1、Designation: D2711 10Standard Test Method forDemulsibility Characteristics of Lubricating Oils1This standard is issued under the fixed designation D2711; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the measurement of the abilityof oil and water to separate from each other. It is intended foruse in testing m
3、edium and high-viscosity lubricating oils.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of
4、the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifu
5、ge Method (Laboratory Procedure)3. Summary of Test Method3.1 For Oils That Do Not Contain Extreme Pressure (EP)AdditivesA 405-mL sample of the oil and 45 mL of distilledwater are stirred together for 5 min at 82C (180F) in a specialgraduated separatory funnel. After a 5-h settling period follow-ing
6、the stirring, a percentage of the water in the oil and thevolumes of water and emulsion separating from the oil aremeasured and recorded.3.2 For Oils That Contain Extreme Pressure (EP)AdditivesA 360-mL sample of the oil and 90 mL of distilledwater are stirred together for 5 min at 82C (180F) in a sp
7、ecialgraduated separatory funnel. After a 5-h settling period follow-ing the stirring, percentage of water in the oil and the volumesof water and emulsion separating from the oil are measured andrecorded.4. Significance and Use4.1 This test provides a guide for determining the demulsi-bility charact
8、eristic of lubricating oils that are prone to watercontamination and may encounter the turbulence of pumpingand circulation capable of producing water-in-oil emulsions.5. Apparatus5.1 Stirrer, constructed from parts shown in Fig. 1 and Fig.2.NOTE 1An air pressure driven motor is suggested to avoid a
9、nypotential electrical sparking hazard.5.2 Special Graduated Separatory Funnel, as shown in Fig.3.5.3 Heating Bath, sufficiently large and deep to permit theimmersion of at least two test separatory funnels in the bathliquid up to their 500-mL graduation mark. The bath shall becapable of maintaining
10、 a temperature of 82 6 1C (180 6 2F)and shall be so equipped to hold the separatory funnelssecurely in a position so that the vertical axis of the stirrercorresponds to the center line of the separatory funnel duringthe mixing of the oil and water.NOTE 2The use of silicone oil as a bath medium is di
11、scouraged, sinceany contamination into the oil/water mixture may cause erroneous results.5.4 Centrifuge, as described in Test Method D1796.5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) asdescribed in Fig. 1 of Test Method D1796.6. Materials6.1 Cleaning SolventAny suitable solvent capable of
12、cleaning and effectively removing any oil or fluid from thestirrer and graduated cylinder. 1,1,1-Trichloroethane has beenfound suitable for use in this test method. (Warning1,1,1Trichloroethane, Harmful if inhaled or swallowed. Eyeirritant. High concentration can cause unconsciousness ordeath.)NOTE
13、3In cases in which the use of 1,1,1 trichloroethane is unac-ceptable, some laboratories are using heptane or mineral spirits asalternative solvents. The effect on the precision of this test method whenusing an alternate solvent has not been determined.6.2 WaterType II reagent grade water conforming
14、toSpecification D1193.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.L0.01 on Machinery Lubricants and Metal Removal Fluids.Current edition approved May 1, 2010. Published June 2010. Originally
15、approved in 1968. Last previous edition approved in 2007 as D271101a(2007)1.DOI: 10.1520/D2711-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Docu
16、ment Summary page onthe ASTM website.1*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.7. Preparation of Apparatus7.1 Clean the graduated separatory funnel by removing a
17、nyfilm of oil with cleaning solvent followed by a wash first withacetone (WarningExtremely flammable vapors may causeflash fires.) and then with tap water. Rinse thoroughly with tapwater and then with reagent grade water.7.2 Clean the stirrer by appropriate means, using the clean-ing solvent (6.1).
18、Allow the stirrer to air dry completely priorto use in the test. (WarningTo minimize any potentialsparking hazard, ensure that the motor is detached from anyelectrical source during the cleaning procedure.)8. Procedure A for Oils That Do Not Contain EPAdditives8.1 Heat the bath liquid to 82 6 1C (18
19、0 6 2F) andmaintain this temperature throughout the test.8.2 Measure the oil under test, at room temperature, directlyinto the separatory funnel to a volume of 405 6 5 mL. Placethe separatory funnel and oil in the constant-temperature bathand bring it to a temperature of 82C (180F). Add 45 6 0.5mL o
20、f distilled water, measured at room temperature, to the oil.Immerse the stirrer in the oil and position it carefully asfollows: lower the stirrer until it touches the bottom of thefunnel, then raise it approximately 25 mm (1 in.). Ensure thatthe vertical axis of the stirrer corresponds with the vert
21、icalcenter line of the funnel. Slowly bring the stirrer motor to aspeed of 4500 6 500 rpm within 25 to 30 s, and operate for atotal of 5 min, including the start-up time. Then withdraw thestirrer from the oil-water mixture but not entirely out of theseparatory funnel. Allow the stirrer to drain for
22、5 min, thenremove from the separatory funnel and clean.NOTE 4It is critical that silcone grease not be used on the stopcock.Use either PTFE (polytetrafluoroethlyene) stopcocks, or use the test oil orother non-silicone containing material as the lubricant for the stopcock.NOTE 5Starting the stirrer a
23、ny more quickly than suggested maycause erroneous results.8.3 Five hours after stirring has stopped, withdraw a 50-mLsample from the center of the funnel and approximately 50 mm(2 in.) below the surface of the oil-water mixture, using a50-mL pipet. Discharge the contents of the pipet into acentrifug
24、e tube and determine the water present in the sampleusing Test Method D1796. Record the volume of water in thecentrifuge tube.8.4 With minimum delay, remove the separatory funnelfrom the bath and draw off any free water that has separatedfrom the oil-water mixture into a 50-mL graduated cylinder.All
25、ow this water to reach room temperature, measure, andrecord the volume.8.5 After removing the free water from the separatoryfunnel, reduce the volume of the fluid remaining to 100 mL byFIG. 1 StirrerD2711 102carefully siphoning the fluid off the top (end of siphon shouldnot be more than 20 mm below
26、the surface of the fluid at anytime) down to the 100-mL graduation mark on the separatoryfunnel. Drain the remaining 100 mL of fluid (oil, water, andemulsion) directly into a centrifuge tube.8.6 Centrifuge the tube and its contents for a period of 10 to15 min at a relative centrifugal force of 700.
27、Record thevolume of water and emulsion separated by centrifuging.8.7 Perform a minimum of two determinations on each oilsample by repeating procedure 8.1-8.6. If the difference in thetwo sets of results obtained is outside the repeatability limits ofProcedure A, discard them and obtain two additiona
28、l sets ofresults.9. Procedure B for Oils That Contain EP Additives9.1 Heat the bath liquid to 82 6 1 C (180 6 2 F) andmaintain this temperature throughout the test.9.2 Measure the oil under test, at room temperature, directlyinto the separatory funnel to a volume of 360 6 5 mL. Placethe separatory f
29、unnel and oil in a constant-temperature bathand bring to a temperature of 82 C (180 F).Add 90 6 0.5 mLof distilled water, measured at room temperature, to the oil.Immerse the stirrer in the oil and position it carefully asfollows: lower the stirrer until it touches the bottom of thefunnel, then rais
30、e it approximately 25 mm (1 in.). Ensure thatthe vertical axis of the stirrer corresponds with the verticalcenter line of the funnel. Slowly bring the stirrer motor to aspeed of 2500 6 250 rpm within 25 to 30 s, and operate for atotal of 5 min, including the start-up time (Note 7). Thenwithdraw the
31、stirrer from the oil-water mixture but not entirelyout of the separatory funnel. Allow the stirrer to drain for 5min, then remove it from the separatory funnel and clean.NOTE 6Starting the stirrer any more quickly than suggested maycause erroneous results.9.3 Five hours after stirring has stopped, w
32、ithdraw a 50-mLsample from the center of the funnel approximately 50 mm (2in.) below the surface of the oil-water mixture, using a 50-mLpipette. Discharge the contents of the pipet into a centrifugetube and determine the water present in the sample using TestMethod D1796. Record the volume of water
33、in the centrifugetube.FIG. 2 Detailed Construction of StirrerD2711 1039.4 With minimum delay, remove the separatory funnelfrom the bath and draw off any free water that has separatedfrom the oil-water mixture into a 100-mL graduated cylinder.Allow this water to reach room temperature, measure, andre
34、cord the volume.9.5 After removing the free water from the separatoryfunnel, reduce the volume of the fluid remaining to 100 mL bycarefully siphoning the fluid off the top (end of siphon shouldnot be more than 20 mm below the surface of the fluid at anytime) down to the 100-mL graduation mark on the
35、 separatoryfunnel. Drain the remaining 100 mL of fluid (oil, water andemulsion) directly into a centrifuge tube.9.6 Centrifuge the tube and its contents for a period of 10 to15 min at a relative centrifugal force of 700. Record thevolume of water and emulsion separated by centrifuging.9.7 Perform a
36、minimum of two determinations on each oilsample by repeating procedure 9.1-9.3. If the difference in thetwo sets of results obtained is outside the repeatability limits ofProcedure B, discard them and obtain two additional sets ofresults.NOTE 7The stirring motor may slow down when testing high-visco
37、sity or emulsion-forming oils. Check speed frequently during the5-min stirring period and adjust as necessary.10. Calculation and Report10.1 Report the procedure used, that is, Procedure A orProcedure B.10.2 Calculate the percentage of water in oil as follows:% water in oil 5 23 volume of water in t
38、he centrifuge tube (1)(see 8.3 or 9.3).10.2.1 If the percent water in oil is less than 0.1 %, report as6.0 4.0 5.6 18 ;23 22 57 ;96AEstimated from inspection of data.D2711 105FIG. X1.1 Sampling Gage and Centering DeviceFIG. X1.2 Device to Reduce Volume in Separatory FunnelFIG. X1.3 Pressure DeviceD2
39、711 106SUMMARY OF CHANGESSubcommittee D02.L0 has identified the location of selected changes to this standard since the last issue(D271101a(2007)1) that may impact the use of this standard.(1) Updated availability information for apparatus. Added airpressure driven motor.(2) Clarified steps in the P
40、rocedure with notes.(3) Updated Calculation and Report section.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such
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43、air hearing you shouldmake 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 s
44、tandard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).FIG. X1.4 Optional EquipmentD2711 107