ASTM D322-97(2012)e1
(Test Method)Standard Test Method for Gasoline Diluent in Used Gasoline Engine Oils by Distillation
Standard Test Method for Gasoline Diluent in Used Gasoline Engine Oils by Distillation
SIGNIFICANCE AND USE
5.1 Some fuel dilution of the engine oil may take place during normal operation. However, excessive fuel dilution is of concern in terms of possible performance problems.
SCOPE
1.1 This test method covers determination of the amount of dilution in crankcase oils of engines when gasoline has been used as the fuel.
Note 1: There may be cases in dispute, therefore, the user of this test method is advised to establish whether this method will be accepted. There may be cases where Test Method D3525 results will be set as the referee value.
1.2 The values stated in acceptable SI units are to be regarded as the standard.
1.3 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 precautionary statement, see 6.4, 7.1, and 9.3.
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´1
Designation: D322 − 97(Reapproved 2012)
Standard Test Method for
Gasoline Diluent in Used Gasoline Engine Oils by
Distillation
This standard is issued under the fixed designation D322; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—The IP logo and designation were removed editorially in September 2016.
1. Scope 2.2 IP Methods for Analyses and Testing, Vol II, Part I
1.1 This test method covers determination of the amount of
dilution in crankcase oils of engines when gasoline has been
3. Terminology
used as the fuel.
3.1 Definitions:
NOTE 1—There may be cases in dispute, therefore, the user of this test
3.1.1 fuel diluent, n—in used oil analysis, unburnt fuel
methodisadvisedtoestablishwhetherthismethodwillbeaccepted.There
components that enter the engine crankcase causing dilution of
may be cases where Test Method D3525 results will be set as the referee
the oil.
value.
3.1.1.1 Discussion—In this test method, the fuel diluent
1.2 The values stated in acceptable SI units are to be
components being determined are from gasoline.
regarded as the standard.
3.1.2 used oil, n—any oil that has been in a piece of
1.3 This standard does not purport to address all of the
equipment (for example, an engine, gearbox, transformer, or
safety concerns, if any, associated with its use. It is the
turbine) whether operated or not. D4175
responsibility of the user of this standard to establish appro-
3.1.2.1 Discussion—In this test method, used oil is from a
priate safety and health practices and determine the applica-
gasoline engine.
bility of regulatory limitations prior to use. For specific
precautionary statement, see 6.4, 7.1, and 9.3.
4. Summary of Test Method
4.1 The sample, mixed with water, is placed in a glass still
2. Referenced Documents
provided with a reflux condenser discharging into a graduated
2.1 ASTM Standards:
trap connected to the still. Heat is applied, and the contents of
D235 Specification for Mineral Spirits (Petroleum Spirits)
the still are brought to boiling. The diluent in the sample is
(Hydrocarbon Dry Cleaning Solvent)
vaporized with the water and then liquefied in the condenser.
D3525 Test Method for Gasoline Diluent in Used Gasoline
The diluent collects at the top of the trap, and the excess water
Engine Oils by Gas Chromatography
runs back to the still where it is again vaporized, carrying over
D4057 Practice for Manual Sampling of Petroleum and
an additional quantity of diluent. The boiling is continued until
Petroleum Products
all the diluent has been boiled out and recovered in the trap.
D4175 Terminology Relating to Petroleum Products, Liquid
The volume is recorded.
Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and
5. Significance and Use
Petroleum Products
5.1 Some fuel dilution of the engine oil may take place
duringnormaloperation.However,excessivefueldilutionisof
concern in terms of possible performance problems.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
6. Apparatus
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
Current edition approved Nov. 1, 2012. Published November 2012. Originally
6.1 Flask, round-bottom type (see Fig. 1 and A1.1).
approved in 1930. Last previous edition approved in 2007 as D322 – 97 (2012).
DOI: 10.1520/D0322-97R12E01.
6.2 Condenser, Liebig straight-tube type (see A1.2).
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
the ASTM website. U.K., http://www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D322 − 97 (2012)
FIG. 1 Apparatus for Determining Diluent in Gasoline Engine Crankcase Oil
6.3 Trap, 5 mL, graduated in 0.1 mL increments (see Fig. 1 cylinder. Add additional water to the flask to make a total of
and Fig. 2 and A1.3). approximately 500 mL of water. Fill the trap with cold water
and add 1 mL 6 0.1 mL of denatured ethanol to the water in
6.4 Heater—Any suitable gas burner or electric heater may
the trap.
be used with the glass flask. (Warning—Hot exposed surface.
Avoid contact by wearing protective equipment as required.) 9.2 Assemble the apparatus as shown in Fig. 1, so that the
tip of the condenser is directly over the indentation in the trap.
7. Reagents and Materials
9.3 Apply heat to the flask at such a rate that refluxing starts
7.1 Ethanol, Denatured , conforming to either Formula No.
within 7 min to 10 min after heat is applied, with the water and
30 or 3A of the US Bureau of Internal Revenue. (Warning—
sample being at 21 °C to 38 °C prior to application of heat.
Flammable. Denatured. Cannot be made non-toxic.)
After boiling and condensation has commenced, adjust the rate
of boiling so that condensed distillate is discharged from the
7.2 Mineral Spirits (Petroleum Spirits), conforming to
condenser at a rate of 1 to 3 drops per s. (Warning—Hot
Specification D235.
exposed surface. Avoid contact by wearing protective equip-
NOTE 2—In Annex A1.3, the use of reagent grade heptane may be the
ment as required.)
preferred solvent because the use of commerical grade heptane or mineral
spirits can cause complications of container disposal that may not be
NOTE 3—Bumping with a tendency to froth over is often experienced
required for the disposal of the containers for reagent grade heptane.
with dirty oils. The use of boiling stones, steel wool, or about 5 mL of
concentrated hydrochloric acid (HCl) in the flask is often helpful in
8. Sampling
elimi
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D322 − 97 (Reapproved 2012) D322 − 97 (Reapproved 2012)
Designation: 23/2000
Standard Test Method for
Gasoline Diluent in Used Gasoline Engine Oils by
Distillation
This standard is issued under the fixed designation D322; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
ε NOTE—The IP logo and designation were removed editorially in September 2016.
1. Scope
1.1 This test method covers determination of the amount of dilution in crankcase oils of engines when gasoline has been used
as the fuel.
NOTE 1—There may be cases in dispute, therefore, the user of this test method is advised to establish whether this method will be accepted. There may
be cases where Test Method D3525 results will be set as the referee value.
1.2 The values stated in acceptable SI units are to be regarded as the standard.
1.3 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 precautionary statement, see 6.4, 7.1, and 9.3.
2. Referenced Documents
2.1 ASTM Standards:
D235 Specification for Mineral Spirits (Petroleum Spirits) (Hydrocarbon Dry Cleaning Solvent)
D3525 Test Method for Gasoline Diluent in Used Gasoline Engine Oils by Gas Chromatography
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
2.2 IP Methods for Analyses and Testing, Vol II, Part I
3. Terminology
3.1 Definitions:
3.1.1 fuel diluent, n—in used oil analysis, unburnt fuel components that enter the engine crankcase causing dilution of the oil.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Liquid Fuels and Lubricants.
This test method was adopted as a joint ASTM-IP standard in 1964. In the IP, this method is under the jurisdiction of the Standardization Committee.
Current edition approved Nov. 1, 2012. Published November 2012. Originally approved in 1930. Last previous edition approved in 2007 as D322 – 97 (2012). DOI:
10.1520/D0322-97R12.
Current edition approved Nov. 1, 2012. Published November 2012. Originally approved in 1930. Last previous edition approved in 2007 as D322 – 97 (2012). DOI:
10.1520/D0322-97R12E01.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.energyinst.org.uk.
3.1.1.1 Discussion—
In this test method, the fuel diluent components being determined are from gasoline.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
´1
D322 − 97 (2012)
FIG. 1 Apparatus for Determining Diluent in Gasoline Engine Crankcase Oil
3.1.2 used oil, n—any oil that has been in a piece of equipment (for example, an engine, gearbox, transformer, or turbine)
whether operated or not. D4175
3.1.2.1 Discussion—
In this test method, used oil is from a gasoline engine.
4. Summary of Test Method
4.1 The sample, mixed with water, is placed in a glass still provided with a reflux condenser discharging into a graduated trap
connected to the still. Heat is applied, and the contents of the still are brought to boiling. The diluent in the sample is vaporized
with the water and then liquefied in the condenser. The diluent collects at the top of the trap, and the excess water runs back to
the still where it is again vaporized, carrying over an additional quantity of diluent. The boiling is continued until all the diluent
has been boiled out and recovered in the trap. The volume is recorded.
5. Significance and Use
5.1 Some fuel dilution of the engine oil may take place during normal operation. However, excessive fuel dilution is of concern
in terms of possible performance problems.
6. Apparatus
6.1 Flask, round-bottom type (see Fig. 1 and A1.1).
6.2 Condenser, Liebig straight-tube type (see A1.2).
6.3 Trap, 5 mL, 5 mL, graduated in 0.1-mL0.1 mL increments (see Fig. 1 and Fig. 2 and A1.3).
6.4 Heater—Any suitable gas burner or electric heater may be used with the glass flask. (Warning—Hot exposed surface. Avoid
contact by wearing protective equipment as required.)
7. Reagents and Materials
7.1 Ethanol, Denatured , conforming to either Formula No. 30 or 3A of the US Bureau of Internal Revenue. (Warning—
Flammable. Denatured. Cannot be made non-toxic.)
7.2 Mineral Spirits (Petroleum Spirits), conforming to Specification D235.
NOTE 2—In Annex A1.3, the use of reagent grade heptane may be the preferred solvent because the use of commerical grade heptane or mineral spirits
can cause complications of container disposal that may not be required for the disposal of the containers for reagent grade heptane.
8. Sampling
8.1 Obtain a representative sample using either Practices D4057 or D4177.
´1
D322 − 97 (2012)
All dimensions are in millimetres
FIG. 2 Alternate Closures for Diluent Trap
9. Procedure
9.1 Mix the sample thoroughly, measure 2525 mL 6 5 mL 5 mL by means of a 25-mL25 mL graduated cylinder, and transfer
as much as possible of the contents of the cylinder by pouring it into the flask. Wash the graduated cylinder with successive portions
of hot water until only a negligible amount of oil is left in the cylinder. Add additional water to the flask to make a total of
approximately 500 mL 500 mL of water. Fill the trap with cold water and add 11 mL 6 0.1 mL of denatured ethanol to
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