ASTM D6186-08(2013)
(Test Method)Standard Test Method for Oxidation Induction Time of Lubricating Oils by Pressure Differential Scanning Calorimetry (PDSC)
Standard Test Method for Oxidation Induction Time of Lubricating Oils by Pressure Differential Scanning Calorimetry (PDSC)
SIGNIFICANCE AND USE
4.1 Oxidation induction time, as determined under the conditions of this test method, may be used as an indication of oxidation stability.2 This test method is faster than other oil oxidation tests and requires a very small amount of sample. It may be used for research and development, quality control, and specification purposes. However, no correlation has been established between the results of this test method and service performance.
SCOPE
1.1 This test method covers the determination of oxidation induction time of lubricating oils subjected to oxygen at 3.5 MPa (500 psig) and temperatures between 130 and 210°C.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.2.1 Exception—Pressure measurement appears in MPa with psig provided in parentheses for information only.
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.
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Designation: D6186 − 08 (Reapproved 2013)
Standard Test Method for
Oxidation Induction Time of Lubricating Oils by Pressure
1
Differential Scanning Calorimetry (PDSC)
This standard is issued under the fixed designation D6186; 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 reported as the oxidation induction time for the lubricating oil
at the specified test temperature.
1.1 This test method covers the determination of oxidation
induction time of lubricating oils subjected to oxygen at 3.5
4. Significance and Use
MPa (500 psig) and temperatures between 130 and 210°C.
4.1 Oxidation induction time, as determined under the
1.2 The values stated in SI units are to be regarded as
conditions of this test method, may be used as an indication of
standard. No other units of measurement are included in this
2
oxidation stability. This test method is faster than other oil
standard.
oxidation tests and requires a very small amount of sample. It
1.2.1 Exception—Pressure measurement appears in MPa
maybeusedforresearchanddevelopment,qualitycontrol,and
with psig provided in parentheses for information only.
specification purposes. However, no correlation has been
1.3 This standard does not purport to address all of the
established between the results of this test method and service
safety concerns, if any, associated with its use. It is the
performance.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
5. Apparatus
bility of regulatory limitations prior to use.
5.1 Pressure Differential Scanning Calorimeter (PDSC),
equipped with the following items:
2. Terminology
5.1.1 Sample Enclosure, with capability to 3.5 6 0.2 MPa
2.1 Definitions of Terms Specific to This Standard:
(500 6 25 psig) at 210°C and pressure gauge graduated at
2.1.1 extrapolated onset time, n—a time determined on a
intervals of 200 KPa (28.6 psig) or less.
thermal curve, as the intersection of the extrapolated baseline
5.1.2 Thermal Analyzer.
and a line tangent to the oxidation exotherm constructed at its
5.1.3 Aluminum Solid Fat Index (SFI) Sample Pan—See
maximum rate.
Note 1.
2.1.2 oxidation induction time, (OIT), n— a period of time
5.1.4 Oxidation Stability Software.
during which the oxidation rate accelerates from zero to a
5.1.5 Calibration Software.
maximum and which corresponds to the extrapolated onset
5.1.6 Calibrated Flowmeter, with a capacity of at least 200
time.
mL/min and graduated in intervals of 5 mL or less.
5.1.7 Sample Encapsulation Press.
2.1.3 thermal curve, n—a graph of sample heat flow versus
time.
NOTE 1—It has been found that when oil samples are prepared with SFI
pans which have more consistent surface areas than standard flat bottom
3. Summary of Test Method
pans, reproducibility is improved.
NOTE 2—Stainless steel or copper tubing is compatible with oxygen.
3.1 Asmall quantity of oil is weighed into a sample pan and
NOTE 3—See Fig. 1 for a diagram of a typical test unit.
placed in a test cell. The cell is heated to a specified
temperature and then pressurized with oxygen. The cell is held
6. Reagents and Materials
at a regulated temperature and pressure until an exothermic
6.1 Oxygen, a minimum purity of 99.5 % oxygen by vol-
reaction occurs. The extrapolated onset time is measured and
ume. (Warning—Oxidizer. Gas under pressure. )
6.2 Indium, of not less than 99.9 % indium by mass.
1
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 D02.09.0D on Oxidation of Lubricants.
2
Current edition approved Dec. 1, 2013. Published December 2013. Originally Rhee, In-Sik, “Development of New Oxidation Stability Test Method for
approved in 1997. Last previous edition approved in 2008 as D6186 – 08. DOI: Lubricating Oils Using a Pressure Differential Scanning Calorimeter (PDSC),”
10.1520/D6186-08R13. NLGI Spokesman, Vol 65, No. 3, June 2001, pp. 16–23.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D6186 − 08 (2013)
FIG. 1 PDSC Test Unit
7. Calibration
FIG. 2 Calibration Curve for PDSC
7.1 Sample Temperature Calibration:
7.1.1 Weigh approximately 10 mg of indium into an alumi-
num sample pan, insert a lid and crimp the lid to the pan using
ment does not have this function, the control calibration shall
the encapsulation press. Place the crimped pan onto the sample
be followed according to the equipment manufacturer’s
...
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