ASTM D3524-90(1999)
(Test Method)Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography
Standard Test Method for Diesel Fuel Diluent in Used Diesel Engine Oils by Gas Chromatography
SCOPE
1.1 This test method covers the determination of diesel fuel as a contaminant in used lubricating oil. The method is limited to SAE 30 oil. Note 1-This test method may be applicable to higher viscosity grade oils. However, such oils were not included in the program used to develop the precision statement.
1.2 There is some overlap of the boiling ranges of diesel fuel and SAE 30 engine oils. Moreover, the boiling range of SAE 30 oils from various sources can vary appreciably. As a result, the calibration can be altered by as much as 2%, in terms of fuel dilution. When testing unknown or mixed brands of used engine oil, it should be realized that the precision of the method may be poorer than the precision obtained when calibrating with a new oil representative of the used oil being tested.
1.3 The values stated in SI units are to be regarded as the standard. The values stated in inch-pound units are for information only.
1.4 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.
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An American National Standard
Designation:D3524–90(Reapproved 1999)
Standard Test Method for
Diesel Fuel Diluent in Used Diesel Engine Oils by Gas
Chromatography
This standard is issued under the fixed designation D 3524; 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
For example: normal decane n–C
iso-tetradecane i–C
1.1 This test method covers the determination of diesel fuel
as a contaminant in used lubricating oil. The method is limited
3. Summary of Test Method
to SAE 30 oil.
3.1 A mixture of n-decane and used lubricating oil is
introduced into a gas chromatographic column which separates
NOTE 1—This test method may be applicable to higher viscosity grade
oils. However, such oils were not included in the program used to develop
hydrocarbonsinboilingpointorder.Thecolumntemperatureis
the precision statement.
raised at a reproducible rate and the resulting chromatogram is
interpreted for diesel fuel dilution.
1.2 There is some overlap of the boiling ranges of diesel
fuel and SAE 30 engine oils. Moreover, the boiling range of
4. Significance and Use
SAE 30 oils from various sources can vary appreciably. As a
4.1 Some fuel dilution of the engine oil may take place
result, the calibration can be altered by as much as 2 %, in
duringnormaloperation.However,excessivefueldilutionisof
terms of fuel dilution. When testing unknown or mixed brands
concern in terms of possible performance problems.
ofusedengineoil,itshouldberealizedthattheprecisionofthe
method may be poorer than the precision obtained when
5. Apparatus
calibrating with a new oil representative of the used oil being
5.1 Gas Chromatograph—Any gas chromatograph can be
tested.
used that has the following performance characteristics:
1.3 The values stated in SI units are to be regarded as the
5.1.1 Detector—Either a thermal conductivity or flame
standard. The values stated in inch-pound units are for infor-
ionization detector can be used. The detector must have
mation only.
sufficient sensitivity to detect 1.0 % decane with a peak height
1.4 This standard does not purport to address all of the
of at least 10 % of full scale on the recorder under the
safety concerns, if any, associated with its use. It is the
conditions prescribed in this method, and without loss of
responsibility of the user of this standard to establish appro-
resolution as defined in 7.1.3. The detector also must be
priate safety and health practices and determine the applica-
capable of operating continuously at a temperature equivalent
bility of regulatory limitations prior to use.
to the maximum column temperature employed, and it must be
2. Terminology
connected to the column so as to avoid any cold spots. Under
the conditions described for the method, the drift should not be
2.1 Definitions of Terms Specific to This Standard:
more than 1 % of full scale per hour.
2.1.1 fuel dilution—the amount, expressed as a percentage,
5.1.2 Column Temperature Programmer— The chromato-
of engine fuel found in engine lubricating oil. This may be the
graph must be capable of program temperature operation over
result of engine wear or improper performance.
a range sufficient to establish a retention time of at least 1 min
2.2 Abbreviations:
for the initial peak(s) and to elute the entire sample. The
2.2.1 Acommon abbreviation of hydrocarbon compounds is
programming rate must be sufficiently reproducible to obtain
to designate the number of carbon atoms in the compound. A
retention time repeatability of 0.1 min for each component in
prefix is used to indicate the carbon chain form, while a
the calibration mixture (6.4).
subscripted suffix denotes the number of carbon atoms.
5.1.3 Sample Inlet System—The sample inlet system must
be capable of operating continuously at a temperature equiva-
This test method is under the jurisdiction of ASTM Committe D-2 on
lenttothemaximumcolumntemperatureemployed,orprovide
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
on-column injection with some means of programming the
D02.04.0H on Chromatographic Methods.
entire column, including point of sample introduction up to the
Current edition approved Oct. 26, 1990. Published December 1990. Originally
published as D 3524 – 76. Last previous edition D 3524 – 86.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D3524
maximum temperature required. The sample inlet system must 6.4 Calibration Mixtures—Aminimum of three mixtures of
beconnectedtothechromatographiccolumnsoastoavoidany diesel fuel and lubricating oil (Warning—See Note 5.) of a
cold spots. similar type to that being analyzed are prepared to cover the
5.2 Recorder—A recording potentiometer with a full-scale range from 0 to 12 weight% (mass%) diesel fuel, calculated as
response time of2sor less must be used. If a manual method follows:
of area measurement, such as a planimeter, is employed, the
Diesel fuel, wt% ~mass %!
chart speed must be at least 152 cm/h (60 in./h) to minimize
errors in peak area measurements. This requirement is waived weight ~mass! of fuel
5 3 100
weight ~mass! of fuel and oil
if a ball-and-disc integrator or an electronic integrator is
(1)
employed.
5.3 Column—Any column and conditions may be used,
NOTE 3—Warning: Argon, helium, and nitrogen are compressed gases
provided, under the conditions of the test, separations are in under pressure.
NOTE 4—Warning: Hydrogen is an extremely flammable gas under
order of boiling points and the column resolution, R, is at least
pressure.
3 and not more than 5 (7.1.3). Since a stable baseline is an
NOTE 5—Warning: Combustible liquid.
essential requirement of this method, matching dual columns
are required to compensate for column bleed, which cannot be 6.5 n-Decane, 99 % pure. (Warning—See Note 6.)
eliminated completely by conditioning alone.
NOTE 6—Warning: Combustible, vapor harmful.
5.4 Integrator—Means must be provided for determining
the accumulated area under the chromatogram. This can be 7. Preparation of Apparatus
done manually by means of a polar planimeter. Mechanical
7.1 Column Preparation—Any satisfactory method used in
means, such as the disc integrator, may be used also. However,
the practice of the gas chromatography that will produce a
best precision and automatic operation can be achieved with
column meeting the requirements of 5.3 may be used. The
electronic integration.
column must be conditioned at the maximum operating tem-
5.5 Flow Controllers—Chromatographs using thermal con-
perature until baseline shift due to column bleeding has been
ductivity detectors also must be equipped with constant-flow
reduced to a minimum.
controllers capable of holding carrier gas flow constant to
7.1.1 The column can be conditioned very rapidly and
61 % over the full operating temperature range.
effectively by the following procedure:
5.6 Sample Device:
7.1.1.1 Disconnect the column from the detector.
5.6.1 Micro Syringe—A micro syringe, usually 10 µL, is
7.1.1.2 Purgethecolumnthoroughlyatambienttemperature
used for sample introduction.
with carrier gas.
5.6.2 Automatic sampling devices or other sampling means,
7.1.1.3 Turn off the carrier gas and allow the column to
such as indium encapsulation, may be used, provided the
depressurize completely.
system can be operated at a temperature sufficiently high to
7.1.1.4 Raise the column temperature to the maximum
vaporize completely hydrocarbons with an atmospheric boiling
operating temperature and hold at this temperature for at least
pointof538°C(1000°F),andthesamplingsystemisconnected
1 h with no flow through the column.
to the chro
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