Designation: D972 − 16

Standard Test Method for

Evaporation Loss of Lubricating Greases and Oils1
This standard is issued under the fixed designation D972; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope* 3.1.1.1 Discussion—The dispersion of the thickener forms a

1.1 This test method covers the determination of the loss in two-phase system and immobilizes the liquid lubricant by
mass by evaporation of lubricating greases and oils for surface tension and other physical forces. Other ingredients are
applications where evaporation loss is a factor. Evaporation commonly D217 included to impart special properties.
loss data can be obtained at any temperature in the range from 3.1.2 thickener, n—in lubricating grease, a substance com-
100 °C to 150 °C (210 °F to 300 °F). posed of finely divided particles dispersed in a liquid to form
the product’s structure.
1.2 The values stated in SI units are to be regarded as
3.1.2.1 Discussion—Thickeners can be fibers (such as vari-
standard.
ous metallic soaps) or plates or spheres (such as certain
1.2.1 Exception—The values given in parentheses are for
non-soap thickeners), which are insoluble or, at most, only very
information only.
slightly soluble in the liquid lubricant. The general require-
1.3 This standard does not purport to address all of the ments are that the solid particles are extremely small, uni-
safety concerns, if any, associated with its use. It is the formly dispersed, and capable of forming a relatively stable,
responsibility of the user of this standard to establish appro- gel-like structure with the D217 liquid lubricant.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 4. Summary of Test Method
4.1 The weighed sample of lubricant in an evaporation cell
2. Referenced Documents is placed in a bath maintained at the desired test temperature.
2.1 ASTM Standards:2 Heated air is passed over its surface for 22 h. The evaporation
A240/A240M Specification for Chromium and Chromium- loss is calculated from the loss in mass of the sample.
Nickel Stainless Steel Plate, Sheet, and Strip for Pressure
Vessels and for General Applications 5. Significance and Use
D217 Test Methods for Cone Penetration of Lubricating 5.1 The loss of volatile materials from greases and oils can
Grease adversely effect the original performance characteristics of a
D2595 Test Method for Evaporation Loss of Lubricating lubricant and therefore could be a significant factor in evalu-
Greases Over Wide-Temperature Range ating a lubricant for a specific use. Such volatiles can also be
E2251 Specification for Liquid-in-Glass ASTM Thermom- considered contaminants in the environment in which the
eters with Low-Hazard Precision Liquids lubricant is to be used. Correlation between results from this
test method and service performance has not been established.
3. Terminology
5.2 The test can be run at any agreed upon temperature
3.1 Definitions: between 100 °C and 150 °C (210 °F to 300 °F).
3.1.1 lubricating grease, n—a semi-fluid to solid product of
NOTE 1—The specified flow of air, 2.58 g ⁄ min 6 0.02 g ⁄ min, (2 L ⁄ min
a thickener in a liquid lubricant.
at standard temperature and pressure), assumes dry air. It is not known that
the original work involved dry air but it has since been shown that this can
be a factor in reproducibility and should be addressed. A dew point of less
1
This test method is under the jurisdiction of ASTM Committee D02 on than 10 °C at standard temperature and pressure will be satisfactory.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of NOTE 2—To determine evaporation loss at temperatures above 150 °C
Subcommittee D02.G0.03 on Physical Tests. (300 °F), see Test Methods D2595.
Current edition approved April 1, 2016. Published May 2016. Originally
approved in 1948. Last previous edition approved in 2008 as D972 – 02 (2008). 6. Apparatus
DOI: 10.1520/D0972-16.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 6.1 Evaporation Cell, (Fig. 1) as described in Annex A1.
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 6.2 Air Supply System, capable of supplying to the cell the
the ASTM website. required flow of air free of entrained particles. A 400 mm

*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

1
 D972 − 16

FIG. 1 Evaporation Test Cell FIG. 1a Assembled Apparatus

Key mm in. Key mm in.
A 6.4 0.25 D 124/130 5.0 ± 0.125
B 1830 72 E 3.2 0.125
C 13 0.5 ± 0.1 = 25 F 1.3/1.8 0.051/0.072
G 73.1 2.875
Tolerances: ±0.4 mm (±0.0156 in.) unless otherwise noted

(16 in.) length of 25 mm (1 in.) diameter pipe packed with 7.2 Each oil test will require at least 10 g of sample for a
glass wool has been found satisfactory for filtering the air. single run. Therefore, sufficient sample should be available to
6.3 Oil Bath, shown in Fig. 1a and described in Annex A1. observe any gross contamination or phase separation. If any
abnormal conditions are found, obtain a new sample.
NOTE 3—Other constant-temperature baths may be used if they are
equivalent in heat capacity and thermal gradient characteristics to the oil
bath.
8. Preparation of Apparatus
6.4 Thermometers—For tests at 100 °C (210 °F) an ASTM 8.1 Clean and inspect all components and particularly for
Thermometer having a range from 95 °C to 103 °C (204 °F to wear or damage to threads on sample cups and hood assem-
218 °F) and conforming to the requirements for Thermometer blies. Repair or replace if mating is impaired.
S22C (S22F) as prescribed in Specification E2251 shall be 8.2 Verify unrestricted air flow through tubing on test cell
used. For tests at temperatures above 100 °C (210 °F), an and through eduction tube through cover.
ASTM Precision Thermometer conforming to the requirements
8.3 Check that the oil bath is filled with a sufficient quantity
for Thermometer S67C (S67F) as prescribed in Specification
of fluid to allow submersion of the evaporation cell to the
E2251 is suitable.
proper level as required in 9.2.
6.5 Flowmeter—A rotameter calibrated to deliver air at a
rate of 2.58 g ⁄min 6 0.02 g ⁄ min between 15 °C and 30 °C 8.4 Check flowmeter before running any test if there is
(60 °F and 85 °F) (2 L ⁄ min at standard temperature and doubt of its accuracy.
pressure). It shall be furnished with a needle valve and
mounted as shown in Fig. 1. 9. Procedure for Greases
9.1 Weigh the clean grease-sample cup and hood (Fig. 2) to
7. Sampling the nearest 1 mg. Remove the hood and fill the cup with
7.1 Each grease test will require approximately 20 g to fill sample, taking care to avoid occlusion of air. Smooth the
the sample cup for a single cup for a single run. Therefore, the surface level with the rim of the cup with a straight-edged
sample presented for analysis should be large enough to make spatula. Remove with a clean cloth any grease which may
possible the selection of a representative portion for testing. remain on the rim or threads of the cup. Thread the hood tightly
Examine the sample for any indication of non-homogenity onto the cup without disturbing the smoothed grease surface.
such as oil separation, phase changes, or gross contamination. Weigh the assembly and record the mass of the sample to the
If any abnormal conditions are found, obtain a new sample. nearest 1 mg.

2
 D972 − 16

FIG. 2 Grease Sample Cup FIG. 2a Oil Sample Cup

Key mm in. Key mm in.

H 66 2.625 O 5.40/5.65 0.213/0.223
I 7.62 0.3125 P 1.45/1.70 0.057/0.067
J 6.35 0.25 Q 54.64/54.89 2.15/2.16
K 1.6 0.0625 R 6.9/7.4 0.27/0.29
L 5 0.1875 S 3 0.125
M 33 1.3125 T 4 0.16
N 40 1.6 U 58.7 2.3
Tolerances: ±0.4 mm (±0.0156 in.) unless otherwise noted

9.2 With the cover in place, but without the hood and 0.05 g of sample to the cup. Assemble the cup and hood, being
sample cup attached, allow the evaporation cell to acquire the careful not to splash oil on the underside of the hood. Weigh
temperature of the bath (controlled to 60.5 °C (61 °F)) at the assembly and record the net sample mass to the nearest
which the test is to be made by immersing the cell in the bath, 1 mg.
as shown in Fig. 2. Ensure the cell is immersed to the 10.2 Evaporate the sample as described in 9.2 and 9.3.
designated depth using the support rod adjustment. Allow the
cell to remain in the bath at least 1⁄2 h before beginning the test. 11. Calculation
During this period, allow clean air to flow through the cell at
the prescribed rate, 2.58 g ⁄ min 60.02 g ⁄ min (2 L ⁄min at 11.1 Calculate the evaporation loss of the sample as follows:
standard temperature and pressure), as indicated by the rotame- Evaporation loss, mass % 5 @ ~ S 2 W ! /S # 3 100 (1)
ter. Remove the cover, thread the weighed hood and sample
where:
cup into place, and replace the cover. Tighten the three
cover-tightening screws securely to prevent air leakage under S = initial mass of sample, g, and
the cover. Pass clean air through the cell at the prescribed rate W = mass of sample, g, after the test.
for 22 h 6 5 min.
12. Precision and Bias
9.3 Remove the assembled sample cup and hood from the
cell. At the end of the 22 h period allow to cool to room 12.1 The precision of this test method is not known to have
temperature. Determine the mass of the sample to the nearest been obtained in accordance with currently accepted guidelines
1 mg. (in Committee D02 research report RR:D02-1007, “Manual on
Determining Precision Data for ASTM Methods on Petroleum
10. Procedure for Oils Products and Lubricants”).
10.1 Weigh the clean oil-sample cup and hood (Fig. 2a) to 12.2 The precision of this test method as determined by
the nearest 1 mg. Transfer, by means of a pipet, 10.00 g 6 statistical examination of interlaboratory results is as follows:

3
 D972 − 16
12.2.1 Repeatability—The difference between two test the long run, in the normal and correct operation of the test
results, obtained by the same operator with the same apparatus method, exceed the following value only in one case in twenty:
under constant operating conditions on identical test material, 0.10M (3)
would in the long run, in the normal and correct operation of
the test method, exceed the following value only in one case in where:
twenty: M = mean of two values.
0.025M (2) 12.3 Bias—The procedure in this test method for measuring
evaporation loss of lubricating greases and oils has no bias
where:
because the value of loss in mass is defined only in terms of
M = mean of two values. this test method.
12.2.2 Reproducibility—The difference between two single
and independent results obtained by different operators work- 13. Keywords
ing in different laboratories on identical test material would, in 13.1 evaporation; grease; oil; oil bath; rotameter; volatiles

ANNEX

(Mandatory Information)

A1. APPARATUS

A1.1 Evaporation Cell, with attachments conforming with A1.1.3 The cover of the cell shall be made airtight.
the dimensional tolerances as indicated in Fig. 1 and Fig. 1a
and capable of being supported upright in the oil bath. Other A1.2 Oil Bath , of sufficient depth to allow submersion of
structural details are as follows: the evaporation cell to the proper level and capable of being
controlled at the desired test temperature within 60.5 °C
A1.1.1 The body and cover of the cell shall be constructed
of stainless steel and the air-heating coil of tinned copper (61 °F), with a maximum variation throughout the bath of
tubing. 60.5 °C (61 °F). Circulation of the oil heating medium by a
pump or stirrer is recommended. Sufficient heat capacity shall
A1.1.2 The sample cups (recommended maximum mass be provided to return the bath to the required temperature
200 g each), hood, eduction tube, and orifice shall be con-
within 60 min after immersion of the cell. The bath shall be
structed of 18 % chromium, 8 % nickel alloy steel. A suitable
provided with a temperature well such that the thermometer
material is an alloy steel conforming to Grade S, Type 304, of
used can be inserted to its proper immersion depth. The bath
Specification A240/A240M. To facilitate removal and separa-
tion of the cup and hood for inserting the sample and weighing, shall be arranged so that there are no wide fluctuations in
the sample cup shall be threaded to the hood and this in turn to temperature around the evaporation cell.
the eduction tube of the cover.

SUMMARY OF CHANGES

Subcommittee D02.G0 has identified the location of selected changes to this standard since the last issue
(D972 – 02 (2008)) that may impact the use of this standard. (Approved April 1, 2016.)

(1) Revised Referenced Documents and subsection 6.4.

4
 D972 − 16
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/