values given in parentheses are for information
5. Apparatus
only.
5.1 Gas Chromatograph—Any gas chromatograph
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the equipped with the following:
5.1.1 Flame Ionization Detector, capable of operating con-
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- tinuously at a temperature equivalent to the maximum column
temperature employed, and connected to the column so as to
bility of regulatory limitations prior to use. For specific hazard
statements see Notes 2-5. avoid any cold spots.
5.1.2 Sample Inlet System, providing for on-column injec-
NOTE 1—A qualitative determination of glycol-base antifreeze is pro-
tion and capable of operating continuously at a temperature
vided in Test Method D 2982. ProcedureAis sensitive to about 100 ppm.
equivalent to the maximum column temperature employed.
2. Referenced Documents 5.2 Recorder—Recording potentiometer with a full-scale
response time of2sor less may be used.
2.1 ASTM Standards:
5.3 Column—1.2-m (4-ft) by 6.4-mm ( ⁄4-in.) copper tube
D 1193 Specification for Reagent Water
packed with 5 mass % Carbowax 20-M liquid phase on 30/60
D 2982 Test Methods for Detecting Glycol-BaseAntifreeze
3 mesh Chromosorb T solid support.
in Used Lubricating Oils
5.4 Integrator—Manual, mechanical, or electronic integra-
D 4057 Practice for Manual Sampling of Petroleum and
4 tion is required to determine the peak area. However, best
Petroleum Products
precision and automated operation can be achieved with
3. Summary of Test Method electronic integration.
5.5 Centrifuge—RCF 600 minimum and centrifuge tubes
3.1 The sample of oil is extracted with water and the
with stoppers.
analysis is performed on the water extract. A reproducible
5.6 Syringe—A microsyringe, 10 µL is needed for sample
volume of the extract is injected into a gas chromatograph
introduction.
using on-column injection and the eluting compounds are
5.7 Pasteur Pipets.
detected by a flame ionization detector. The ethylene glycol
5.8 Vials, 2 mL, with crimped septum caps.
peak area is determined and compared with areas obtained
from the injection of freshly prepared known standards.
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be
This test method is under the jurisdiction of ASTM Committee D-2 on
used in all tests. Unless otherwise indicated, it is intended that
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
all reagents conform to the specifications of the Committee on
D02.04on Hydrocarbon Analysis and D02.06 on Analysis of Lubricants.
Analytical Reagents of the American Chemical Society where
Current edition approved Aug. 15, 1993. Published October 1993. Originally
published as D 4291 – 83. Last previous edition D 4291 – 88.
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4291
such specifications are available. Other grades may be used, 7.3 Column Conditioning—The column must be condi-
provided it is first ascertained that the reagent is of sufficiently tioned at the operating temperature to reduce baseline shift due
high purity to permit its use without lessening the accuracy of to bleeding of column substrate.
the determination. 7.4 Chromatograph—Place in service in accordance with
6.2 Purity of Water—Unless otherwise indicated, references manufacturer’s instructions. Typical operating conditions are
to water shall be understood to mean reagent water as defined shown in Table 1.
by Type II of Specification D 1193.
8. Calibration
6.3 Air and Hydrogen—Warning: Precaution—See Note
2. (Warning—See Note 3.)
8.1 Analyze each of the calibration mixtures following the
procedure in Section 10, injecting exactly 5 µL and record the
NOTE 2—Precaution: The air supply may be from a cylinder under
area of the ethylene glycol peak.
high pressure.
NOTE 3—Warning: Hydrogen is an extremely flammable gas under 8.2 Calculate a response factor for each calibration mixture
pressure.
as follows:
6.4 Calibration Mixtures—Aminimum of three mixtures of
F 5 C/A (1)
water and ethylene glycol are prepared to cover the range from
where:
5 to 200 mass ppm. Prepare one blend of approximately 2000
F = response factor for ethylene glycol,
mass ppm ethylene glycol in water to provide for accurate
C = concentration in mass ppm of ethylene glycol in water,
weighing; then, prepare dilutions of that solution.
and
6.5 Carrier Gas, helium or nitrogen may be used with the
A = peak area for ethylene glycol.
flame ionization detector. (Warning: Precaution—See Note
8.3 Calculate an average response factor.
4.)
NOTE 7—A calibration curve may be employed to obtain the response
NOTE 4—Precaution: Helium and nitrogen are compressed gases un-
factor.
der high pressure.
6.6 Ethylene Glycol, 99 mass % pure. 9. Prep
...