Designation: D 6184 – 98

AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Method for

Oil Separation from Lubricating Grease (Conical Sieve
Method)1
This standard is issued under the fixed designation D 6184; 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.

INTRODUCTION

The conical sieve method for measuring leakage from lubricating grease (commonly known as the
cone bleed test) is virtually the same as Federal Test Method (FTM) 791C Method 321.3, Oil
Separation from Lubricating Grease (Static Technique). Despite the lack of a precision statement,
Method 321.3 has been used for many years in military and industrial grease specifications to
determine fluid separation tendencies. Test Method D 6184 overcomes the deficiencies of the Method
321.3. It reflects the procedures and precision determinations used in a cooperative study in
Subcommittee G of Committee D–2 and is intended to supersede the FTM method.

1. Scope Separation from Lubricating Greases (Static Method)4

1.1 This test method is used to determine the tendency of 3. Terminology
lubricating grease to separate oil at an elevated temperature.
This test method shall be conducted at 100°C for 30 h unless 3.1 Definitions:
other conditions are required by the grease specification. 3.1.1 lubricating grease, n—a semifluid to solid product of
1.2 This test method is not suitable for greases having a a dispersion of a thickener in a liquid lubricant.
penetration (Test Methods D 217) greater than 340 (softer than 3.1.1.1 Discussion—The dispersion of the thickener forms a
NLGI No. 1 grade).2 two-phase system and immobilizes the liquid lubricant by
1.3 Values stated in acceptable SI units are to be regarded as surface tension and other physical forces. Other ingredients
the standard. imparting special properties are often included. D 217
1.4 This standard does not purport to address all the safety 3.1.2 oil separation, n—the appearance of a liquid fraction
concerns, if any, associated with its use. It is the responsibility from an otherwise homogeneous lubricating composition.
of the user of this standard to establish appropriate safety D 1742
practices and determine the applicability of regulatory limita- 3.1.3 thickener, n—in a lubricating grease, a substance
tions prior to use. composed of finely divided particles dispersed in a liquid
lubricant to form the product’s structure.
2. Referenced Documents 3.1.3.1 Discussion—The thickener can be fibers (such as
2.1 ASTM Standards: various metallic soaps) or plates or spheres (such as certain
D 217 Test Methods for Cone Penetration of Lubricating non-soap thickeners) which are insoluble or, at most, only very
Grease2 slightly soluble in the liquid lubricant. The general require-
D 1742 Test Methods for Oil Separation from Lubricating ments are that the solid particles be extremely small, uniformly
Grease During Storage2 dispersed, and capable of forming a relatively stable, gel-like
E 437 Specification for Industrial Wire Cloth and Screens structure with the liquid lubricant D 217
(Square Opening Series)3
4. Summary of Test Method
2.2 Government Standard:
Federal Test Method (FTM) 791C Method 321.3, Oil 4.1 The weighed sample is placed in a cone-shaped, wire-
cloth sieve, suspended in a beaker, then heated under static
conditions for the specified time and temperature. Unless
otherwise required by the grease specification, the sample is
1
This test method is under the jurisdiction of ASTM Committee D-2 on tested at standard conditions of 1006 0.5°C for 30 6 0.25 h.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee The separated oil is weighed and reported as a percentage of
D02.G on Lubricating Grease.
Current edition approved June 10, 1998. Published September 1998.
Originally published as D 6184-97. Last previous edition D 6184-97.
2 4
Annual Book of Standards, Vol 05.01. Available from Standardization Documents Order Desk, Bldg. 4 Section D, 700
3
Annual Book of Standards, Vol 14.02. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.

1
 D 6184
the mass of the starting test sample. sensitivity of at least 0.01 g.
5. Significance and Use 7. Sampling
5.1 When a lubricating grease separates oil, the residual 7.1 Examine the sample for any indication of non-
material changes in consistency, which can affect the ability of homogeneity such as oil separation, phase changes, or gross
the product to function as designed. Test results obtained with contamination. If any abnormal conditions are found, obtain a
this procedure are intended to correlate with oil separation that new sample.
occurs in 35-lb pails of grease during storage. They are not 7.2 The sample submitted for analysis should be minimally
intended to predict oil separation tendencies of grease under sufficient for duplicate testing.
dynamic service conditions. 7.3 Although the mass of the test grease is determined, the
sieve is filled by volume rather than mass. Each test will
NOTE 1—No quantitative relationship between results and oil separa-
tion in 35-lb pails has been developed.
require a quantity sufficient to fill the sieve to approximately
the same level as indicated in Fig. 1 (about 10 mL). Approxi-
5.2 This test method is used for specifications and quality mately the same volume shall be used for each test regardless
control. of the grease density; the mass will range from about 8 to 12
NOTE 2—No data has been developed to compare results between this g.
test method and Test Methods D 1742.
8. Preparation of Apparatus
6. Apparatus 8.1 Carefully clean the sieve, beaker, and cover, by wiping
6.1 Test Apparatus— The assembled apparatus consists of a with a suitable solvent. Allow the sieve to air dry. See Note 4.
cone-shaped sieve constructed of 60-mesh, corrosion -resistant NOTE 4—Use of an ultrasonic solvent bath has been found helpful in
wire cloth, a 200-mL tall-form beaker without spout, and a cleaning the sieve.
closely fitting cover with a hook in the center. Construction
details and dimensions are shown in Fig. 1. 8.2 Inspect the sieve to make certain that it is clean and free
6.1.1 The conical sieve shall be fabricated of stainless steel, of deposits that could affect the passage of oil. It shall be free
monel, or nickel wire cloth, of No. 60 medium-heavy mesh as of any screen irregularities such as tears, dents, creases, or
defined in Table 2 of Specification E 437 and shall be fabri- enlarged or diminished openings.
cated to the dimensions and requirements shown in Fig. 1. 9. Procedure
NOTE 3—Sieves of stapled or wire-bound construction, instead of silver 9.1 Preheat the oven to test temperature. Unless otherwise
soldered construction, have been used in the past. Such sieves do not specified, the test shall be conducted at standard conditions of
conform to this test method. 100 6 0.5°C for 30 6 0.25 h.
6.2 Oven, capable of maintaining the specified temperature, 9.2 Weigh the beaker to within 0.01 g, Wi.
100 6 0.5°C. 9.3 Tare the assembled apparatus consisting of the sieve,
6.3 Balance, having a minimum capacity of 250 g and a cover, and beaker as shown in Fig. 1 to the nearest 0.01 g.

NOTE 1—Dimensions are provided in millimetres (with in./lb. units in parentheses) as follows:
38.1 6 0.3 (1.50 6 0.01) radius
27.0 6 0.3 (1.06 6 0.01) height
70 (2.8) approximately (to fit beaker)
9.7 6 3.3 (0.38 6 0.13) length
100 (4) approximately
36 (1.4) approximately

FIG. 1 Cone Fabrication and Test Setup

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 D 6184
9.4 With a suitable spatula, fill the cone sieve with sufficient TABLE 1 Precision Values for Several Oil Separation
grease to approximate the level shown in Fig. 1, being careful Percentages
to avoid inclusion of air. Exercise care not to force grease Oil Separation, % Repeatability Reproducibility
through the screen. Smooth and shape the top of the grease into 1 1.15 1.51
a slightly convex surface to prevent trapping free oil. 5 2.57 3.39
10 3.64 4.79
9.5 Assemble the entire apparatus as shown in Fig. 1, and 20 5.15 6.78
weigh to the nearest 0.01 g. Calculate the mass of the grease by
difference, G. 12.2 The precision of the percent oil separation as
9.6 Place the assembled apparatus in the oven for the determined by this test method was obtained in accordance
specified time and temperature. with guidelines currently accepted by Committee D-2
9.7 Remove the apparatus from the oven and cool to room (computer program: D2PP, Calculation of Precision Data:
temperature. Remove the cone from the beaker, tapping it Petroleum Test Methods).6
gently against the inside of the beaker to take off any oil 12.3 The repeatability and reproducibility of the test method
adhering to its tip. Weigh the beaker containing the collected as determined by statistical examination of the interlaboratory
oil to the nearest 0.01 g, Wf. results are as follows:
9.8 Soon after completion of the test, clean the apparatus 12.3.1 Repeatability—The difference between two test
(Section 8) in preparation for subsequent testing. results, obtained by the same operator with the same apparatus
10. Calculation under constant specified operating conditions on identical test
material would, in the long run, in the normal and correct
10.1 Calculate the oil separation as the percentage separated operation of the test method, exceed the following values only
from the original sample as follows: in one case in twenty:
W f – Wi
oil separation, % 5 repeatability, % oil separation 5 1.151 3 ~M!0.5
G 3 100 (1) (2)

where: where:
Wi 5 mass of the beaker before heating, M 5 mean of two determinations.
Wf 5 mass of the beaker after heating, and 12.3.2 Reproducibility—The difference between two single
G 5 mass of the grease tested. and independent results by two different operators working in
different laboratories on identical test material would, in the
11. Report long run, in the normal and correct operation of the test
11.1 Report the following information: method, exceed the following values only in one case in
11.1.1 Grease identity, twenty:
11.1.2 Test date, reproducibility, % oil separation 5 1.5173 ~M!0.5 (3)
11.1.3 Test temperature and duration, and
11.1.4 Oil separation, nearest 0.1 %. where
M 5 mean of two determinations.
12. Precision and Bias 12.4 Bias—The procedure for measuring the oil separation
12.1 Precision—Eight cooperators tested eight greases for from lubricating grease has no bias because the value of the oil
leakage in a cooperative program conducted in accordance loss is defined only in terms of this test method.
with the design-of-experiments described in RR: D02-1007.5 13. Keywords
All tests were run in duplicate. The total range of results were
13.1 cone-bleed test; leakage; lubricating grease; oil bleed;
from 0.1 to 23.7 % leakage (see Table 1).
oil separation

5 6
RR: D02-1007, “Manual on Determining Precision Data for ASTM Methods on D2PP, Calculation of Precision Data: Petroleum Test Methods, Publication
Petroleum Products and Lubricants”, Annual Book of Standards, Vol 05.03. Code Number (PCN) 13-4020000-12, is available from ASTM Headquarters.

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