An American National Standard

Designation: D 5483 – 02

Standard Test Method for

Oxidation Induction Time of Lubricating Greases by
Pressure Differential Scanning Calorimetry1
This standard is issued under the fixed designation D 5483; 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
1.1 This test method covers the determination of oxidation
induction time of lubricating greases subjected to oxygen at 3.5
MPa (500 psig) and temperatures between 155 and 210°C.
1.2 The values stated in 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
FIG. 1 PDSC Test Unit
E 473 Terminology Relating to Thermal Analysis2
3. Terminology
at a regulated temperature and pressure until an exothermic
3.1 Definitions of Terms Specific to This Standard: reaction occurs. The extrapolated onset time is measured and
3.1.1 extrapolated onset time, n—a time determined on a reported as the oxidation induction time for the grease under
thermal curve, as the intersection of the extrapolated baseline the specified test temperature.
and a line tangent to the oxidation exotherm constructed at its 4.2 A kinetic equation incorporated with this test method
maximum rate. can estimate oxidation induction times at other temperatures.
3.1.2 oxidation induction time (OIT), n— the period of time
from the first exposure to an oxidizing atmosphere until the 5. Significance and Use
extrapolated onset time. 5.1 Oxidation induction time, as determined under the
3.1.3 pressure differential scanning calorimeter, (PDSC), conditions of this test method, can be used as an indication of
n—a differential scanning calorimeter, as defined in Terminol- oxidation stability.3 This test method can be used for research
ogy E 473, that is capable of maintaining the test sample at a and development, quality control and specification purposes.
controlled, elevated pressure. However, no correlation has been determined between the
3.1.4 thermal curve, n—a graph of sample heat flow versus results of this test method and service performance.
time.
6. Apparatus
4. Summary of Test Method 6.1 Pressure Differential Scanning Calorimeter (PDSC),
4.1 A small quantity of grease is weighed into a sample pan equipped with the following items (See Fig. 1).4
and placed in a test cell. The cell is heated to a specified
temperature and then pressurized with oxygen. The cell is held
3
Rhee, In-Sik, “Development of a New Oxidation Stability Test Method for
Greases Using a Pressure Differential Scanning Calorimeter (PDSC),” NLGI
Spokesman, Vol 55, No. 4, July 1991, pp. 123–132.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on Available from TA Instruments, Inc., 109 Lukens Drive, New Castle, DE
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 19720. At the time that the round robin data for this test method was generated, only
D02.O9.0E on Greases. this company manufactured equipment that met the requirements of 5.1. Subse-
Current edition approved January 10, 2002. Published March 2002. Originally quently, other companies have manufactured equipment meeting these require-
published as D 5483 – 93. Last previous edition D 5483 – 95. ments. Their use is permitted provided their performance is consistent with the
2
Annual Book of ASTM Standards, Vol 14.02. repeatability and reproducibility described in Section 10.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 5483 – 02

FIG. 2 Calibration

the encapsulation press. Place the crimped pan onto the sample
platform in the pressure cell. Seal an empty pan in the same
manner and place it on the reference platform. Set the cell
cover in place and close the cell.
8.1.2 Open the oxygen cylinder valve slightly and set a
pressure of 3.5 6 0.2 MPa (500 6 25 psig) on the cell inlet line
with the pressure regulator. Partially open the inlet valve on the
FIG. 3 Sample Preparation on SFI Pan cell and allow the pressure to slowly build up in the cell. This
should require approximately 2 min. Using the outlet valve,
6.1.1 Sample Enclosure, with capability to 3.5 MPa (500 adjust the oxygen purge rate through the flowmeter to 100 6
psig) at 210°C and pressure gage graduated at intervals of 200 10 mL/min. The open position of these valves should remain
kPa (28.6 psi) or less. fixed during the test.
6.2 Thermal Analyzer. 8.1.3 Set the thermal analyzer to heat from ambient tem-
6.3 Aluminum Sample Solid Fat Index (SFI), pan (see Note perature (approximately 22°C) to 180°C) at a programmed rate
1). of 10°C/min. After completion of the run, measure the melting
6.4 Oxidation Stability Software. (Warning—In addition to temperature of the indium. If the melting temperature differs
other precautions, use stainless steel or copper tubing which is from 157.4 6 0.2°C (see Note 4), correct the difference by
compatible with oxygen, and pressure gages which are desig- using either the hardware or software calibration procedure
nated for use with oxygen.) described in the manufacturer’s instruction manual. If the
6.5 Calibration Software. hardware calibration procedure is used, the temperature cor-
6.6 Flowmeter, with a capacity of at least 200 mL/min. rection should be performed under 3.5 MPa (500 psig) oxygen
6.7 Sample Encapsulation Press. pressure with a 100 mL/min purge rate. A typical melting
calibration curve is shown in Fig. 2.
NOTE 1—It has been found that grease samples can be prepared with
more consistent surface areas using SFI pans as compared to flat bottom NOTE 4—The melting temperature of indium is 156.6°C at atmospheric
pans, resulting in better reproducibility. pressure, but has been found to be elevated to 157.4°C under the
NOTE 2—See Fig. 1 for a diagram of a typical test unit. conditions of this test method, 3.5 MPa (500 psig) of oxygen.5
8.2 Temperature Controller Calibration:
7. Reagents and Materials
8.2.1 Remove both the sample pan and the reference pan
7.1 Oxygen, extra dry, of not less than 99.5 % by volume. from the cell, then close the cell. Slowly pressurize the cell
NOTE 3—Warning: Oxidizer. Gas under pressure. with 3.5 6 0.2 MPa (500 6 25 psig) oxygen and adjust the
purge rate to 100 6 10 mL/min using the cell outlet valve.
7.2 Indium, of not less than 99.9 % by mass.
Select the desired test temperature (either 210, 180, or 155°C).
8. Calibration
8.1 Sample Temperature Calibration:
8.1.1 Weigh approximately 10 mg of indium into an alumi- 5
Supporting data are available from ASTM International Headquarters. Request
num sample pan, insert a lid and crimp the lid to the pan using RR:D02-1007.

2
 D 5483 – 02

FIG. 4 Typical PDSC Thermal Curve

8.2.2 Program the cell to maintain the selected test tempera- dence on one PDSC manufacturer and is not expected to significantly
ture. If, after 10 min, the displayed cell temperature differs by affect the measured OIT since this step precedes the pressurization of the
more than 60.2°C from the selected temperature, slowly adjust test cell with oxygen.
the temperature controller until they agree. After making an 9.6 Open the oxygen valve and slowly pressurize the cell to
adjustment, wait at least 5 min to make certain that the 3.5 6 0.2 MPa (500 6 25 psig). This should require approxi-
temperature is stable before continuing. mately 2 min to reach maximum pressure. The oxidation
8.3 Cell Base Pressure Gage Calibration: induction time is measured from the time when the oxygen
8.3.1 The calibration should be conducted using a calibrated valve is opened.
pressure transducer or a previously calibrated gage according 9.7 As soon as the pressure has equilibrated, check the cell
to the pressure cell manufacturer’s instructions. purge rate and adjust to 100 6 10 mL/min with the outlet
valve.
9. Procedure
9.8 After a duration of 120 min from the time when the
9.1 Before starting a test, the control thermocouple calibra- oxygen valve was opened, close the oxygen valve and slowly
tion shall be conducted at the test temperature (either 210, 180, release the cell pressure by opening the cell pressure release
or 155°C) according to 8.2.1 and 8.2.2. When the test tempera- valve. In the case of a sample for which the approximate
ture is not known, the calibration should be conducted at oxidation induction time is known, the test can be stopped after
210°C. the oxidation exotherm has occurred.
9.2 Weigh 2.0 6 0.1 mg of grease into a sample pan. Spread 9.9 Plot the thermal curve and measure the extrapolated
the sample evenly upon the flat portion. Do not spill any of the onset time for the oxidation exotherm. Report this time, to the
sample into the trough portion of the pan (See Fig. 3). nearest tenth of one minute, as the oxidation induction time for
NOTE 5—Examples of suitable and poor sample on pan patterns are the sample. If more than one oxidation exotherm is observed,
shown in Fig. 3. record the oxidation induction time for the largest exotherm
9.3 Place the uncovered pan containing the sample onto the (See Fig. 4).
platform of the cell according to the PDSC manufacturer’s NOTE 7—A typical thermal curve is shown in Fig. 4.
instructions for placing the sample pan. Place an empty pan of
the same configuration onto the cell platform according to the 9.10 If the induction time is less than 10 min, rerun the test
PDSC manufacturer’s instructions for placing the reference at the next lower temperature, starting at 9.2. Allow the cell to
pan. Close the cell and the pressure release valve. cool to ambient temperature before running the test at the next
9.4 Beginning at ambient temperature (approximately lower temperature.
22°C), program the sample temperature to increase at a rate of 9.11 After the oxidation induction time requirement speci-
100°C/min to the test temperature. fied in 8.10 is satisfied, perform a duplicate test.
9.5 Allow the sample to equilibrate at the test temperature 9.12 If the difference between the two results is greater than
for 2 min. the 95% determinability limit stated in the Precision and Bias
NOTE 6—This step did not appear in the test method which was used in
section of this test method (Section 12), then reject the results
the round robin to generate the precision statement. The round robin test and determine two more oxidation induction times for the
method used the software of a PDSC manufacturer to determine when grease by returning to 9.2. Otherwise, average the oxidation
equilibration at test temperatures occurred. Step 8.5 removes this depen- induction times of both runs.

3
 D 5483 – 02
10. Calculation of Induction Times for Other 12.1.1 Determinability— The difference between the pair of
Temperatures determinations averaged to obtain a test result would, in the
10.1 After an oxidation induction time has been determined long run, in the normal and correct operation of the test
for a particular grease, a value can be estimated for other method, exceed the following value in only one case in twenty:
temperatures using the following equation2: Determinability 5 0.59=m (3)
t 5 A exp ~17 500/T! (1)

where: where:
t = estimated oxidation induction time, min, m = the mean of the two determinations
A = oxidation coefficient of the grease, and 12.1.2 Repeatability— The difference between successive
T = temperature, K (for desired temperature). results (each the mean of a pair of determinations) obtained by
The oxidation coefficient (A) is constant for a given grease the same operator with the same apparatus under constant
and is calculated by (Eq 1) using the oxidation induction time operating conditions on identical material, would in the long
reported in 9.1.2, thus, run, in the normal and correct operation of the test method,
A 5 oxidation induction time/exp~17 500/test temperature, K!. exceed the following value in only one case in twenty:
(2) Repeatability 5 0.42=m (4)
The estimated oxidation induction time can be used as a
guide for choosing appropriate alternative test temperatures for
a grease. The estimated oxidation induction time is not a part where:
m = is the mean of the two results
of the report for this test method.
12.1.3 Reproducibility—The difference between two inde-
11. Report pendent results (each the mean of a pair of determinations)
11.1 Report the following information: obtained by different operators working in different laborato-
11.1.1 Report, to the nearest tenth of one minute, the ries would, in the long run, exceed the following value only
average value calculated in 9.12 as the oxidation induction one case in twenty:
time (OIT) for the sample. Reproducibility 5 0.71=m (5)
11.1.2 Report the test temperature.
where:
12. Precision and Bias 6 m = the mean of the two test results.
12.1 The precision of this test method as determined by the 12.2 Bias—The procedure in this test method has no bias
statistical examination of interlaboratory test results involving because the value of oxidation induction time can be defined
eleven samples, five laboratories, three test temperatures (155, only in terms of a test method.
180, and 210°C), and oxidation induction times of from 9.0 to
45.3 minutes is as follows. 13. Keywords
13.1 differential scanning calorimetry; lubricating grease;
6
Supporting data may be obtained from ASTM Headquarters. Request RR:D02- OIT; onset temperature; oxidation; oxidation coefficient; oxi-
1314. dation induction time; PDSC; thermal analysis

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 D 5483 – 02

APPENDIX

(Nonmandatory Information)

X1. PDSC ROUND ROBIN DATA

X1.1 PDSC Round Robin Data

X1.1.1 See Table X1.1.

NOTE 1—The numbers in this table are the oxidation induction times in minutes. The pairs of oxidation times for each grease represent two single
determinations.
Grease Sample
Lab
A B C D E F G H I J K
1 40.0 13.2 51.3 11.6 15.4 13.7 44.8 16.8 36.2 11.6 30.6
45.3 13.6 48.1 11.3 14.8 16.0 46.8 17.3 31.6 10.3 31.3
2 41.3 15.1 48.8 10.4 15.9 14.0 39.5 17.2 30.5 11.2 31.4
43.4 15.6 48.8 10.1 14.7 13.7 42.2 15.7 29.0 11.6 31.0
3 44.9 15.5 48.6 9.6 15.9 11.4 44.0 14.6 32.8 10.6 30.8
41.9 17.2 47.4 9.2 13.9 13.5 43.0 14.9 24.0 9.0 31.2
4 42.4 15.5 48.8 10.2 14.9 13.6 42.7 16.5 28.8 10.7 33.9
43.8 15.5 48.7 10.5 15.2 13.3 43.0 16.9 28.9 11.1 34.5
5 39.8 13.6 50.1 10.9 17.5 13.0 47.4 16.1 12.9 10.3 28.6
42.5 13.3 49.7 11.3 15.5 13.9 45.0 14.6 10.5 10.1 28.7
Test temperature, °C 210 210 210 210 210 210 180 180 210 210 155

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