1、Designation: D6922 11D6922 13Standard Test Method forDetermination of Homogeneity and Miscibility in AutomotiveEngine Oils1This standard is issued under the fixed designation D6922; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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.1. Scope Scope*1.1 This test method covers the determination if an automotive engine oil is homogeneous and will remain
3、 so, and if it ismiscible with certain standard reference oils after being submitted to a prescribed cycle of temperature changes. This test methodis very similar to the homogeneity and miscibility test described in FEDSTD791/3470.1.1.2 The values stated in SI units are to be regarded as standard. N
4、o other units of measurement are included in this standard.1.3 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionsh
5、ould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into
6、your state or country may be prohibited by law.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regul
7、atorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD5844 Test Method for Evaluation of Automotive Engine Oils for Inhibition of Rusting (Sequence IID) (With
8、drawn 2003)3D6557 Test Method for Evaluation of Rust Preventive Characteristics of Automotive Engine OilsE1 Specification for ASTM Liquid-in-Glass ThermometersE344 Terminology Relating to Thermometry and Hydrometry2.2 Federal Test Method Standard:4FEDSTD791/3470.1 Homogeneity and Miscibility of Oils
9、3. Terminology3.1 Definitions:3.1.1 calibrate, vto determine the indication or output of a measuring device with the respect of that of a standard. E3443.1.2 homogeneity, nthe ability of a test oil itself to remain the same in appearance throughout (uniform) after submission toa series of temperatur
10、e changes.3.1.3 miscibility, nthe ability of a reference oil and test oil to form a uniform mixture after blending and not separate into twophases after submission to a series of temperature changes.3.1.4 reference oil, nan oil of known performance characteristics, used as a basis for comparison.1 T
11、his test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.B0 onAutomotive Lubricants.Current edition approved July 1, 2011May 1, 2013. Published August 2011May 2013. Originally approved in 2003. Last prev
12、ious edition approved in 20032011 asD692203.D6922 11. DOI: 10.1520/D6922-11. DOI:10.1520/D6922-13.2 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 Docum
13、ent Summary page on the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.4 Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.This documen
14、t 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 prior editions as app
15、ropriate. 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 19428-2959. United St
16、ates13.1.4.1 DiscussionReference oils are used to calibrate testing facilities, to compare the performance of other oils, or to evaluate other materials (suchas seals) that interact with oils. D58443.1.5 specimen, na piece or portion of test oil used to make a test.3.1.6 test oil, nany oil subjected
17、 to evaluation in an established procedure. D65574. Summary of Test Method4.1 Visual color determinations and observations are made on an undiluted test oil specimen, along with six blends of the sametest oil that have been combined with specific reference oils. The pour point is then determined for
18、 the undiluted test oil specimenand the six blends. The undiluted test oil specimen and six blends are then allowed to warm to room temperature. Colordeterminations and observations are again made on the undiluted test oil specimen and six blends. The undiluted test oil specimenand six blends are he
19、ated to 232C,232 C, then allowed to cool to room temperature, and then stored at their pour pointtemperatures for 18 h to 24 h. The undiluted test oil specimen and six blends are then allowed to thaw and a series of colordeterminations and observations are made as they reach room temperature. All da
20、ta are recorded on a report form.5. Significance and Use5.1 It is important that engine oils from different manufacturers be homogeneous and miscible with each other, becauseoperators of automotive engines often do not have prior knowledge of the manufacturer of the oil that is currently used in the
21、irapplication, and engine failure can occur if oils are combined that do not stay homogeneous and function properly.6. Apparatus6.1 Test Jarcylindrical, of clear glass, flat bottom, 33.233.2 mm to 34.8-mm34.8 mm outside diameter, and 115115 mm to 125mm 125 mm in height. The inside diameter of the ja
22、r can range from 30.030.0 mm to 32.4 mm, 32.4 mm, within the constraintthat the wall thickness be no greater than 1.6 mm. 1.6 mm. The jar shall have a line to indicate a sample height 563 5 mm 6 3mm above the inside bottom.6.2 ThermometersASTM 6C, calibrated with a range of (80 to +20) C, conforming
23、 to Specification E1. In addition,temperature measuring devices such as liquid-in-glass thermometers, thermocouples, or platinum resistance thermometers canmaybe used, if they provide equivalent or better accuracy and precision, and cover the required temperature range.6.3 Stoppersclean stoppers, so
24、me unbored and others centrally bored for test thermometers.6.4 Jacketa glass or metal, water tight, cylindrical form with a flat bottom and approximately 120 mm in depth. The insidediameter of the jacket shall be 9.09.0 mm to 12.0 mm 12.0 mm greater than the outside diameter of the test jar.6.5 Dis
25、kcork or felt, about 6 mm in thickness and of the same diameter as the inside of the jacket.6.6 Gasketa ring gasket, about 5.0 mm in thickness, to fit snugly around the outside of the test jar and loosely inside the jacket.The purpose of the ring gasket is to prevent the test jar from touching the j
26、acket.6.7 Batha liquid cooling bath suitable to obtain the required temperatures.6.8 Ovena constant temperature oven suitable to obtain the required temperatures.6.9 Automated Pour Point Tester (Alternative)There are automated pour point testers available and in use whichthat may beadvantageous. The
27、y save test time, permit the use of smaller samples, and have other factors which may merit their use. Ifautomated testers are used, the user shall ensure that all of the manufacturersmanufacturers instructions for calibration,adjustment, and operation of the instrument are followed. It shall be rep
28、orted Report that the pour point was determined by anautomatic instrument. In some cases, precision of automatic pour point testers may not have been determined. In any case ofdispute, consider the pour point as determined by the manual method described herein shall be considered the referee test.7.
29、 Reagents7.1 Reference Oils, HMA through HMFThese are available from the Test Monitoring Center.58. Sampling8.1 Take samples to be tested in accordance with the instructions in Practice D4057.9. Test Preparation9.1 Place the seven clean test jars in a holder.9.2 Measure and mark each test jar as fol
30、lows:5 ASTM Test Monitoring Center, 6555 Penn Ave., Pittsburgh, PA 15206-4489. This test method is supplemented by Information Letters and Memoranda issued by theASTM Test Monitoring Center; users of this test method can contact the ASTM Test Monitoring Center to obtain the most recent of these.D692
31、2 1329.2.1 Measuring inside the test jar, mark each jar at 23 mm and 54 mm from the bottom.9.2.2 Mark the first test jar for use with the undiluted test oil specimen.9.2.3 Mark six test jars with the letters A through F to designate which reference oil will be mixed with the test oil.9.3 Vigorously
32、shake the test oil.9.4 Using test oil, fill the six jars (that were marked for use with reference oil) to the 23-mm23 mm mark.9.5 Fill the test jar that was marked for the undiluted test oil, to the 54-mm54 mm mark.9.6 Vigorously shake the six reference oils.9.7 Fill the test jars marked A through F
33、 with the corresponding reference oil to the 54-mm54 mm mark.9.8 Firmly place the unbored stoppers in each of the test jars and 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 2CC 6 2 C in a constant tempera
34、ture oven or liquid bath.10.2 Remove the test jars from the oven and allow to cool to room temperature.10.3 For each test specimen record evidence of separation, its location, color, and particle size, and the color of the test specimenon the record form under Before Treatment (see Fig. A1.1).10.4 D
35、etermination of Pour Point:NOTE 1This pour point procedure is based on the method described in Test Method D97 but with the exception indicated in Note 2.10.4.1 Place a ring gasket around each test jar just below the oil level.10.4.2 Place a calibrated thermometer with bored stopper in each of the t
36、est jars. Ensure that the thermometer bulb is immersedsuch that the beginning of the capillary is 3 mm below the surface of the oil.10.4.3 Place a calibrated thermometer in the cooling bath that is maintained at a temperature of 18 to 15C. 18 C to 15C.10.4.4 Place the test jars into the jacket in th
37、e cooling bath.10.4.5 Pour points are expressed in integers that are positive or negative multiples of 3C.3 C. Begin to examine the appearanceof each test specimen when its temperature is 12C12 C above the expected pour point (estimated as a multiple of 3C).3 C).Remove the test jar from the jacket c
38、arefully and tilt it just enough to ascertain whether there is movement of the test specimenin the jar.10.4.6 If there is movement of the test specimen in the test jar, return it immediately to the jacket. (The complete operation ofremoval and replacement shall require no more than 3 s.)3 s.)10.4.7
39、If the test specimen in the test jar does not flow when the jar is tilted:10.4.7.1 Hold the test jar in a horizontal position for 5 s 5 s as noted by a timing device.10.4.7.2 If the test specimen shows any movement under these conditions, return the jar to the jacket.10.4.7.3 If the test specimen sh
40、ows no movement, record the test temperature for this test jar on the record form, in C, degreesCelsius, under Cooled to Pour Point (see Fig. A1.1). Place the test jar in a holder to thaw.NOTE 2Test Method D97 requires that 3C3 C be added to the temperature and reported. This is not the case here. T
41、he actual observed temperatureis reported.10.4.8 If the test specimen has not ceased to flow when it reaches 6C,6 C, place the test jar and jacket in a second bathmaintained at a temperature of 3535 C to 32C.32 C.10.4.9 Continue to perform steps 10.4.5 through 10.4.7 at 3C3 C intervals for each of t
42、he test jars.10.4.10 If the test specimen has not ceased to flow when the temperature of 24C24 C has been reached, place the test jarsin a third bath maintained at a temperature of 5252 C to 49C.49 C.10.4.11 Continue to perform steps 10.4.5 through 10.4.7 at 3C3 C intervals for each of the test jars
43、.10.4.11.1 For determinations of very low or very high pour points, additional cold baths should be maintained with temperaturedifferentials of about 17C.17 C. In each case transfer the test jar when the temperature of the test specimen reaches a point of28C28 C above the temperature of the new bath
44、.10.4.12 Allow the test specimens to thaw.10.4.13 When each of the test specimens become transparent and the cloudiness has disappeared observe for the evidence ofseparation, its location, color, and particle size, and the color of the test specimen. Record the information requested on the recordfor
45、m under Warmed Just Above Cloud Point (see Fig. A1.1).10.5 Heating of the Test Specimens:10.5.1 Wait until the test specimens have reached room temperature.10.5.2 Remove the thermometers and stoppers from the test jars.10.5.3 Remove the ring gaskets from the test jars.D6922 13310.5.4 Place all test
46、jars in an appropriate oven or liquid bath where the temperature has been set to a point that will allow thetest specimen temperatures to reach 232 6 2C 232 C 6 2 C within 90 min.NOTE 3Heating rates of 25 min to 90 min have been found to be acceptable.10.5.5 When the test specimen temperatures reach
47、 232 6 2C, 232 C 6 2 C, immediately discontinue the heating process andallow the test jars to cool to room temperature.10.6 Storage of the Test Specimens at Pour Point:10.6.1 Store the undiluted test oil specimen and the six blends at the pour point of the undiluted test oil specimen for 1818 hto 24
48、 h 24 h in the appropriate cold box.10.6.2 At the end of the storage period, remove the test specimens from the cold box and allow them to warm.10.6.3 When the test specimens become transparent and cloudiness has disappeared, observe and record the informationrequested on the record form under Heat
49、to 232C232 C Stored at Sample Pour Point Temperature Store 18 h 18 h WarmAbove Pour Point (see Fig. A1.1).10.6.4 Allow the test specimens to warm to room temperature.10.6.5 Observe the test specimens and record the information requested on the record form under Warm to Room Temperature(see Fig. A1.1).10.6.6 Discard the test specimens as required.11. Report11.1 Report the data on the homogeneity and miscibility test form located in Fig. A1.1.12. Precision and Bias12.1 No informatio
