ASTM D2711-2017 Standard Test Method for Demulsibility Characteristics of Lubricating Oils《润滑油抗乳化性能的标准试验方法》.pdf

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1、Designation: D2711 11D2711 17Standard 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 revi

2、sion. A 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 ability of oil and water to separate from each other. It is intended for usein

3、testing medium and high-viscosity lubricating oils.1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the respon

4、sibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.1.4 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the

5、Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1796 Test Method for Water and Sediment

6、 in Fuel Oils by the Centrifuge Method (Laboratory Procedure)D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants3. Terminology3.1 Definitions:3.1.1 demulsibility, nin petroleum products, the ability of a mixture of liquids (usually hydrocarbons and water) to separateinto i

7、ts components after the mixture has been vigorously agitated. D41754. Summary of Test Method4.1 For Oils That Do Not Contain Extreme Pressure (EP) AdditivesA 405-mL405 mL sample of the oil and 45 mL 45 mLof distilled water are stirred together for 5 min 5 min at 82C82 C in a special graduated separa

8、tory funnel.After a 5-h5 h settlingperiod following the stirring, a percentage of the water in the oil and the volumes of water and emulsion separating from the oilare measured and recorded.4.2 For Oils That Contain Extreme Pressure (EP) AdditivesA360-mL360 mL sample of the oil and 90 mL 90 mL of di

9、stilledwater are stirred together for 5 min 5 min at 82C82 C in a special graduated separatory funnel. After a 5-h5 h settling periodfollowing the stirring, percentage of water in the oil and the volumes of water and emulsion separating from the oil are measuredand recorded.5. Significance and Use5.

10、1 This test provides a guide for determining the demulsibility characteristic of lubricating oils that are prone to watercontamination and may encounter the turbulence of pumping and circulation capable of producing water-in-oil emulsions.1 This test method is under the jurisdiction ofASTM Committee

11、 D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.L0.01 on Metal Removal Fluids and Lubricants.Current edition approved Oct. 1, 2011June 1, 2017. Published November 2011June 2017. Originally approved in 1968. Last previous edition approved i

12、n 20102011 asD2711D2711 11.10. DOI: 10.1520/D2711-11.10.1520/D2711-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM

13、 website.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. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult

14、prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA

15、19428-2959. United States16. Apparatus6.1 Stirrer, constructed from parts shown in Figs. 1-3.NOTE 1An air pressure driven motor is suggested to avoid any potential electrical sparking hazard.6.2 Special Graduated Separatory Funnel, as shown in Fig. 4.6.3 Heating Bath, sufficiently large and deep to

16、permit the immersion of at least two test separatory funnels in the bath liquidup to their 500-mL500 mL graduation mark. The bath shall be capable of maintaining a temperature of 8282 C 6 1C1 C andshall be so equipped to hold the separatory funnels securely in a position so that the vertical axis of

17、 the stirrer corresponds to thecenter line of the separatory funnel during the mixing of the oil and water.NOTE 2The use of silicone oil as a bath medium is discouraged, since any contamination into the oil/water mixture may cause erroneous results.6.4 Centrifuge, as described in Test Method D1796.6

18、.5 Centrifuge Tubes, long-form, 195195 mm to 203 mm as described in Fig. 1 of Test Method D1796.7. Materials7.1 Cleaning SolventAny suitable solvent capable of cleaning and effectively removing any oil or fluid from the stirrer andgraduated cylinder. 1,1,1-Trichloroethane has been found suitable for

19、 use in this test method. (WarningWarning1,1,1Trichloroethane, Harmful if inhaled or swallowed. Eye irritant. High concentration can cause unconsciousness or death.)NOTE 3In cases in which the use of 1,1,1 trichloroethane is unacceptable, some laboratories are using heptane or mineral spirits as alt

20、ernativesolvents. The effect on the precision of this test method when using an alternate solvent has not been determined.7.2 WaterType II reagent grade water conforming to Specification D1193.8. Preparation of Apparatus8.1 Clean the graduated separatory funnel by removing any film of oil with clean

21、ing solvent followed by a wash first withacetone (WarningWarningExtremely flammable vapors may cause flash fires. Use of a sparkless motor recommended) andthen with tap water. Rinse thoroughly with tap water and then with reagent grade water.8.2 Clean the stirrer by appropriate means, using the clea

22、ning solvent (6.17.1). Allow the stirrer to air dry completely prior touse in the test. (WarningTo minimize any potential sparking hazard, ensure that the motor is detached from any electrical sourceduring the cleaning procedure.)FIG. 1 StirrerD2711 1729. Procedure A for Oils That Do Not Contain EPA

23、dditives9.1 Heat the bath liquid to 8282 C 6 1C1 C 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 405405 mL 6 5 mL.5 mL. Place the separatory funnel and oil in the constant-temperature bath and

24、 bring it to a temperature of 82C.82 C. Add4545 mL 6 0.5 mL 0.5 mL of distilled water, measured at room temperature, to the oil. Immerse the stirrer in the oil and positionit carefully as follows: lower the stirrer until it touches the bottom of the funnel, then raise it approximately 25 mm. 25 mm.

25、Ensurethat the vertical axis of the stirrer corresponds with the vertical center line of the funnel. Slowly bring the stirrer motor to a speedNOTE 1All dimensions are in millimetres.FIG. 2 Detailed Construction of Stirrer, Part 1NOTE 1All dimensions are in millimetres.FIG. 3 Detailed Construction of

26、 Stirrer, Part 2D2711 173NOTE 1Stopcock placed as close to tube body as possible.FIG. 4 Graduated Separatory FunnelD2711 174of 45004500 rmin 6 500500 r rpm min within 2525 s to 30 s, 30 s, and operate for a total of 5 min, 5 min, including the start-uptime. Then withdraw the stirrer from the oil-wat

27、er mixture but not entirely out of the separatory funnel. Allow the stirrer to drainfor 5 min, 5 min, then remove 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 or oth

28、ernon-silicone containing material as the lubricant for the stopcock.NOTE 5Starting the stirrer any more quickly than suggested may cause erroneous results.9.3 Five hours after stirring has stopped, withdraw a 50-mL50 mL sample from the center of the funnel and approximately 50mm 50 mm below the sur

29、face of the oil-water mixture, using a 50-mL50 mL pipet. Discharge the contents of the pipet into acentrifuge tube and determine the water present in the sample using Test Method D1796. Record the volume of water in thecentrifuge tube.9.4 With minimum delay, remove the separatory funnel from the bat

30、h and draw off any free water that has separated from theoil-water mixture into a 50-mL50 mL graduated cylinder. Allow this water to reach room temperature, measure, and record thevolume.9.5 After removing the free water from the separatory funnel, reduce the volume of the fluid remaining to 100 mL

31、100 mL bycarefully siphoning the fluid off the top (end of siphon should not be more than 20 mm 20 mm below the surface of the fluid atany time) down to the 100-mL100 mLgraduation mark on the separatory funnel. Drain the remaining 100 mL100 mLof fluid (oil,water, and emulsion) directly into a centri

32、fuge tube.9.6 Centrifuge the tube and its contents for a period of 1010 min to 15 min 15 min at a relative centrifugal force of 700. Recordthe volume of water and emulsion separated by centrifuging.9.7 Perform a minimum of two determinations on each oil sample by repeating procedure 8.19.1 8.69.6. I

33、f the difference inthe two sets of results obtained is outside the repeatability limits of Procedure A, discard them and obtain two additional sets ofresults.10. Procedure B for Oils That Contain EPAdditives10.1 Heat the bath liquid to 8282 C 6 1C1 C and maintain this temperature throughout the test

34、.10.2 Measure the oil under test, at room temperature, directly into the separatory funnel to a volume of 360360 mL 6 5 mL.5 mL. Place the separatory funnel and oil in a constant-temperature bath and bring to a temperature of 82C.82 C. Add 9090 mL6 0.5 mL0.5 mLof distilled water, measured at room te

35、mperature, to the oil. Immerse the stirrer in the oil and position it carefullyas follows: lower the stirrer until it touches the bottom of the funnel, then raise it approximately 25 mm. 25 mm. Ensure that thevertical axis of the stirrer corresponds with the vertical center line of the funnel. Slowl

36、y bring the stirrer motor to a speed of25002500 rmin 6 250250 r rpm min within 2525 s to 30 s, 30 s, and operate for a total of 5 min, 5 min, including the start-uptime (Note 7). Then withdraw the stirrer from the oil-water mixture but not entirely out of the separatory funnel. Allow the stirrerto d

37、rain for 5 min, 5 min, then remove it from the separatory funnel and clean.NOTE 6Starting the stirrer any more quickly than suggested may cause erroneous results.10.3 Five hours after stirring has stopped, withdraw a 50-mL50 mL sample from the center of the funnel approximately 50 mm50 mm below the

38、surface of the oil-water mixture, using a 50-mL50 mL pipette. Discharge the contents of the pipet into acentrifuge tube and determine the water present in the sample using Test Method D1796. Record the volume of water in thecentrifuge tube.10.4 With minimum delay, remove the separatory funnel from t

39、he bath and draw off any free water that has separated from theoil-water mixture into a 100-mL100 mL graduated cylinder. Allow this water to reach room temperature, measure, and record thevolume.10.5 After removing the free water from the separatory funnel, reduce the volume of the fluid remaining t

40、o 100 mL 100 mL bycarefully siphoning the fluid off the top (end of siphon should not be more than 20 mm 20 mm below the surface of the fluid atany time) down to the 100-mL100 mLgraduation mark on the separatory funnel. Drain the remaining 100 mL100 mLof fluid (oil,water and emulsion) directly into

41、a centrifuge tube.10.6 Centrifuge the tube and its contents for a period of 1010 min to 15 min 15 min at a relative centrifugal force of 700. Recordthe volume of water and emulsion separated by centrifuging.10.7 Perform a minimum of two determinations on each oil sample by repeating procedure 9.110.

42、1 9.310.3. If the differencein the two sets of results obtained is outside the repeatability limits of Procedure B, discard them and obtain two additional setsof results.NOTE 7The stirring motor may slow down when testing high-viscosity or emulsion-forming oils. Check speed frequently during the 5-m

43、in5 minstirring period and adjust as necessary. PID motor controller with feedback recommended.D2711 17511. Calculation and Report11.1 Report the procedure used, that is, Procedure A or Procedure B.11.2 Calculate the percentage of water in oil as follows:%water in oil5volume mL!of water in centrifug

44、e tube/50 mL3100 (1)(see 8.39.3 or 9.310.3).11.2.1 If the percent water in oil is less than 0.1 %, report as 6.0 4.0 5.6 18 ;23 22 57 ;96A Estimated from inspection of data.D2711 17614. Bias14.1 The procedure in Test Method D2711 has no bias because the values of total free water and emulsion can be

45、 defined onlyin terms of a test method.15. Keywords15.1 demulsibility; water contamination; water/oil separationAPPENDIX(Nonmandatory Information)X1. APPARATUSX1.1 Gage and Centering Device,Fig. X1.1 is an aid in obtaining the 50-mL50 mL samples from the separatory funnel for the“percent water in th

46、e oil” determination (8.39.3).X1.2 Fig. X1.2 illustrates a rapid method for reducing the volume of fluid remaining in the separatory funnel to 100 mL 100 mLby siphoning the fluid off the top (end of siphon shall be not more than 34 in. (20 mm) in. (20 mm) below the surface of the fluidat any time) d

47、own to the 100-mL100 mL graduation mark on the separatory funnel (8.59.5).X1.2.1 The time required to drain the 100 mL 100 mL of fluid from the separatory funnel into the centrifuge tube can be reduced,especially in the case of high-viscosity oils or the presence of a “mayonnaise”-type emulsion, by

48、applying a slight amount ofpressure (Fig. X1.3) to the open end of the separatory funnel to force the flow of the oil or emulsion, or both, into the centrifugetube.X1.3 Fig. X1.4(a) shows a suggested container for the solvent used to clean the stirrer after mixing the oil and water (8.29.2) andFig.

49、X1.4(b) shows a suggested method for air drying the stirrer after the above (solvent) washing.D2711 177D2711 178NOTE 1All dimensions are in millimetres.D2711 179FIG. X1.1 Sampling Gage and Centering DeviceFIG. X1.2 Device to Reduce Volume in Separatory FunnelFIG. X1.3 Pressure DeviceD2711 1710SUMMARY OF CHANGESSubcommittee D02.L0 has identified the location of selected changes to this standard since the last issue(D2711D2711 1111) that may impact the use of this standard. (Approved June 1, 2017.)(1) Corrected Eq