ASTM D4291-04(2009)
(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
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 D 2982. Procedure A is sensitive to about 100 ppm.
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Designation: D4291 − 04(Reapproved 2009)
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 and Lubricants and is the direct responsibility of Subcommittee
D02.04.0L on Gas Chromatography Methods.
Current edition approved April 15, 2009. Published July 2009. Originally
6. Reagents and Materials
approved in 1983. Last previous edition approved in 2004 as D4291 – 04. DOI:
10.1520/D4291-04R09.
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 (2009)
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 eac
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard Designation: D 4291 – 04 (Reapproved 2009)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1This 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.
1.2The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3
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 hazard statements see Notes 2-5For specific warning statements, see Section 6.
NOTE 1—A qualitative determination of glycol-base antifreeze is provided in Test Methods D 2982. Procedure A is sensitive to about 100 ppm.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 2982 Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
D 4057 Practice for Manual Sampling of Petroleum and Petroleum Products
3. Summary of Test Method
3.1 The sample of oil is extracted with water and the analysis is performed on the water extract.Areproducible volume of the
extract is injected into a gas chromatograph using on-column injection and the eluting compounds are detected by a flame
ionization detector. The ethylene glycol peak area is determined and compared with areas obtained from the injection of freshly
prepared known standards.
4. 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.
5. Apparatus
5.1 Gas Chromatograph—Any gas chromatograph equipped with the following:
5.1.1 Flame Ionization Detector, capable of operating continuously at a temperature equivalent to the maximum column
temperature employed, and connected to the column so as to avoid any cold spots.
5.1.2 SampleInletSystem, providing for on-column injection and capable of operating continuously at a temperature equivalent
to the maximum column temperature employed.
5.2 Recorder—Recording potentiometer with a full-scale response time of2sor less may be used.
5.3 Column—1.2-m (4-ft) by 6.4-mm ( ⁄4-in.) copper tube packed with 5 mass% Carbowax 20-M liquid phase on 30/60 mesh
ChromosorbTsolidsupport.Columns—1.2-m(4-ft)by6.4-mm( ⁄4-in.)coppertubepackedwith5mass %Carbowax20-Mliquid
This test method is under the jurisdiction of ASTM Committee D-2 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.04 on
Hydrocarbon Analysis and D02.06 on Analysis of Lubricants.
Current edition approved Aug. 15, 1993. Published October 1993. Originally published as D4291–83. Last previous edition D4291–88.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.04.0L
on Gas Chromatography Methods.
Current edition approved April 15, 2009. Published July 2009. Originally approved in 1983. Last previous edition approved in 2004 as D 4291 – 04.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4291–04 (2009)
phase on 30/60 mesh Chromosorb T solid support. As an alternative, a fused silica capillary column, 15 m long with a 0.53–mm
ID and 2.0–micron film thickness of a bonded polyethylene glycol can be used.
5.4 Integrator—Manual, mechanical, or electronic integration is required to determine the peak area. However, best precision
and automated operation can be achieved with electronic integration.
5.5 Centrifuge—RCF 600 minimum and centrifuge tubes with stoppers.
5.6 Syringe—A microsyringe, 10 µL is needed for sample introduction.
5.7 Pasteur Pipets.
5.8 Vials, 2 mL, with crimped septum caps.
6. Reagents and Materials
6.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity
to permit its use without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II of Specification D 1193.
6.3 Air and Hydrogen—Warning: Precaution—See Note 2. (Warning—See Note 3.)
NOTE2—Precaution:The air supply may be from a cylinder under high pressure.
NOTE3—Warning:Hydrogen is an extremely flammable gas under pressure.
6.4—(Warning—The air supply may be from a cylinder under high pressure. Hydrogen is an extremely flammable gas under
pressure.)
6.4 Calibration Mixtures—A minimum of three mixtures of water and ethylene glycol are prepared to cover the range from 5
to 200 mass ppm. Prepare one blend of approximately 2000 mass ppm ethylene glycol in water to provide for accurate weighing;
then, prepare dilutions of that solution.
6.5 Carrier Gas, helium or nitrogen may be used with the flame ionization detector. (Warning: Precaution—See Note 4.)
NOTE4—Precaution:Helium and nitrogen are compressed gases under high pressure. , helium or nitrogen may be used with the flame ionization
detector. (Warning— Helium and nitrogen are compressed gases under high pressure.)
6.6 Ethylene Glycol, 99 mass % pure.
6.7 n-Hexane, 99 mol% pure. (Warning: Precaution—See Note 5.)
NOTE5—Precaution:, 99 mol% pure. (Warning—n-Hexane is extremely flammable, harmful if inhaled, may produce nerve cell damage; see A1.1.
damage.)
6.8 Liquid Phase and Solid Support , 5 mass % Carbowax 20-M liquid phase on 30/60 mesh Chromosorb T solid support.
6.9 Tubing, 6.4 mm ( ⁄4 in.) in outside diameter, 1.2 m (4 ft) long of copper.
6.10 Water, deionized or distilled.
7. Preparation of Apparatus
7.1 ColumnPreparation—Preparethecolumnbythefollowingsteps:PackedColumnPreparation—Ifapackedcolumnisused,
prepare it using the following steps:
7.1.1 Prepare the packing, 5 mass % Carbowax 20-M liquid phase on 30/60 mesh Chromosorb T solid support, by any
satisfactory method used
...
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