An American National Standard

Designation: D 2711 – 01a

Standard Test Method for

Demulsibility Characteristics of Lubricating Oils1
This standard is issued under the fixed designation D 2711; 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 4. Significance and Use

1.1 This test method covers the measurement of the ability 4.1 This test provides a guide for determining the demulsi-
of oil and water to separate from each other. It is intended for bility characteristic of lubricating oils that are prone to water
use in testing medium and high-viscosity lubricating oils. contamination and may encounter the turbulence of pumping
1.2 The values stated in SI units are to be regarded as the and circulation capable of producing water-in-oil emulsions.
standard. The values given in parentheses are for information
only. 5. Apparatus
1.3 This standard does not purport to address all of the 5.1 Stirrer, 4 constructed from parts shown in Fig. 1 and Fig.
safety concerns, if any, associated with its use. It is the 2.
responsibility of the user of this standard to establish appro- 5.2 Special Graduated Separatory Funnel,4 as shown in
priate safety and health practices and determine the applica- Fig. 3.
bility of regulatory limitations prior to use. 5.3 Heating Bath, sufficiently large and deep to permit the
immersion of at least two test separatory funnels in the bath
2. Referenced Documents liquid up to their 500-mL graduation mark. The bath shall be
2.1 ASTM Standards: capable of maintaining a temperature of 82 6 1°C (180 6 2°F)
D 1193 Specification for Reagent Water2 and shall be so equipped to hold the separatory funnels
D 1796 Test Method for Water and Sediment in Fuel Oils by securely in a position so that the vertical axis of the stirrer
the Centrifuge Method (Laboratory Procedure)3 corresponds to the center line of the separatory funnel during
the mixing of the oil and water.
3. Summary of Test Method 5.4 Centrifuge, as described in Test Method D 1796.
3.1 For Oils That Do Not Contain Extreme Pressure (EP) 5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) as
Additives—A 405-mL sample of the oil and 45 mL of distilled described in Fig. 1 of Test Method D 1796.
water are stirred together for 5 min at 82°C (180°F) in a special
graduated separatory funnel. After a 5-h settling period follow- 6. Materials
ing the stirring, a percentage of the water in the oil and the 6.1 Cleaning Solvent—Any suitable solvent capable of
volumes of water and emulsion separating from the oil are cleaning and effectively removing any oil or fluid from the
measured and recorded. stirrer and graduated cylinder. 1,1,1-Trichloroethane has been
3.2 For Oils That Contain Extreme Pressure (EP) found suitable for use in this test method. (Warning—
Additives—A 360-mL sample of the oil and 90 mL of distilled 1,1,1–Trichloroethane, Harmful if inhaled or swallowed. Eye
water are stirred together for 5 min at 82 °C (180 °F) in a irritant. High concentration can cause unconsciousness or
special graduated separatory funnel. After a 5-h settling period death.)
following the stirring, percentage of water in the oil and the NOTE 1—In cases in which the use of 1,1,1 trichloroethane is unac-
volumes of water and emulsion separating from the oil are ceptable, some laboratories are using heptane or mineral spirits as
measured and recorded. alternative solvents. The effect on the precision of this test method when
using an alternate solvent has not been determined.
1
This test method is under the jurisdiction of ASTM Committee D02 on
6.2 Water—Type II reagent grade water conforming to
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee Specification D 1193.
D02.L on Industrial Lubricants.
Current edition approved Nov. 10, 2001. Published November 2001. Originally
published as D 2711 – 68 T. Last previous edition D 2711 – 01.
2 4
Annual Book of ASTM Standards, Vol 11.01. Available from Research Appliance Co., Moose Lodge Rd., Dept. T, Cam-
3
Annual Book of ASTM Standards, Vol 05.01. bridge, MD 21613.

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

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 D 2711 – 01a

FIG. 1 Stirrer

7. Preparation of Apparatus total of 5 min, including the start-up time. Then withdraw the
7.1 Clean the graduated separatory funnel by removing any stirrer from the oil-water mixture but not entirely out of the
film of oil with cleaning solvent followed by a wash first with separatory funnel. Allow the stirrer to drain for 5 min, then
acetone (Warning—Extremely flammable vapors may cause remove from the separatory funnel and clean.
flash fires.) and then with tap water. Rinse thoroughly with tap 8.3 Five hours after stirring has stopped, withdraw a 50-mL
water and then with reagent grade water. sample from the center of the funnel and approximately 50 mm
7.2 Clean the stirrer by appropriate means, using the clean- (2 in.) below the surface of the oil-water mixture, using a
ing solvent (6.1). Allow the stirrer to air dry completely prior 50-mL pipet. Discharge the contents of the pipet into a
to use in the test. centrifuge tube and determine the water present in the sample
using Test Method D 1796. Record the results as “percent
8. Procedure A for Oils That Do Not Contain EP
water in the oil.”
Additives
8.4 With minimum delay, after sampling for the “percentage
8.1 Heat the bath liquid to 82 6 1°C (180 6 2°F) and
of water in the oil,” remove the separatory funnel from the bath
maintain this temperature throughout the test.
and draw off any free water that has separated from the
8.2 Measure the oil under test, at room temperature, directly
oil-water mixture into a 50-mL graduated cylinder. Allow this
into the separatory funnel to a volume of 405 6 5 mL. Place
water to reach room temperature, measure, and record the
the separatory funnel and oil in the constant-temperature bath
and bring it to a temperature of 82°C (180°F). Add 45 6 0.5 volume.
mL of distilled water, measured at room temperature, to the oil. 8.5 After removing the free water from the separatory
Immerse the stirrer in the oil and position it carefully as funnel, reduce the volume of the fluid remaining to 100 mL by
follows: lower the stirrer until it touches the bottom of the carefully siphoning the fluid off the top (end of siphon should
funnel, then raise it approximately 25 mm (1 in.). Ensure that not be more than 20 mm below the surface of the fluid at any
the vertical axis of the stirrer corresponds with the vertical time) down to the 100-mL graduation mark on the separatory
center line of the funnel. Slowly bring the stirrer motor to a funnel. Drain the remaining 100 mL of fluid (oil, water, and
speed of 4500 6 500 rpm within 25 to 30 s, and operate for a emulsion) directly into a centrifuge tube.

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 D 2711 – 01a

FIG. 2 Detailed Construction of Stirrer

8.6 Centrifuge the tube and its contents for a period of 10 to center line of the funnel. Slowly bring the stirrer motor to a
15 min at a relative centrifugal force of 700. Record the speed of 2500 6 250 rpm within 25 to 30 s, and operate for a
volume of water and emulsion separated by centrifuging. total of 5 min, including the start-up time (Note 2). Then
8.7 Perform a minimum of two determinations on each oil withdraw the stirrer from the oil-water mixture but not entirely
sample by repeating procedure 8.1-8.6. If the difference in the out of the separatory funnel. Allow the stirrer to drain for 5
two sets of results obtained is outside the repeatability limits of min, then remove it from the separatory funnel and clean.
Procedure A, discard them and obtain two additional sets of 9.3 Five hours after stirring has stopped, withdraw a 50-mL
results. sample from the center of the funnel approximately 50 mm (2
in.) below the surface of the oil-water mixture, using a 50-mL
9. Procedure B for Oils That Contain EP Additives pipete. Discharge the contents of the pipet into a centrifuge
9.1 Heat the bath liquid to 82 6 1 °C (180 6 2 °F) and tube and determine the water present in the sample using Test
maintain this temperature throughout the test. Method D 1796. Record the results as “percent water in the
9.2 Measure the oil under test, at room temperature, directly oil”.
into the separatory funnel to a volume of 360 6 5 mL. Place 9.4 Immediately after sampling for the “percentage of water
the separatory funnel and oil in a constant-temperature bath in the oil”, remove the separatory funnel from the bath and
and bring to a temperature of 82 °C (180 °F). Add 90 6 0.5 mL draw off any free water that has separated from the oil-water
of distilled water, measured at room temperature, to the oil. mixture into a 100-mL graduated cylinder. Allow this water to
Immerse the stirrer in the oil and position it carefully as reach room temperature, measure, and record the volume.
follows: lower the stirrer until it touches the bottom of the 9.5 After removing the free water from the separatory
funnel, then raise it approximately 25 mm (1 in.). Ensure that funnel, reduce the volume of the fluid remaining to 100 mL by
the vertical axis of the stirrer corresponds with the vertical carefully siphoning the fluid off the top (end of siphon should

3
 D 2711 – 01a

FIG. 3 Graduated Separatory Funnel

not be more than 20 mm below the surface of the fluid at any NOTE 4—The “total millilitres of free water” is the sum of the millilitres
time) down to the 100-mL graduation mark on the separatory of free water collected in the 50-mL graduated cylinder (8.4) and the
funnel. Drain the remaining 100 mL of fluid (oil, water and millilitres of free water separated by centrifuging (8.6).
emulsion) directly into a centrifuge tube. 11. Precision for Procedure A
9.6 Centrifuge the tube and its contents for a period of 10 to
11.1 The precision for Procedure A does not use the matrix
15 min at a relative centrifugal force of 700. Record the
of laboratories and samples required by RR: D02 – 1007.5 The
volume of water and emulsion separated by centrifuging.
following criteria should be used for judging the acceptability
9.7 Perform a minimum of two determinations on each oil
of results (95 % confidence). This precision statement is based
sample by repeating procedure 9.1-9.3. If the difference in the
on results obtained by seven laboratories on three oils and is
two sets of results obtained is outside the repeatability limits of
applicable to oils with viscosity grades ranging from ISO 220
Procedure B, discard them and obtain two additional sets of
to ISO 460 (1000 SUS to 2000 SUS of 100°F).
results.
11.1.1 Repeatability—The difference between successive
NOTE 2—The stirring motor may slow down when testing high- results obtained by the same operator with the same apparatus
viscosity or emuslion-forming oils. Check speed frequently during the under constant operating conditions on identical test material
5-min stirring period and adjust as necessary.
would, in the long run, in the normal and correct operation of
10. Report the test method, exceed the following values only in one case
in twenty:
10.1 Report the procedure used, that is, Procedure A or
Total free water, mL 4.0
Procedure B. Emulsion, mL 0.2
10.2 Report the “percentage of water in the oil,” (Note 3)
“total millilitres of free water” (Note 4) and the “millilitres of 11.1.2 Reproducibility—The difference between two single
emulsion” separated by centrifuging, for each determination and independent results obtained by different operators work-
and the average of each observation for all determinations. ing in different laboratories on identical test material would, in
These are necessary factors in determining the demulsibility the long run, exceed the following values only in one case in
characteristics of a lubricating oil. twenty:

NOTE 3—Percent water in oil, record water present in amounts less than
5
0.1 % as <0.1 % or “trace.” Available from ASTM International Headquarters.

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 D 2711 – 01a
Total free water, mL 8.0 under constant operating conditions on identical test material
Emulsion, mL 0.3 would, in the long run, in the normal and correct operation of
the test method exceed the values shown in Table 1 only in one
12. Precision for Procedure B
case in twenty.
12.1 The precision for Procedure B is based on results of 12.1.2 Reproducibility—The difference between single and
cooperative tests from 13 laboratories on six laboratory- independent results obtained by different operators working in
blended extreme-pressure lubricating oils. Test results, descrip- different laboratories on identical test material would, in the
tions of the oils and analysis of data from this interlaboratory long run, exceed the values shown in Table 1 only in one case
test program may be obtained from ASTM International in twenty.
Headquarters.6 The test oils were classified in three groups
with respect to level of demulsibility as measured by this test 13. Bias
method - A, B and C - and precision data were developed for
each classification. Classification groups and limits, and preci- 13.1 The procedure in Test Method D 2711 has no bias
sion data are shown in Table 1. because the values of total free water and emulsion can be
12.1.1 Repeatability—The difference between successive defined only in terms of a test method.
results obtained by the same operator with the same apparatus
14. Keywords
14.1 demulsibility; water contamination; water/oil separa-
6
Available from ASTM International Headquarters. Request RR: D02–1449.
tion

TABLE 1 Precision for Procedure B on Extreme-Pressure Lubricating Oils

Classification Limits Repeatability, r Reproducibility, R
Demulsibility Water Water
Total Free Emulsion, Total Free Emulsion, Total Free Emulsion,
Classification Water in Oil, % in Oil, in Oil,
Water, mL mL Water, mL mL Water, mL mL
% %
A 1.4 max 79 min 0.2 max 0.4 3.6 0.1A 0.8 5.1 0.2A
B 6.0 max 60 min 4.0 max 4.0 11 1.6 4.2 23 3.5
C >6.0 <60 >4.0 5.6 18 ;23 22 57 ;96
A
Estimated from inspection of data.

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 D 2711 – 01a

APPENDIX

(Nonmandatory Information)

X1. APPARATUS

X1.1 “Gage and Centering Device” (Fig. X1.1), is an aid in especially in the case of high-viscosity oils or the presence of
obtaining the 50-mL samples from the separatory funnel for a “mayonnaise”-type emulsion, by applying a slight amount of
the“ percent water in the oil” determination (8.3). pressure (Fig. X1.3) to the open end of the separatory funnel to
force the flow of the oil or emulsion, or both, into the
X1.2 Fig. X1.2 illustrates a rapid method for reducing the
centrifuge tube.
volume of fluid remaining in the separatory funnel to 100 mL
by siphoning the fluid off the top (end of siphon shall be not
X1.3 Fig. X1.4(a) shows a suggested container for the
more than 3⁄4 in. (20 mm) below the surface of the fluid at any
time) down to the 100-mL graduation mark on the separatory solvent used to clean the stirrer after mixing the oil and water
funnel (8.5). (8.2) and Fig. X1.4(b) shows a suggested method for air drying
the stirrer after the above (solvent) washing.
X1.2.1 The time required to drain the 100 mL of fluid from
the separatory funnel into the centrifuge tube can be reduced,

FIG. X1.1 Sampling Gage and Centering Device

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 D 2711 – 01a

FIG. X1.2 Device to Reduce Volume in Separatory Funnel

FIG. X1.3 Pressure Device

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 D 2711 – 01a

FIG. X1.4 Optional Equipment

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