ASTM D5483-21

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Designation: D5483 − 20 D5483 − 21
Standard Test Method for
Oxidation Induction Time of Lubricating Greases by
Pressure Differential Scanning Calorimetry
This standard is issued under the fixed designation D5483; 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*
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 °C and 210 °C.
1.2 Warning—The original data published in Research Report RR:D02-1314, was not analyzed in accordance the current D2PP.
It also used instruments which are no longer manufactured and in a check of currently used instruments, none of the original
instruments were still in use. The new precision of this test method is still to be established.
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
E697 Practice for Use of Electron-Capture Detectors in Gas Chromatography
E1858 Test Methods for Determining Oxidation Induction Time of Hydrocarbons by Differential Scanning Calorimetry
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 extrapolated onset time, n—a time determined on a thermal curve, as the intersection of the extrapolated baseline and a line
tangent to the oxidation exotherm constructed at its maximum rate.
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
D02.09.0E on Oxidation of Greases.
Current edition approved Jan. 1, 2020Dec. 1, 2021. Published February 2020January 2022. Originally approved in 1993. Last previous edition approved in 20152020 as
D5483 – 05 (2015).D5483 – 20. DOI: 10.1520/D5483-20.10.1520/D5483-21.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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3.1.2 oxidation induction time (OIT), n—the period of time from the first exposure to an oxidizing atmosphere until the
extrapolated onset time.
3.1.3 thermal curve, n—a graph of sample heat flow versus time.
4. Summary of Test Method
4.1 A small quantity of grease is weighed into a sample pan and placed in a test cell. The cell is heated to a specified temperature
and then pressurized with oxygen. The cell is held at a regulated temperature and pressure until an exothermic reaction occurs. The
extrapolated onset time is measured and reported as the oxidation induction time for the grease under the specified test temperature.
5. Significance and Use
5.1 Oxidation induction time, as determined under the conditions of this test method, can be used as an indication of oxidation
stability. This test method can be used for research and development, quality control and specification purposes. However, no
correlation has been determined between the results of this test method and service performance.
6. Apparatus
6.1 Pressure Differential Scanning Calorimeter (PDSC), the essential instrumentation required to provide the minimum
differential scanning calorimetric capability for these test methods include:
6.1.1 Pressure System, consisting of:
6.1.1.1 Pressure Vessel, or similar means of sealing the test chamber at any applied oxygen pressure within the pressure limits of
these test methods.
6.1.1.2 Temperature Sensor, to provide an indication of the specimen/furnace temperature to 60.4 °C.
6.1.1.3 Differential Sensors, to detect a heat flow difference between specimen and reference with a sensitivity of 5 μW.
6.1.1.4 Pressure Transducer, or similar device to measure the pressure inside the test chamber to 60.2 MPa, including any
temperature dependence of the transducer.
6.1.1.5 A source of pressurized oxygen or air capable of sustaining a regulated gas pressure in the test chamber of up to 3.5 MPa.
6.1.1.6 A means of sustaining a Test Chamber Environment of a purge gas of 50 mL/min within 5 %.
6.1.2 Temperature Controller, capable of executing a specific temperature program by operating the furnace(s) between selected
temperature limits at a rate of temperature change of 40 °C ⁄min constant to 1 % and an isothermal temperature constant to 60.4 °C
6.1.3 Data Collection Device, to provide a means of acquiring, storing, and displaying measured or calculated signals, or both.
The minimum output signals required for DSC are heat flow, temperature and time.
NOTE 1—At the time that the original round robin data for this test method was generated, only DuPont Instruments (now TA instruments) manufactured
equipment that met the requirements of 6.1. Subsequently, other companies have manufactured equipment meeting these requirements. Their use is
permitted provided their performance is consistent with the repeatability and reproducibility described in Section 11.
NOTE 2—The link between the test chamber and the pressure transducer should allow for fast pressure equilibrium to ensure accurate recording of the
pressure above the specimen during testing.
NOTE 3—The capability to record the first derivative of the heat flow curve will be helpful in cases where the baseline is not constant.
6.2 Flow Meter, capable of reading 200 mL ⁄min or another selected flow rate, accurate to within 65 %. Ensure the flowmeter is
calibrated.
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.
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FIG. 1 Calibration
6.3 Analytical Balance, with a capacity of at least 100 mg and capable of weighing to the nearest 0.01 mg or less than 1 % of
the specimen mass.
7. Reagents and Materials
7.1 Oxygen, extra dry, of not less than 99.5 % purity by volume. (Warning—Oxidizer. Gas under pressure. In addition to other
precautions, use stainless steel or copper tubing which is compatible with oxygen, and pressure gauges which are designated for
use with oxygen.)
7.2 Indium, of not less than 99.9 % purity by mass.
8. Calibration
8.1 Sample Temperature Calibration:
8.1.1 Weigh approximately 10 mg of indium into an aluminum sample pan, insert a lid and crimp the lid to the pan using 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 MPa 6 0.2 MPa (500 psig 6 25 psig) on the cell inlet line
with the pressure regulator. Partially open the inlet valve on the cell and allow the pressure to slowly build up in the cell. This
should require approximately 2 min. Using the outlet valve, adjust the oxygen purge rate through the flowmeter to 100 mL ⁄min
6 10 mL ⁄min. The open position of these valves should remain fixed during the test.
8.1.3 Set the thermal analyzer to heat from ambient temperature (approximately 22 °C) to 180 °C) at a programmed rate of
10 °C ⁄min. After completion of the run, measure the melting temperature of the indium. If the melting temperature differs from
157.4 °C 6 0.2 °C (see Note 4), correct the difference by using either the hardware or software calibration procedure described
in the manufacturer’s instruction manual. If the hardware calibration procedure is used, the temperature correction should be
performed under 3.5 MPa (500 psig) oxygen pressure with a 100 mL ⁄min purge rate. A typical melting calibration curve is shown
in Fig. 1.
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FIG. 2 Sample Preparation on SFI Pan
NOTE 4—The melting temperature of indium
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