1、Designation: D 6922 03An American National StandardStandard Test Method forDetermination of Homogeneity and Miscibility in AutomotiveEngine Oils1This standard is issued under the fixed designation D 6922; 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination if an automo-tive engine oil is homogeneo
3、us and will remain so, and if it ismiscible with certain standard reference oils after being sub-mitted to a prescribed cycle of temperature changes. This testmethod is very similar to the homogeneity and miscibility testdescribed in FEDSTD791/3470.1.1.2 The values stated in SI units are to be regar
4、ded 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 the user of this standard to establish appro-priate safety and health practices and determi
5、ne the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:D 97 Test Method for Pour Point of Petroleum Products2D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products3D 5844 Test Method for Evaluation of Automotive EngineOils for Inhibitio
6、n of Rusting (Sequence IID)4D 6557 Test Method for Evaluation of Rust PreventiveCharacteristics of Automotive Engine Oils5E 1 Specification for ASTM Thermometers6E 344 Terminology Relating to Thermometry and Hydrom-etry62.2 Federal Test Method Standard:FEDSTD791/3470.1 Homogeneity and Miscibility of
7、Oils73. Terminology3.1 Definitions:3.1.1 calibrate, vto determine the indication or output ofa measuring device with the respect of that of a standard.E 3443.1.2 homogeneity, nthe ability of a test oil itself toremain the same in appearance throughout (uniform) aftersubmission to a series of tempera
8、ture changes.3.1.3 miscibility, nthe ability of a reference oil and test oilto form a uniform mixture after blending and not separate intotwo phases after submission to a series of temperature changes.3.1.4 reference oil, nan oil of known performance char-acteristics, used as a basis for comparison.
9、3.1.4.1 DiscussionReference oils are used to calibratetesting facilities, to compare the performance of other oils, orto evaluate other materials (such as seals) that interact withoils. D 58443.1.5 specimen, na piece or portion of test oil used tomake a test.3.1.6 test oil, nany oil subjected to eva
10、luation in anestablished procedure. D 65574. Summary of Test Method4.1 Visual color determinations and observations are madeon an undiluted test oil specimen, along with six blends of thesame test oil that have been combined with specific referenceoils. The pour point is then determined for the undi
11、luted test oilspecimen and the six blends. The undiluted test oil specimenand six blends are then allowed to warm to room temperature.Color determinations and observations are again made on theundiluted test oil specimen and six blends. The undiluted testoil specimen and six blends are heated to 232
12、C, then allowedto cool to room temperature, and then stored at their pour pointtemperatures for 18 to 24 h. The undiluted test oil specimenand six blends are then allowed to thaw and a series of colordeterminations and observations are made as they reach roomtemperature. All data are recorded on a r
13、eport form.5. Significance and Use5.1 It is important that engine oils from different manufac-turers be homogeneous and miscible with each other, becauseoperators of automotive engines often do not have prior1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and L
14、ubricants and is the direct responsibility of SubcommitteeD02.B0 on Automotive Lubricants.Current edition approved June 10, 2003. Published July 2003.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 05.02.4Annual Book of ASTM Standards, Vol 05.03.5Annual Book of ASTM Sta
15、ndards, Vol 05.04.6Annual Book of ASTM Standards, Vol 14.03.7Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United State
16、s.knowledge of the manufacturer of the oil that is currently usedin their application, and engine failure can occur if oils arecombined that do not stay homogeneous and function properly.6. Apparatus6.1 Test Jarcylindrical, of clear glass, flat bottom, 33.2 to34.8-mm outside diameter, and 115 to 125
17、 mm in height. Theinside diameter of the jar can range from 30.0 to 32.4 mm,within the constraint that the wall thickness be no greater than1.6 mm. The jar shall have a line to indicate a sample height563 mm above the inside bottom.6.2 ThermometersASTM 6C, calibrated with a range of80 to +20C, confo
18、rming to Specification E 1.6.3 Stoppersclean stoppers, some unbored and otherscentrally bored for test thermometers.6.4 Jacketa glass or metal, water tight, cylindrical formwith a flat bottom and approximately 120 mm in depth. Theinside diameter of the jacket shall be 9.0 to 12.0 mm greaterthan the
19、outside diameter of the test jar.6.5 Diskcork or felt, about 6 mm in thickness and of thesame diameter as the inside of the jacket.6.6 Gasketa ring gasket, about 5.0 mm in thickness, to fitsnugly around the outside of the test jar and loosely inside thejacket. The purpose of the ring gasket is to pr
20、event the test jarfrom touching the jacket.6.7 Batha liquid cooling bath suitable to obtain therequired temperatures.6.8 Ovena constant temperature oven suitable to obtainthe required temperatures.6.9 Automated Pour Point Tester (Alternative)There areautomated pour point testers available and in use
21、 which may beadvantageous. They save test time, permit the use of smallersamples, and have other factors which may merit their use. Ifautomated testers are used, the user shall ensure that all of themanufacturers instructions for calibration, adjustment, andoperation of the instrument are followed.
22、It shall be reportedthat the pour point was determined by an automatic instrument.In some cases, precision of automatic pour point testers maynot have been determined. In any case of dispute, the pourpoint as determined by the manual method described hereinshall be considered the referee test.7. Rea
23、gents7.1 Reference Oils, HMA through HMFThese are avail-able from the Test Monitoring Center.88. Sampling8.1 Take samples to be tested in accordance with theinstructions in Practice D 4057.9. Test Preparation9.1 Place the seven clean test jars in a holder.9.2 Measure and mark each test jar as follow
24、s:9.2.1 Measuring inside the test jar, mark each jar at 23 and54 mm from the bottom.9.2.2 Mark the first test jar for use with the undiluted test oilspecimen.9.2.3 Mark six test jars with the letters A through F todesignate which reference oil will be mixed with the test oil.9.3 Vigorously shake the
25、 test oil.9.4 Using test oil, fill the six jars (that were marked for usewith reference oil) to the 23-mm mark.9.5 Fill the test jar that was marked for the undiluted test oil,to the 54-mm mark.9.6 Vigorously shake the six reference oils.9.7 Fill the test jars marked A through F with the corre-spond
26、ing reference oil to the 54-mm mark.9.8 Firmly place the unbored stoppers in each of the test jarsand shake the test jars vigorously.9.9 Remove the stoppers from each test jar.10. Procedure10.1 Heat the test specimens in the test jars to 46 6 2C ina constant temperature oven or liquid bath.10.2 Remo
27、ve the test jars from the oven and allow to cool toroom temperature.10.3 For each test specimen record evidence of separation,its location, color, and particle size, and the color of the testspecimen on the record form under Before Treatment (see Fig.A1.1).10.4 Determination of Pour Point:NOTE 1This
28、 pour point procedure is based on the method described inTest Method D 97 but with the exception indicated in Note 2.10.4.1 Place a ring gasket around each test jar just below theoil level.10.4.2 Place a calibrated thermometer with bored stopper ineach of the test jars. Ensure that the thermometer b
29、ulb isimmersed such that the beginning of the capillary is 3 mmbelow the surface of the oil.10.4.3 Place a calibrated thermometer in the cooling baththat is maintained at a temperature of 18 to 15C.10.4.4 Place the test jars into the jacket in the cooling bath.10.4.5 Pour points are expressed in int
30、egers that are positiveor negative multiples of 3C. Begin to examine the appearanceof each test specimen when its temperature is 12C above theexpected pour point (estimated as a multiple of 3C). Removethe test jar from the jacket carefully and tilt it just enough toascertain whether there is movemen
31、t of the test specimen in thejar.10.4.6 If there is movement of the test specimen in the testjar, return it immediately to the jacket. (The complete operationof removal and replacement shall require no more than 3 s.)10.4.7 If the test specimen in the test jar does not flow whenthe jar is tilted:10.
32、4.7.1 Hold the test jar in a horizontal position for5sasnoted by a timing device.10.4.7.2 If the test specimen shows any movement underthese conditions, return the jar to the jacket.8ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 152006-4489.This test method is supplemented by Informati
33、on Letters and Memoranda issued bythe ASTM Test Monitoring Center; users of this test method can contact the ASTMTest Monitoring Center to obtain the most recent of these.D692203210.4.7.3 If the test specimen shows no movement, recordthe test temperature for this test jar on the record form, in C,un
34、der Cooled to Pour Point (see Fig. A1.1). Place the test jarin a holder to thaw.NOTE 2Test Method D 97 requires that 3C be added to the tempera-ture and reported. This is not the case here. The actual observedtemperature is reported.10.4.8 If the test specimen has not ceased to flow when itreaches 6
35、C, place the test jar and jacket in a second bathmaintained at a temperature of 35 to 32C.10.4.9 Continue to perform steps 10.4.5 through 10.4.7 at3C intervals for each of the test jars.10.4.10 If the test specimen has not ceased to flow when thetemperature of 24C has been reached, place the test ja
36、rs in athird bath maintained at a temperature of 52 to 49C.10.4.11 Continue to perform steps 10.4.5 through 10.4.7 at3C intervals for each of the test jars.10.4.11.1 For determinations of very low or very high pourpoints, additional cold baths should be maintained with tem-perature differentials of
37、about 17C. In each case transfer thetest jar when the temperature of the test specimen reaches apoint of 28C above the temperature of the new bath.10.4.12 Allow the test specimens to thaw.10.4.13 When each of the test specimens become transpar-ent and the cloudiness has disappeared observe for the e
38、vi-dence of separation, its location, color, and particle size, andthe color of the test specimen. Record the information re-quested on the record form under Warmed Just Above CloudPoint (see Fig. A1.1).10.5 Heating of the Test Specimens:10.5.1 Wait until the test specimens have reached roomtemperat
39、ure.10.5.2 Remove the thermometers and stoppers from the testjars.10.5.3 Remove the ring gaskets from the test jars.10.5.4 Place all test jars in an appropriate oven or liquidbath where the temperature has been set to a point that willallow the test specimen temperatures to reach 232 6 2Cwithin 90 m
40、in.NOTE 3Heating rates of 25 to 90 min have been found to beacceptable.10.5.5 When the test specimen temperatures reach 232 62C, immediately discontinue the heating process and allowthe test jars to cool to room temperature.10.6 Storage of the Test Specimens at Pour Point:10.6.1 Store the undiluted
41、test oil specimen and the sixblends at the pour point of the undiluted test oil specimen for18 to 24 h in the appropriate cold box.10.6.2 At the end of the storage period, remove the testspecimens from the cold box and allow them to warm.10.6.3 When the test specimens become transparent andcloudines
42、s has disappeared, observe and record the informationrequested on the record form under Heat to 232C Stored atSample Pour Point Temperature Store 18hWarmAbovePour Point (see Fig. A1.1).10.6.4 Allow the test specimens to warm to room tempera-ture.10.6.5 Observe the test specimens and record the infor
43、ma-tion requested on the record form under Warm to RoomTemperature (see Fig. A1.1).10.6.6 Discard the test specimens as required.11. Report11.1 Report the data on the homogeneity and miscibility testform located in Fig. A1.1.12. Precision and Bias12.1 No information is presented about either the pre
44、cisionor bias of Test Method D 6922 for measuring homogeneity andmiscibility since the test results are nonquantitative.13. Keywords13.1 automotive engine oil; homogeneity; miscibilityD6922033ANNEX(Mandatory Information)A1. REPORT FORMASTM International takes no position respecting the validity of a
45、ny 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 the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to re
46、vision 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 of this standard or for additional standardsand should be addressed to ASTM International Headquarters. You
47、r 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 shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copy
48、righted 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.or
49、g (e-mail); or through the ASTM website(www.astm.org).Sample No.: Date:Reference Oil Added To Test Oil None HMA HMB HMC HMD HME HMFThermometer Serial NumberBefore TreatmentEvidence of SeparationLocationColorParticle SizeVisual Appearance of the Test SpecimenCooled to Pour Point, CWarmed Just Above Cloud PointEvidence of SeparationLocationColorParticle SizeVisual Appearance of the Test SpecimenHeat to 232C Stored at Sample Pour Point Temperature Store 18 Hours Warm Above Pour PointEvidence of SeparationLocationColorPartic
