ASTM D2711-2011 Standard Test Method for Demulsibility Characteristics of Lubricating Oils《润滑油抗乳化特性的标准试验方法》.pdf

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1、Designation: D2711 11Standard 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 asstandard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of t

4、he 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 Centrifug

5、e 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 in a specialgraduated separatory funnel. After a 5-h settling period follow-ing the stir

6、ring, 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 in a specialgraduated

7、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 characteristic of lubr

8、icating 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 Figs. 1-3.NOTE 1An air pressure driven motor is suggested to avoid anypotential electrical

9、 sparking hazard.5.2 Special Graduated Separatory Funnel, as shown in Fig.4.5.3 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 a temperature of 82 6

10、 1C and shall beso equipped to hold the separatory funnels securely in aposition so that the vertical axis of the stirrer corresponds to thecenter line of the separatory funnel during the mixing of the oiland water.NOTE 2The use of silicone oil as a bath medium is discouraged, sinceany contamination

11、 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 as de-scribed in Fig. 1 of Test Method D1796.6. Materials6.1 Cleaning SolventAny suitable solvent capable ofcleaning and effectively removing any o

12、il 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 3In cases in which the use of 1,1,1 tri

13、chloroethane is unac-ceptable, some laboratories are using heptane or mineral spirits as1This 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.Cur

14、rent edition approved Oct. 1, 2011. Published November 2011. Originallyapproved in 1968. Last previous edition approved in 2010 as D271110. DOI:10.1520/D2711-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book o

15、f ASTMStandards volume information, refer to the standards Document 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.alternative solvent

16、s. 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 D1193.7. Preparation of Apparatus7.1 Clean the graduated separatory funnel by removing anyfilm of oil with cleaning solvent follow

17、ed by a wash first withacetone (WarningExtremely flammable vapors may causeflash fires. Use of a sparkless motor recommended) and thenwith tap water. Rinse thoroughly with tap water and then withreagent grade water.7.2 Clean the stirrer by appropriate means, using the clean-ing solvent (6.1). Allow

18、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 and maint

19、ain thistemperature 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. Add 45 6 0.5 mL ofdistilled water, measu

20、red 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. Ensure that thevertical axis of the stirrer corresponds with the vertical centerline of the funnel. S

21、lowly bring the stirrer motor to a speed of4500 6 500 rpm within 25 to 30 s, and operate for a total of 5min, including the start-up time. Then withdraw the stirrerfrom the oil-water mixture but not entirely out of the separatoryfunnel. Allow the stirrer to drain for 5 min, then remove fromthe separ

22、atory 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 any more quickly than suggested m

23、aycause erroneous results.8.3 Five hours after stirring has stopped, withdraw a 50-mLsample from the center of the funnel and approximately 50 mmbelow the surface of the oil-water mixture, using a 50-mLpipet. Discharge the contents of the pipet into a centrifuge tubeand determine the water present i

24、n the sample using TestMethod D1796. Record the volume of water in the centrifugetube.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.Allow this water to reach room temperature,

25、 measure, andrecord the volume.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 fluid at anytime) down to the 100-mL graduat

26、ion mark on the separatoryFIG. 1 StirrerD2711 112funnel. 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. Record thevolume of water and emulsion s

27、eparated 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 additional sets ofresults.9. Procedure B for Oils

28、 That Contain EP Additives9.1 Heat the bath liquid to 82 6 1C and maintain thistemperature throughout the test.NOTEAll dimensions are in millimetres.FIG. 2 Detailed Construction of Stirrer, Part 1NOTEAll dimensions are in millimetres.FIG. 3 Detailed Construction of Stirrer, Part 2D2711 113NOTEStopco

29、ck placed as close to tube body as possible.FIG. 4 Graduated Separatory FunnelD2711 1149.2 Measure the oil under test, at room temperature, directlyinto the separatory funnel to a volume of 360 6 5 mL. Placethe separatory funnel and oil in a constant-temperature bathand bring to a temperature of 82C

30、. Add 90 6 0.5 mL ofdistilled 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. Ensure that thevertical axis of the stirrer corresponds wit

31、h the vertical centerline of the funnel. Slowly bring the stirrer motor to a speed of2500 6 250 rpm within 25 to 30 s, and operate for a total of 5min, including the start-up time (Note 7). Then withdraw thestirrer from the oil-water mixture but not entirely out of theseparatory funnel. Allow the st

32、irrer to drain for 5 min, thenremove 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, withdraw a 50-mLsample from the center of the funnel approximately 50 mmbelow the surface of t

33、he 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 in the centrifugetube.9.4 With minimum delay, remove the separatory funnelfrom the bath and draw off

34、any free water that has separatedfrom the oil-water mixture into a 100-mL graduated cylinder.Allow this water to reach room temperature, measure, andrecord the volume.9.5 After removing the free water from the separatoryfunnel, reduce the volume of the fluid remaining to 100 mL bycarefully siphoning

35、 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 separatoryfunnel. Drain the remaining 100 mL of fluid (oil, water andemulsion) directly into a centrifuge tube.9.6 Centrifuge the tube and its conte

36、nts 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 determinations on each oilsample by repeating procedure 9.1-9.3. If the difference in thetwo sets of results obtained is outside the r

37、epeatability limits ofProcedure B, discard them and obtain two additional sets ofresults.NOTE 7The stirring motor may slow down when testing high-viscosity or emulsion-forming oils. Check speed frequently during the5-min stirring period and adjust as necessary. PID motor controller withfeedback reco

38、mmended.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 volume mL! of water in centrifuge tube / 50 mL!3 100 (1)(see 8.3 or 9.3).10.2.1 If the percent water in oil is less than 0.1

39、%, report as6.0 4.0 5.6 18 ;23 22 57 ;96AEstimated from inspection of data.D2711 116NOTEAll dimensions are in millimetres.FIG. X1.1 Sampling Gage and Centering DeviceFIG. X1.2 Device to Reduce Volume in Separatory FunnelD2711 117SUMMARY OF CHANGESSubcommittee D02.L0 has identified the location of se

40、lected changes to this standard since the last issue(D271111) that may impact the use of this standard.(1) Corrected Eq 1.(2) Added motor controller recommendation in Note 7.(3) Deleted inch-pound units throughout.(4) Expanded warning information in 7.1.(5) Reworked all figures.FIG. X1.3 Pressure De

41、viceFIG. X1.4 Optional EquipmentD2711 118ASTM 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 patent rights, and th

42、e riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by 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 o

43、f this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive 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 should

44、make 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 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D2711 119