ASTM D2711-01a(2007)e1
(Test Method)Standard Test Method for Demulsibility Characteristics of Lubricating Oils
Standard Test Method for Demulsibility Characteristics of Lubricating Oils
SIGNIFICANCE AND USE
This test provides a guide for determining the demulsibility characteristic of lubricating oils that are prone to water contamination and may encounter the turbulence of pumping and circulation capable of producing water-in-oil emulsions.
SCOPE
1.1 This test method covers the measurement of the ability of oil and water to separate from each other. It is intended for use in testing medium and high-viscosity lubricating oils.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use.
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´1
Designation:D2711–01a (Reapproved 2007)
Standard Test Method for
Demulsibility Characteristics of Lubricating Oils
This standard is issued under the fixed designation D2711; 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.
´ NOTE—Updated supplier footnote and 7.2 editorially in March 2009.
1. Scope ing the stirring, percentage of water in the oil and the volumes
ofwaterandemulsionseparatingfromtheoilaremeasuredand
1.1 This test method covers the measurement of the ability
recorded.
of oil and water to separate from each other. It is intended for
use in testing medium and high-viscosity lubricating oils.
4. Significance and Use
1.2 The values stated in SI units are to be regarded as the
4.1 This test provides a guide for determining the demulsi-
standard. The values given in parentheses are for information
bility characteristic of lubricating oils that are prone to water
only.
contamination and may encounter the turbulence of pumping
1.3 This standard does not purport to address all of the
and circulation capable of producing water-in-oil emulsions.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
5.1 Stirrer, constructedfrompartsshowninFig.1andFig.
bility of regulatory limitations prior to use.
2.
5.2 Special Graduated Separatory Funnel, as shown in
2. Referenced Documents
Fig. 3.
2.1 ASTM Standards:
5.3 Heating Bath, sufficiently large and deep to permit the
D1193 Specification for Reagent Water
immersion of at least two test separatory funnels in the bath
D1796 Test Method forWater and Sediment in Fuel Oils by
liquid up to their 500-mL graduation mark. The bath shall be
the Centrifuge Method (Laboratory Procedure)
capable of maintaining a temperature of 82 6 1°C (180 6 2°F)
3. Summary of Test Method and shall be so equipped to hold the separatory funnels
securely in a position so that the vertical axis of the stirrer
3.1 For Oils That Do Not Contain Extreme Pressure (EP)
corresponds to the center line of the separatory funnel during
Additives—A405-mL sample of the oil and 45 mL of distilled
the mixing of the oil and water.
waterarestirredtogetherfor5minat82°C(180°F)inaspecial
5.4 Centrifuge, as described in Test Method D1796.
graduated separatory funnel.After a 5-h settling period follow-
5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) as
ing the stirring, a percentage of the water in the oil and the
described in Fig. 1 of Test Method D1796.
volumes of water and emulsion separating from the oil are
measured and recorded.
6. Materials
3.2 For Oils That Contain Extreme Pressure (EP)
6.1 Cleaning Solvent—Any suitable solvent capable of
Additives—A360-mL sample of the oil and 90 mL of distilled
cleaning and effectively removing any oil or fluid from the
waterarestirredtogetherfor5minat82°C(180°F)inaspecial
stirrer and graduated cylinder. 1,1,1-Trichloroethane has been
graduated separatory funnel.After a 5-h settling period follow-
found suitable for use in this test method. (Warning—
1,1,1–Trichloroethane, Harmful if inhaled or swallowed. Eye
irritant. High concentration can cause unconsciousness or
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
death.)
D02.L0.01 on Machinery Lubricants and Metal Removal Fluids.
Current edition approved July 15, 2007. Published September 2007. Originally NOTE 1—In cases in which the use of 1,1,1 trichloroethane is unac-
approved in 1968. Last previous edition approved in 2001 as D2711–01a. DOI:
ceptable, some laboratories are using heptane or mineral spirits as
10.1520/D2711-01AR07E01.
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 Formerly available from Research Appliance Co., Moose Lodge Rd., Dept. T,
Standards volume information, refer to the standard’s Document Summary page on Cambridge, MD 21613. Section D02.L0.01 is actively seeking a replacement
the ASTM website. supplier.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D2711–01a (2007)
FIG. 1 Stirrer
alternative solvents. The effect on the precision of this test method when
Immerse the stirrer in the oil and position it carefully as
using an alternate solvent has not been determined.
follows: lower the stirrer until it touches the bottom of the
funnel, then raise it approximately 25 mm (1 in.). Ensure that
6.2 Water—Type II reagent grade water conforming to
the vertical axis of the stirrer corresponds with the vertical
Specification D1193.
center line of the funnel. Slowly bring the stirrer motor to a
7. Preparation of Apparatus
speed of 4500 6 500 rpm within 25 to 30 s, and operate for a
total of 5 min, including the start-up time. Then withdraw the
7.1 Clean the graduated separatory funnel by removing any
film of oil with cleaning solvent followed by a wash first with stirrer from the oil-water mixture but not entirely out of the
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
water and then with reagent grade water. 8.3 Five hours after stirring has stopped, withdraw a 50-mL
sample from the center of the funnel and approximately 50 mm
7.2 Clean the stirrer by appropriate means, using the clean-
ing solvent (6.1). Allow the stirrer to air dry completely prior (2 in.) below the surface of the oil-water mixture, using a
50-mL pipet. Discharge the contents of the pipet into a
to use in the test. (Warning—To minimize any potential
sparking hazard, ensure that the motor is detached from any centrifuge tube and determine the water present in the sample
usingTest Method D1796. Record the results as “percent water
electrical source during the cleaning procedure.)
in the oil.”
8. Procedure A for Oils That Do Not Contain EP
8.4 With minimumdelay, after sampling for the “percentage
Additives
ofwaterintheoil,”removetheseparatoryfunnelfromthebath
8.1 Heat the bath liquid to 82 6 1°C (180 6 2°F) and and draw off any free water that has separated from the
maintain this temperature throughout the test. oil-water mixture into a 50-mL graduated cylinder. Allow this
8.2 Measure the oil under test, at room temperature, directly water to reach room temperature, measure, and record the
into the separatory funnel to a volume of 405 6 5 mL. Place volume.
the separatory funnel and oil in the constant-temperature bath 8.5 After removing the free water from the separatory
and bring it to a temperature of 82°C (180°F). Add 45 6 0.5 funnel, reduce the volume of the fluid remaining to 100 mLby
mLof distilled water, measured at room temperature, to the oil. carefully siphoning the fluid off the top (end of siphon should
´1
D2711–01a (2007)
FIG. 2 Detailed Construction of Stirrer
not be more than 20 mm below the surface of the fluid at any Immerse the stirrer in the oil and position it carefully as
time) down to the 100-mL graduation mark on the separatory follows: lower the stirrer until it touches the bottom of the
funnel. Drain the remaining 100 mL of fluid (oil, water, and funnel, then raise it approximately 25 mm (1 in.). Ensure that
emulsion) directly into a centrifuge tube. the vertical axis of the stirrer corresponds with the vertical
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 th
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
´1
Designation:D2711 –01 Designation:D2711–01a (Reapproved 2007)
Standard Test Method for
Demulsibility Characteristics of Lubricating Oils
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Updated supplier footnote and 7.2 editorially in March 2009.
1. Scope
1.1 This test method covers the measurement of the ability of oil and water to separate from each other. It is intended for use
in testing medium and high-viscosity lubricating oils.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
3. Summary of Test Method
3.1 For Oils That Do Not Contain Extreme Pressure (EP)Additives—A405-mLsample of the oil and 45 mLof distilled water
are stirred together for 5 min at 82°C (180°F) in a special graduated separatory funnel. After a 5-h settling period following the
stirring, a percentage of the water in the oil and the volumes of water and emulsion separating from the oil are measured and
recorded.
3.2 For Oils That Contain Extreme Pressure (EP) Additives—A 360-mL sample of the oil and 90 mL of distilled water are
stirredtogetherfor5minat82°C(180°F)inaspecialgraduatedseparatoryfunnel.Aftera5-hsettlingperiodfollowingthestirring,
percentage of water in the oil and the volumes of water and emulsion separating from the oil are measured and recorded.
4. Significance and Use
4.1 This test provides a guide for determining the demulsibility characteristic of lubricating oils that are prone to water
contamination and may encounter the turbulence of pumping and circulation capable of producing water-in-oil emulsions.
5. Apparatus
5.1 Stirrer, constructed from parts shown in Fig. 1 and Fig. 2.
5.2 Special Graduated Separatory Funnel, as shown in Fig. 3.
5.3 Heating Bath, sufficiently large and deep to permit the immersion of at least two test separatory funnels in the bath liquid
up to their 500-mL graduation mark. The bath shall be capable of maintaining a temperature of 82 6 1°C (180 6 2°F) and shall
be so equipped to hold the separatory funnels securely in a position so that the vertical axis of the stirrer corresponds to the center
line of the separatory funnel during the mixing of the oil and water.
5.4 Centrifuge, as described in Test Method D 1796.
5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) as described in Fig. 1 of Test Method D 1796.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.L on
Industrial Lubricants.
Current edition approved August 10, 2001. Published September 2001. Originally published as D2711–68 T. Last previous edition D2711–99.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.L0.01
on Machinery Lubricants and Metal Removal Fluids.
Current edition approved July 15, 2007. Published September 2007. Originally approved in 1968. Last previous edition approved in 2001 as D 2711–01a.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
, Vol 11.01.volume information, refer to the standard’s Document Summary page on the ASTM website.
Annual Book of ASTM Standards, Vol 05.01.
Formerly available from Research Appliance Co., Moose Lodge Rd., Dept. T, Cambridge, MD 21613. Section D02.L0.01 is actively seeking a replacement supplier.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D2711–01a (2007)
FIG. 1 Stirrer
6. Materials
6.1 Cleaning Solvent—Any suitable solvent capable of cleaning and effectively removing any oil or fluid from the stirrer and
graduated cylinder. 1,1,1-Trichloroethane has been found suitable for use in this test method. (Warning— 1,1,1–Trichloroethane,
Harmful if inhaled or swallowed. Eye irritant. High concentration can cause unconsciousness or death.)
NOTE 1—In cases in which the use of 1,1,1 trichloroethane is unacceptable, some laboratories are using heptane or mineral spirits as alternative
solvents. The effect on the precision of this test method when using an alternate solvent has not been determined.
6.2 Water—Type II reagent grade water conforming to Specification D 1193.
7. Preparation of Apparatus
7.1 Clean the graduated cylinderseparatory funnel by removing any film of oil with cleaning solvent followed by a wash first
with acetone (Warning—Extremely flammable vapors may cause flash fires.) and then with tap water. Rinse thoroughly with tap
water and then with reagent grade water.
7.2 Clean the stirrer by appropriate means, using the cleaning solvent (6.1).Allow the stirrer to air dry completely prior to use
in the test. ).Allow the stirrer to air dry completely prior to use in the test. (Warning—To minimize any potential sparking hazard,
ensure that the motor is detached from any electrical source during the cleaning procedure.)
8. Procedure A for Oils That Do Not Contain EPAdditives
8.1 Heat the bath liquid to 82 6 1°C (180 6 2°F) and maintain this temperature throughout the test.
8.2 Measure the oil under test, at room temperature, directly into the separatory funnel to a volume of 405 6 5 mL. Place 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 mL of
distilled water, measured at room temperature, to the oil. Immerse the stirrer in the oil and position it carefully as follows: lower
the stirrer until it touches the bottom of the funnel, then raise it approximately 25 mm (1 in.). Ensure that the vertical axis of the
stirrer corresponds with the vertical center line of the funnel. Slowly bring the stirrer motor to a speed of 4500 6 500 rpm within
25 to 30 s, and operate for a total of 5 min, including the start-up time. Then withdraw the stirrer from the oil-water mixture but
not entirely out of the separatory funnel. Allow the stirrer to drain for 5 min, then remove from the separatory funnel and clean.
´1
D2711–01a (2007)
FIG. 2 Detailed Construction of Stirrer
8.3 Five hours after stirring has stopped, withdraw a 50-mL sample from the center of the funnel and approximately 50 mm (2
in.) below the surface of the oil-water mixture, using a 50-mLpipet. Discharge the contents of the pipet into a centrifuge tube and
determine the water present in the sample using Test Method D 1796. Record the results as “percent water in the oil.”
8.4 With minimum delay, after sampling for the “percentage of water in the oil,” remove the separatory funnel from the bath
and draw off any free water that has separated from the oil-water mixture into a 50-mL graduated cylinder. Allow this water to
reach room temperature, measure, and record the volume.
8.5 After removing the free water from the separatory funnel, reduce the volume of the fluid remaining to 100 mLby carefully
siphoning the fluid off the top (end of siphon should not be more than 20 mm below the surface of the fluid at any time) down
to the 100-mL graduation mark on the separatory funnel. Drain the remaining 100 mL of fluid (oil, water, and emulsion) directly
into a centrifuge tube.
8.6 Centrifuge the tube and its contents for a period of 10 to 15 min at a relative centrifugal force of 700. Record the volume
of water and emulsion separated by centrifuging.
8.7 Perform a minimum of two determinations on each oil sample by repeating procedure 8.1-8.6. If the difference in the two
sets of results obtained is outside the repeatability limits of Procedure A, discard them and obtain two additional sets of results.
9. Procedure B for Oils That Contain EPAdditives
9.1 Heat the bath liquid to 82 6 1 °C (180 6 2 °F) and maintain this temperature throughout the test.
9.2 Measure the oil under test, at room temperature, directly into the separatory funnel to a volume of 360 6 5 mL. Place the
separatoryfunnelandoilinaconstant-temperaturebathandbringtoatemperatureof82°C(180°F).Add90 60.5mLofdistilled
water, measured at room temperature, to the oil. Immerse the stirrer in the oil and position it carefully as follows: lower the stirrer
until it touches the bottom of the funnel, then raise it approximately 25 mm (1 in.). Ensure that the vertical axis of the stirrer
´1
D2711–01a (2007)
FIG.
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
An American National Standard
´1
Designation:D2711–01a (Reapproved 2007)
Standard Test Method for
Demulsibility Characteristics of Lubricating Oils
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 (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Updated supplier footnote and 7.2 editorially in March 2009.
1. Scope
1.1 This test method covers the measurement of the ability of oil and water to separate from each other. It is intended for use
in testing medium and high-viscosity lubricating oils.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 1193 Specification for Reagent Water
D 1796 Test Method for Water and Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)
3. Summary of Test Method
3.1 For Oils That Do Not Contain Extreme Pressure (EP)Additives—A405-mLsample of the oil and 45 mLof distilled water
are stirred together for 5 min at 82°C (180°F) in a special graduated separatory funnel. After a 5-h settling period following the
stirring, a percentage of the water in the oil and the volumes of water and emulsion separating from the oil are measured and
recorded.
3.2 For Oils That Contain Extreme Pressure (EP) Additives—A 360-mL sample of the oil and 90 mL of distilled water are
stirredtogetherfor5minat82°C(180°F)inaspecialgraduatedseparatoryfunnel.Aftera5-hsettlingperiodfollowingthestirring,
percentage of water in the oil and the volumes of water and emulsion separating from the oil are measured and recorded.
4. Significance and Use
4.1 This test provides a guide for determining the demulsibility characteristic of lubricating oils that are prone to water
contamination and may encounter the turbulence of pumping and circulation capable of producing water-in-oil emulsions.
5. Apparatus
5.1 Stirrer, constructed from parts shown in Fig. 1 and Fig. 2.
5.2 Special Graduated Separatory Funnel, as shown in Fig. 3.
5.3 Heating Bath, sufficiently large and deep to permit the immersion of at least two test separatory funnels in the bath liquid
up to their 500-mL graduation mark. The bath shall be capable of maintaining a temperature of 82 6 1°C (180 6 2°F) and shall
be so equipped to hold the separatory funnels securely in a position so that the vertical axis of the stirrer corresponds to the center
line of the separatory funnel during the mixing of the oil and water.
5.4 Centrifuge, as described in Test Method D 1796.
5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) as described in Fig. 1 of Test Method D 1796.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.L0.01
on Metal Removal Fluids and Lubricants. on Machinery Lubricants and Metal Removal Fluids.
Current edition approved July 15, 2007. Published September 2007. Originally approved in 1968. Last previous edition approved in 2001 as D 2711–01a.
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. ForAnnualBookofASTMStandards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The sole source of supply of the apparatus known to the committee at this time is Research Appliance Co., Moose Lodge Rd., Dept. T, Cambridge, MD 21613. If you
are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of
the responsible technical committee, which you may attend.
Formerly available from Research Appliance Co., Moose Lodge Rd., Dept. T, Cambridge, MD 21613. Section D02.L0.01 is actively seeking a replacement supplier.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
´1
D2711–01a (2007)
FIG. 1 Stirrer
6. Materials
6.1 Cleaning Solvent—Any suitable solvent capable of cleaning and effectively removing any oil or fluid from the stirrer and
graduated cylinder. 1,1,1-Trichloroethane has been found suitable for use in this test method. (Warning— 1,1,1–Trichloroethane,
Harmful if inhaled or swallowed. Eye irritant. High concentration can cause unconsciousness or death.)
NOTE 1—In cases in which the use of 1,1,1 trichloroethane is unacceptable, some laboratories are using heptane or mineral spirits as alternative
solvents. The effect on the precision of this test method when using an alternate solvent has not been determined.
6.2 Water—Type II reagent grade water conforming to Specification D 1193.
7. Preparation of Apparatus
7.1 Clean the graduated separatory funnel by removing any film of oil with cleaning solvent followed by a wash first with
acetone (Warning—Extremely flammable vapors may cause flash fires.) and then with tap water. Rinse thoroughly with tap water
and then with reagent grade water.
7.2 Clean the stirrer by appropriate means, using the cleaning solvent (6.1).Allow the stirrer to air dry completely prior to use
in the test. ).Allow the stirrer to air dry completely prior to use in the test. (Warning—To minimize any potential sparking hazard,
ensure that the motor is detached from any electrical source during the cleaning procedure.)
8. Procedure A for Oils That Do Not Contain EPAdditives
8.1 Heat the bath liquid to 82 6 1°C (180 6 2°F) and maintain this temperature throughout the test.
8.2 Measure the oil under test, at room temperature, directly into the separatory funnel to a volume of 405 6 5 mL. Place 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 mL of
distilled water, measured at room temperature, to the oil. Immerse the stirrer in the oil and position it carefully as follows: lower
the stirrer until it touches the bottom of the funnel, then raise it approximately 25 mm (1 in.). Ensure that the vertical axis of the
stirrer corresponds with the vertical center line of the funnel. Slowly bring the stirrer motor to a speed of 4500 6 500 rpm within
25 to 30 s, and operate for a total of 5 min, including the start-up time. Then withdraw the stirrer from the oil-water mixture but
not entirely out of the separatory funnel. Allow the stirrer to drain for 5 min, then remove from the separatory funnel and clean.
´1
D2711–01a (2007)
FIG. 2 Detailed Construction of Stirrer
8.3 Five hours after stirring has stopped, withdraw a 50-mL sample from the center of the funnel and approximately 50 mm (2
in.) below the surface of the oil-water mixture, using a 50-mLpipet. Discharge the contents of the pipet into a centrifuge tube and
determine the water present in the sample using Test Method D 1796. Record the results as “percent water in the oil.”
8.4 With minimum delay, after sampling for the “percentage of water in the oil,” remove the separatory funnel from the bath
and draw off any free water that has separated from the oil-water mixture into a 50-mL graduated cylinder. Allow this water to
reach room temperature, measure, and record the volume.
8.5 After removing the free water from the separatory funnel, reduce the volume of the fluid remaining to 100 mLby carefully
siphoning the fluid off the top (end of siphon should not be more than 20 mm below the surface of the fluid at any time) down
to the 100-mL graduation mark on the separatory funnel. Drain the remaining 100 mL of fluid (oil, water, and emulsion) directly
into a centrifuge tube.
8.6 Centrifuge the tube and its contents for a period of 10 to 15 min at a relative centrifugal force of 700. Record the volume
of water and emulsion separated by centrifuging.
8.7 Perform a minimum of two determinations on each oil sample by repeating procedure 8.1-8.6. If the difference in the two
sets of results obtained is outside the repeatability limits of Procedure A, discard them and obtain two additional sets of results.
9. Procedure B for Oils That Contain EPAdditives
9.1 Heat the bath liquid to 82 6 1 °C (180 6 2 °F) and maintain this temperature throughout the test.
9.2 Measure the oil under test, at room temperature, directly into the separatory funnel to a volume of 360 6 5 mL. Place the
separatoryfunnelandoilinaconstant-temperaturebathandbringtoatemperatureof82°C
...
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