ASTM D3525-93(1997)
(Test Method)Standard Test Method for Gasoline Diluent in Used Gasoline Engine Oils by Gas Chromatography
Standard Test Method for Gasoline Diluent in Used Gasoline Engine Oils by Gas Chromatography
SCOPE
1.1 This test method utilizes gas chromatography to determine the amount of dilution in used gasoline fuel engine oils.
1.2 This test method is limited to gas chromatographs equipped with flame ionization detector and programmable oven. Note 1-The use of other detectors and instrumentation has been reported. However, the precision statement applies only when the instrumentation specified is employed.
1.3 The applicability of this method to gelled used engine oils has not been adequately investigated to ensure compliance with the indicated repeatability and reproducibility. Gelled oils are defined as oils that develop structure on standing, but that return to their original fluidity with light agitation.
1.4 The values stated in SI units are to be regarded as the standard. Inch-pound units are provided for information only.
1.5 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.
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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.
Designation: D 3525 – 93 (Reapproved 1997)
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Gasoline Diluent in Used Gasoline Engine Oils by Gas
Chromatography
This standard is issued under the fixed designation D 3525; 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
3. Summary of Test Method
1.1 This test method utilizes gas chromatography to
3.1 Gas chromatographic techniques are used with the
determine the amount of dilution in used gasoline fuel engine
sample, containing a known percentage of n-tetradecane as an
oils.
internal standard, to determine the weight percent of the
1.2 This test method is limited to gas chromatographs
sample boiling below the boiling point of the internal standard.
equipped with flame ionization detector and programmable
oven.
4. Significance and Use
NOTE 1—The use of other detectors and instrumentation has been
4.1 Some fuel dilution of the engine oil may take place
reported. However, the precision statement applies only when the
during normal operation. However, excessive fuel dilution is of
instrumentation specified is employed.
concern in terms of possible performance problems.
1.3 The applicability of this method to gelled used engine
oils has not been adequately investigated to ensure compliance
5. Apparatus
with the indicated repeatability and reproducibility. Gelled oils
5.1 Gas Chromatograph—Any gas chromatograph may be
are defined as oils that develop structure on standing, but that
used that has the following performance characteristics:
return to their original fluidity with light agitation.
5.1.1 Detector—Only a flame detector can be used in this
1.4 The values stated in SI units are to be regarded as the
method. The detector must have sufficient sensitivity to detect
standard. Inch-pound units are provided for information only.
1.0 % n-tetradecane with a peak height of at least 40 % of full
1.5 This standard does not purport to address all of the
scale on the recorder under the conditions prescribed in this
safety concerns, if any, associated with its use. It is the
method, and without loss of resolution. The detector must be
responsibility of the user of this standard to establish
capable of operating continuously at a temperature equivalent
appropriate safety and health practices and determine the
to the maximum column temperature employed, and it must be
applicability of regulatory limitations prior to use.
connected to the column so as to avoid any cold spots. When
operating at this sensitivity level, detector stability must be
2. Terminology
such that the baseline drift of not more than 1 % per hour is
2.1 Definitions of Terms Specific to This Standard:
obtained.
2.1.1 fuel dilution—the amount, expressed as a percentage,
5.1.2 Column Temperature Programmer—The
of engine fuel found in engine lubricating oil. This may be the
chromatograph must be capable of temperature program
result of engine wear or improper performance.
operation over a range sufficient to establish a retention time of
2.2 Abbreviations:
0.25 min (15 s) for the initial peak and to elute the internal
2.2.1 A common abreviation of hydrocarbon compounds is
standard totally. For determination of fuel dilution the
to designate the number of carbon atoms in the compound. A
reproducibility of the programming rate is not significant,
prefix is used to indicate the carbon chain form, while a
although a retention time repeatability of 0.3 min (18 s) should
subscripted suffix denotes the number of carbon atoms.
be available.
Example:
5.1.3 Sample Inlet System—The sample inlet system must
normal decane n-C
be capable of operating continuously at a temperature
iso-tetradecane i-C
equivalent to the maximum column temperature employed.
The sample inlet system must be connected to the
chromatograph column so as to avoid any cold spot.
5.2 Recorder—A recording potentiometer with a full-scale
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee response time of1sor less can be used.
D02.04.0Hon Chromatographic Methods.
5.3 Column—Any column and conditions may be used,
Current edition approved Aug. 15, 1993. Published October 1993. Originally
provided, under the conditions of the test, separations are in
published as D 3525 – 76. Last previous edition D 3525 – 90.
NOTICE:¬This¬standard¬has¬either¬been¬superceded¬and¬replaced¬by¬a¬new¬version¬or¬discontinued.¬
Contact¬ASTM¬International¬(www.astm.org)¬for¬the¬latest¬information.¬
D 3525
order of boiling points and the column resolution, R, is at least meeting the requirements of 4.3 may be used. The column must
3 and not more than 8. Since a stable baseline is an essential be conditioned at the maximum operating temperature until
requirement of this method, electronic single column baseline drift due to column bleeding has been reduced to less
compensation is required to compensate for column bleed, than 1 % per hour.
which cannot be eliminated completely by conditioning alone.
NOTE 8—Difficulty in achieving the baseline drift requirement may
5.4 Means must be provided for measuring the accumulated
indicate injection port or column overloading from contamination.
area under the chromatogram. This can be done by a computer
Remove and clean the injection port. Reassemble and increase the
or electronic integrator. The computer or integrator must have temperature of the injection port, column oven, and detector to the
maximum limits of the gas chromatographic column employed.
the capability of subtracting an area profile obtained in a blank
run from the corresponding area profile obtained during a
7.1.1 To test column resolution prepare a mixture of 1
sample run.
volume % each of C and C normal paraffins in a suitable
14 16
solvent such as octane (Warning—C and C n-paraffins, see
14 16
NOTE 2—Some commercially available gas chromatographs permit the
Note 4) (Warning—n-octane, see Note 5). Inject the same
storing of data as a baseline profile of a blank run (without sample
injection). With such instruments, sample run data can be corrected for volume of this mixture as to be used in analysis of samples and
baseline drift through subtraction of the internally stored baseline profile
obtain the chromatogram by the procedure described below.
data from the sample run profile data. With this feature, further baseline
Calculate the resolution, R, from the distance between C and
correction need not be required.
C normal paraffin peaks at the peak maxima, d, and the width
5.5 Flow Controllers—Control of baseline drift to not more
of the peaks at the baseline, Y and Y , as follows:
1 2
than 1 % of full scale per hour as covered in 5.1.1 will require
R 5 @2~d 2 d !#/~Y 1 Y ! (1)
1 2 1 2
that the gas chromatograph be equipped with constant-flow
Resolution, R, using the above equation, must be at least 3
controllers.
and not more than 8.
5.6 Sample Introduction Apparatus—The sample is
7.2 Chromatograph and Related Equipment—Place in
introduced by use of a micro syringe, automatic sampling
service in accordance with manufacturer’s instructions. Typical
device
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.