An American National Standard

Designation: D 942 – 02

Designation: 142/85 (92)

Standard Test Method for

Oxidation Stability of Lubricating Greases by the Oxygen
Pressure Vessel Method1
This standard is issued under the fixed designation D 942; 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.

This test method has been approved by the sponsoring committee and accepted by the cooperating societies in accordance with the
established procedures.

This standard has been approved for use by agencies of the Department of Defense.

1. Scope * 3. Summary of Test Method

1.1 This test method determines resistance of lubricating 3.1 The sample of grease is oxidized in a pressure vessel
greases to oxidation when stored statically in an oxygen heated to 99°C (210°F) and filled with oxygen at 110 psi (758
atmosphere in a sealed system at an elevated temperature under kPa). Pressure is observed and recorded at stated intervals. The
conditions of test. degree of oxidation after a given period of time is determined
1.2 This standard does not purport to address all of the by the corresponding decrease in oxygen pressure.
safety concerns, if any, associated with its use. It is the
NOTE 1—The pressure vessel has been referred to as “a bomb” in
responsibility of the user of this standard to establish appro- previous issues of this test method.
priate safety and health practices and determine the applica- NOTE 2—The accepted unit of pressure is the pascal (Pa) for ASTM
bility of regulatory limitations prior to use. For specific hazard methods and will be parenthetically included after the conventional
statements see Sections 6 and 7. pound-force per square inch (psi) value. The Institute of Petroleum uses
the bar as a pressure measurement. Conversion of units may be obtained
2. Referenced Documents as follows:
To convert from pound-force per square inch (psi) to pascal (Pa)
2.1 ASTM Standards: multiply by 6.894757 3 103.
A 240 Specification for Heat-Resisting Chromium and To convert from pound-force per square inch (psi) to bar multiply by
Chromium-Nickel Stainless Steel Plate, Sheet, and Strip 0.06894757.
for Pressure Vessels2 To convert from bar to pascal (Pa) multiply by 105.
D 525 Test Method for Oxidation Stability of Gasoline
(Induction Period Method)3 4. Significance and Use
E 1 Specification for ASTM Thermometers4 4.1 This test method measures the net change in pressure
2.2 Other Standards: resulting from consumption of oxygen by oxidation and gain in
IP Specification for Standard IP Thermometers5 pressure due to formation of volatile oxidation by-products.
BS 970:1983 Part I, Section S6 This test method may be used for quality control to indicate
batch-to-batch uniformity. It predicts neither the stability of
greases under dynamic service conditions, nor the stability of
1
This test method is under the jurisdiction of ASTM Committee D02 on greases stored in containers for long periods, nor the stability
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.09 on Oxidation. of films of greases on bearings and motor-parts. It should not
In the IP, this test method is under the jurisdiction of the Standardization be used to estimate the relative oxidation resistance of different
Committee. grease types.
Current edition approved June 10, 2002. Published September 2002. Originally
published as D 942–47. Last previous edition D 942–90(1995)e1. 5. Apparatus
2
Annual Book of ASTM Standards, Vol 01.03.
3
Annual Book of ASTM Standards, Vol 05.01. 5.1 Oxidation Pressure Vessel, Sample Dish, Dish Holder,
4
Annual Book of ASTM Standards, Vol 14.03. Pressure Gage and Oil Bath as described in detail in the
5
Available from The Institute of Petroleum, 61 New Cavendish St., London
W1M, 8AR, England.
Annex.
6
Available from British Standards Institute, 2 Park St., London, England
WIA2B5.

*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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 D 942 – 02
NOTE 3—Other constant-temperature baths may be used if they are function as an alternate to the preferred procedure, cleaning
equivalent in heat capacity and thermal gradient characteristics to the oil with detergent solutions.
bath described in the Annex and can be shown to maintain the pressure
vessel at the prescribed test temperature.
7. Preparation of Apparatus
5.2 Thermometer, having a range as shown below and 7.1 Clean the sample dishes from all contamination from
conforming to the requirements as prescribed in Specification previous runs and from dust settling from the air by washing
E 1 or in the Specifications for IP Standard Thermometers: them with n-heptane and then with a cleaning solution. Follow
Thermometer Number the final cleaning operation by a thorough tap water rinse, a
Temperature Range ASTM IP
95 to 103°C 22C 24C distilled water rinse, and drying in an oven. Handle the clean
204 to 218°F 22F 24F dishes only with forceps. (Warning—Handle in well-
ventilated area, preferably in a hood. Keep away from heat,
6. Material sparks, and open flame. Keep container closed when not in
6.1 Oxygen, of not less than 99.5 % purity. use.) (Warning—See 6.3, and avoid skin contact, which may
6.2 (Warning—Since oxygen vigorously accelerates com- cause severe burns.)
bustion, observe the following procedures: (1) Keep oil and 7.2 If lacquer is found after a run, clean the inside of the
grease away from oxygen at high pressure. Keep oil and grease oxidation pressure vessel and the metal supports for the
away from all regulators, gages and control equipment. (2) Use pressure vessel dishes by immersing in an appropriate solvent
oxygen only with equipment conditioned for oxygen service by capable of removing the lacquer, such as gum solvent as
careful cleaning to remove oil and grease from area in contact specified in Test Method D 525, and scrubbing with a bristle
with high pressure oxygen. (3) Keep combustibles away from brush followed by drying. Scrub further with water and a fine
oxygen and eliminate ignition sources. (4) Keep surfaces clean scouring powder until all the lacquer deposits are removed.
to prevent ignition or explosion, or both, upon contact with Follow the scouring operation by a thorough tap water rinse, a
high pressure oxygen. (5) Always use a pressure regulator to distilled water rinse, and drying in an oven. Handle the clean
deliver oxygen. Release regulator tension before opening metal supports only with forceps.
oxygen cylinder. (6) All equipment used must be suitable and
recommended for oxygen service. (7) Never attempt to transfer 8. Procedure
oxygen from cylinder in which it is received to any other 8.1 Fill each of the five dishes with 4.00 6 0.01 g of grease.
cylinder prior to use. (8) Do not drop oxygen cylinders. (9) Distribute the samples in the dishes in a uniform layer with a
Keep cylinder valve closed when not in use. (10) Stand away smooth level upper surface. Place the filled dishes on the five
from valve when opening cylinder. (11) Do not breathe or use bottom shelves of the holder, leaving the top shelf to act as a
technical grade oxygen for inhalation purposes. (12) See cover to prevent condensing volatile products from dropping
Compressed Gas Association Booklets G-4 and G-4-17 for into the grease samples. When assembling the pressure vessel,
details of safe practice in the use of oxygen.) place a small ball of glass wool in the bottom of the stem.
6.3 n-Heptane—(Warning—Flammable. Harmful if in- 8.2 Place the dish holder in the pressure vessel with a
haled. Keep away from heat, sparks, and open flame. Keep sealing gasket in place, and close the pressure vessel by
container closed. Use with adequate ventilation. Avoid breath- tightening the bolts slowly and uniformly. Clear the air from
ing vapor or spray mist. Avoid prolonged or repeated contact the pressure vessel by introducing oxygen slowly until a
with skin.) pressure of 100 psi (689 kPa) is attained, then allow the oxygen
6.4 Cleaning Solution, capable of satisfactorily cleaning the to escape slowly; repeat four times. Bring the oxygen pressure
glassware used in the test. The criterion for satisfactory to a value as shown in the following table:
cleaning shall be a matching of the quality of that obtained with Room Temperature Pressure
chromic acid cleaning solutions (fresh chromic acid, 6-h °C °F psi kPa
soaking period, rinsing with distilled water and drying) or 17 to 20 62 to 68 85 586
20 to 23 68 to 74 86 593
some other equivalently strong oxidizing non-chromium con- 23 to 27 74 to 80 87 600
taining acid cleaning solutions on used sample dishes. 27 to 30 80 to 86 88 607
(Warning—Causes severe burns. A recognized carcinogen. 30 to 33 86 to 92 89 614
33 to 37 92 to 98 90 621
Strong oxidizer; contact with organic material may cause fire. 37 to 40 98 to 104 91 627
Hygroscopic.) (Warning—Do not get in eyes, on skin, or on
clothing. Avoid breathing vapor or mist. Keep container closed. Allow the pressure vessel to stand overnight to make sure
Use with adequate ventilation. Do not take internally.) For this there are no leaks.
comparison, visual appearance and mass loss on heating the NOTE 4—It has been found that pressure readings as shown above will
glassware under test conditions may be used. Detergent clean- result in a pressure reading of 110 6 2 psi (758 6 14 kPa) when the
ing avoids the potential hazards and inconveniences related to pressure vessel is placed in the bath in the following step, 8.3, and
handling corrosive chromic acid solutions; this procedure consequently no release of oxygen will be required in most cases. This
minimizes the chance of a leak developing at the valve after the overnight
remains the reference cleaning practice and as such may
check for leaks has shown the pressure vessel to be satisfactory.
8.3 Place the pressure vessel in the oil bath maintained at a
7
Available from Compressed Gas Association, 500 Fifth Ave., New York, NY temperature of 99 6 0.5°C (210 6 1.0°F). As the pressure
10036. rises, if needed, intermittently release oxygen from the pressure

2
 D 942 – 02
vessel until a constant pressure of 110 6 2 psi (758 6 14 kPa) 10.2 The following information on the precision of this test
is obtained and maintained for at least 2 h. A gradual drop in method has been developed by the Institute of Petroleum
pressure indicates a continuous leak in the pressure vessel. (London). The precision of this test method as determined by
Observe and record the pressure at least every 24 h. In case a statistical examination of interlaboratory results is as follows:
leak develops, do not report the results but repeat the test. 10.2.1 Repeatability—The difference between two test re-
8.4 Start timing at the moment of immersion of the pressure sults, obtained by the same operator with the same apparatus
vessel in the oil bath, and continue the oxidation for the time under constant operating conditions on identical test material
period specified. would, in the long run, in the normal and correct operation of
the test method, exceed the following values only in one case
NOTE 5—Specifications are usually given in terms of pressure drop in
pounds per square inch, or kilopascals at one or more time intervals, for in twenty:
instance, after 100, 200 h, and so forth. Mean Pressure Mean Pressure
Repeatability Repeatability
Drop, psig Drop, kPa
0 to 2 1 0 5
9. Report 3 to 6 2 5 to 20 10
9.1 Report the average of duplicate determinations as pres- 7 to 10 3 25 to 40 15
11 to 14 4 45 to 60 20
sure drop in pounds per square inch, or kilopascals for the 15 to 18 5 65 to 85 25
specified test time, or times in hours, according to Test Method 19 to 20 6 90 to 105 30
D 942. 110 to 125 35
130 to 140 40

10. Precision and Bias

10.2.2 Reproducibility—The difference between two single
10.1 The precision of this test method as determined by and independent results obtained by different operators work-
statistical examination of interlaboratory results is as follows: ing in different laboratories on identical test material would, in
10.1.1 Repeatability—The difference between two test re- the long run, in the normal and correct operation of the test
sults, obtained by the same operator with the same apparatus method, exceed the following values only in one case in
under constant operating conditions on identical test material twenty:
would, in the long run, in the normal and correct operation of Mean Pressure Reproduci- Mean Pressure Reproduci-
the test method, exceed the following values only in one case Drop, psig bility Drop, kPa bility
in twenty: 0 to 3 2 0 10
4 to 6 3 5 to 20 15
Mean Pressure Drop, psi (kPa) Repeatability 7 to 9 4 25 to 35 20
0 to 5 (34.5) 2 (13.8) 10 to 12 5 40 to 50 25
Over 5 to 10 (34.5 to 68.9) 3 (20.7) 13 to 15 6 55 to 65 30
Over 10 to 20 (68.9 to 138) 6 (41.4) 16 to 17 7 70 to 80 35
Over 20 to 55 (138 to 379) 10 (68.9) 18 to 20 8 85 to 95 40
100 to 110 45
10.1.2 Reproducibility—The difference between two single 115 to 125 50
and independent results obtained by different operators work- 130 to 135 55
ing in different laboratories on identical test material would, in 140 60
the long run, in the normal and correct operation of the test These precision values have been obtained by statistical
method, exceed the following values only in one case in examination of interlaboratory test results,8 and were first
twenty: published in 1965.
Mean Pressure Drop, psi (kPa) Reproducibility 10.3 Bias—The procedure in this test method has no bias
0 to 5 (34.5) 3 (20.7)
Over 5 to 10 (34.5 to 68.9) 5 (34.5)
because the value of oxidation stability can be defined only in
Over 10 to 20 (68.9 to 138) 8 (55.2) terms of a test method.
Over 20 to 55 (138 to 379) 20 (138)
11. Keywords
NOTE 6—These precision values apply only to that portion of the data
for which oxygen is absorbed at a rate approximately proportional to time 11.1 grease; oxidation
(for example, the induction period). The end of the induction period is
evidenced by a rapid acceleration in the rate of oxygen absorption in a
8
short time interval. See IP Standards for Petroleum and Its Products, Part 1, Appendix E.

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 D 942 – 02
ANNEX

(Mandatory Information)

A1. APPARATUS

A1.1 Oxidation Pressure Vessel, of the type and conforming (210°F) and provided with a lead or TFE-fluorocarbon gasket
to the dimensions shown in Fig. A1.1, shall be made of 18 % for sealing. To facilitate cleaning, give a high polish to the
chromium, 8 % nickel alloy steel. A suitable material is an interior surfaces of the pressure vessel, the lid, and the inside
alloy steel conforming to Grade S, Type 304, of Specifications of the pipe carrying the pressure gage. The pressure vessel shall
A 240 or BS 970: 1983 Part 1, Section S (steel 302S31 or be so constructed that its volume without the dish holder and
321S31). The pressure vessel shall be capable of withstanding dishes is 185 6 6 mL, measured to the level of the gage. This
with safety a working pressure of 180 psi (1241 kPa) at 99°C may be checked by assembling the pressure vessel, removing

NOTE—All dimensions are in inches (millimetres).

FIG. A1.1 Apparatus for Oxidation Stability Test of Lubricating Greases

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 D 942 – 02
the gage, and measuring the amount of liquid required to fill submersion of the pressure vessel to the proper depth. Circu-
the pressure vessel to the level of the gage connection. A lation of the oil heating medium by a pump or stirring is
screw-on lid may be used instead of the bolt-on lid shown in recommended. Sufficient heat capacity shall be provided to
Fig. A1.1. return the bath to the required temperature within 60 min after
immersion of the pressure vessel. Provide the bath with a
A1.2 Pressure Gage, suitable for use with oxygen and thermometer well such that the 96.8°C (206°F) point of the
mineral oil, shall be of the indicating type, graduated in thermometer is at the same level as the upper surface of the
intervals of 1 psi (6.89 kPa) per scale division, with a bath cover. Adjust the level of the bath so that the top of the
maximum reading of at least 120 psi (827 kPa) and capable of pressure vessel is submerged approximately 50 mm below its
an accuracy of at least 0.5 psi (3.45 kPa), within the interval 90 surface. Arrange the bath so that there are no drafts or wide
to 120 psi (621 to 827 kPa). Attach the gage to the stem as fluctuations in temperature around the gages.
shown in Fig. A1.1. A recording pressure gage may be used in
place of the prescribed indicating pressure gage if it satisfies A1.4 Dish Holder, constructed of 18 % chromium, 8 %
the volume and accuracy requirements previously stated. nickel alloy steel as described for the oxidation pressure vessel,
shall conform to the dimensions prescribed in Fig. A1.1.
A1.3 Oil Bath, capable of being controlled at 99 6 0.5°C
(2106 1°F), with a temperature gradient less than 1°F (0.5°C) A1.5 Sample Dishes, of glass conforming to the dimensions
in the body of the oil used, and of sufficient depth to allow prescribed in Fig. A1.1.

SUMMARY OF CHANGES

Subcommittee D02.09 has identified the location of selected changes to this standard since the last issue
(D 942–02) that may impact the use of this standard.

(1) Changed the document list and cleaning procedure. (3) Replaced the word “bomb” with “pressure vessel”
(2) Changed the instructions in Paragraph 8.2. throughout.

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