ASTM D2711-2001a(2007)e1 Standard Test Method for Demulsibility Characteristics of Lubricating Oils.pdf

1、Designation: D 2711 01a (Reapproved 2007)1An American National StandardStandard Test Method forDemulsibility Characteristics of Lubricating Oils1This standard is issued under the fixed designation D 2711; the number immediately following the designation indicates the year oforiginal adoption or, in

2、the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEUpdated supplier footnote and 7.2 editorially in March 2009.1. Scope1.1 This test method co

3、vers the measurement of the abilityof oil and water to separate from each other. It is intended foruse in testing medium 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

4、does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of 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 S

5、tandards:2D 1193 Specification for Reagent WaterD 1796 Test Method for Water and Sediment in Fuel Oils bythe Centrifuge 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 stir

6、red together for 5 min at 82C (180F) in a specialgraduated separatory funnel. After a 5-h settling period follow-ing 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

7、)AdditivesA 360-mL sample of the oil and 90 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 the stirring, percentage of water in the oil and the volumesof water and emulsion separating from the oil are

8、measured andrecorded.4. Significance and Use4.1 This test provides a guide for determining the demulsi-bility characteristic 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

9、 Stirrer,3constructed from parts shown in Fig. 1 and Fig.2.5.2 Special Graduated Separatory Funnel,3as shown inFig. 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 beca

10、pable of maintaining 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.5.4 Centrifuge, as described in

11、Test Method D 1796.5.5 Centrifuge Tubes, long-form, 195 to 203 mm (8 in.) asdescribed in Fig. 1 of Test Method D 1796.6. Materials6.1 Cleaning SolventAny suitable solvent capable ofcleaning and effectively removing any oil or fluid from thestirrer and graduated cylinder. 1,1,1-Trichloroethane has be

12、enfound suitable for use in this test method. (Warning1,1,1Trichloroethane, Harmful if inhaled or swallowed. Eyeirritant. High concentration can cause unconsciousness ordeath.)NOTE 1In cases in which the use of 1,1,1 trichloroethane is unac-ceptable, some laboratories are using heptane or mineral sp

13、irits 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 toSpecification D 1193.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubri

14、cants and is the direct responsibility of SubcommitteeD02.L0.01 on Machinery Lubricants and Metal Removal Fluids.Current edition approved July 15, 2007. Published September 2007. Originallyapproved in 1968. Last previous edition approved in 2001 as D 271101a.2For referenced ASTM standards, visit the

15、 ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Formerly available from Research Appliance Co., Moose Lodge Rd., Dept. T,Cambridge, MD 21613. Section

16、 D02.L0.01 is actively seeking a replacementsupplier.1Copyright 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 anyfilm of oil with cleaning solvent followed by a

17、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). Allow the stirrer to air dry completely priorto us

18、e 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 (180 6 2F) andmaintain this temperature throughout th

19、e 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 of distilled water, measured at room temperature, t

20、o 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 verticalcenter line of the funnel. Slowly bring the st

21、irrer 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 5 min, thenremove from the separatory funnel and c

22、lean.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 acentrifuge tube and determine the water present in the sampleu

23、sing Test Method D 1796. Record the results as “percentwater in the oil.”8.4 With minimum delay, after sampling for the “percentageof water in the oil,” remove the separatory funnel from the bathand draw off any free water that has separated from theoil-water mixture into a 50-mL graduated cylinder.

24、 Allow thiswater to reach room temperature, measure, and record thevolume.8.5 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 f

25、luid at anytime) down to the 100-mL graduation mark on the separatoryFIG. 1 StirrerD 2711 01a (2007)12funnel. 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 f

26、orce of 700. 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

27、two additional 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

28、 separatory funnel 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 thefunn

29、el, then raise 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 2). Then

30、withdraw the 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.9.3 Five hours after stirring has stopped, withdraw a 50-mLsample from the center of the funnel approximately 50 mm (

31、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 D 1796. Record the results as “percent water in theoil.”9.4 Immediately after sampling for the “percentage

32、of waterin the oil,” remove the separatory funnel from the bath anddraw off any free water that has separated from the oil-watermixture into a 100-mL graduated cylinder. Allow this water toreach room temperature, measure, and record the volume.FIG. 2 Detailed Construction of StirrerD 2711 01a (2007)

33、139.5 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 separatoryfun

34、nel. 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 minimum of two

35、 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 2The stirring motor may slow down when testing high-viscosity or emusli

36、on-forming oils. Check speed frequently during the5-min stirring period and adjust as necessary.10. Report10.1 Report the procedure used, that is, Procedure A orProcedure B.10.2 Report the “percentage of water in the oil,” (Note 3)“total millilitres of free water” (Note 4) and the “millilitres ofemu

37、lsion” separated by centrifuging, for each determinationand the average of each observation for all determinations.These are necessary factors in determining the demulsibilitycharacteristics of a lubricating oil.NOTE 3Percent water in oil, record water present in amounts less than0.1 % as 6.0 4.0 5.

38、6 18 ;23 22 57 ;96AEstimated from inspection of data.D 2711 01a (2007)15FIG. X1.1 Sampling Gage and Centering DeviceFIG. X1.2 Device to Reduce Volume in Separatory FunnelFIG. X1.3 Pressure DeviceD 2711 01a (2007)16ASTM International takes no position respecting the validity of any patent rights asse

39、rted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by

40、 the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will recei

41、ve careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM Inter

42、national, 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 aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).FIG. X1.4 Optional EquipmentD 2711 01a (2007)17