1、Designation: D 97 06Designation: 15/95An American National StandardStandard Test Method forPour Point of Petroleum Products1This standard is issued under the fixed designation D 97; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, t
2、he year of last revision.Anumber in parentheses indicates the year of last reapproval.Asuperscriptepsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers and
3、is intended for use on anypetroleum product.2A procedure suitable for black specimens,cylinder stock, and nondistillate fuel oil is described in 8.8.Aprocedure for testing the fluidity of a residual fuel oil at aspecified temperature is described in Appendix X1. The cloudpoint procedure formerly par
4、t of this test method now appearsas Test Method D 2500.1.2 Currently there is no ASTM test method for automatedTest Method D 97 pour point measurements.1.3 Several ASTM test methods offering alternative proce-dures for determining pour points using automatic apparatusare available. None of them shar
5、e the same designation numberas Test Method D 97. When an automatic instrument is used,the ASTM test method designation number specific to thetechnique shall be reported with the results. A procedure fortesting the pour point of crude oils is described in Test MethodD 5853.1.4 This standard does not
6、 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 Standards
7、:3D117 Guide for Sampling, Test Methods, and Specifica-tions for Electrical Insulating Oils of Petroleum OriginD 396 Specification for Fuel OilsD 1659 Test Method for Maximum Fluidity Temperature ofResidual Fuel Oil4D 2500 Test Method for Cloud Point of Petroleum ProductsD 3245 Test Method for Pumpa
8、bility of Industrial Fuel OilsD 5853 Test Method for Pour Point of Crude OilsD 6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Energy Institute Standards:Specifications for
9、 IP Standard Thermometers53. Terminology3.1 Definitions:3.1.1 black oil, nlubricant containing asphaltic materials.Black oils are used in heavy-duty equipment applications, suchas mining and quarrying, where extra adhesiveness is desired.3.1.2 cylinder stock, nlubricant for independently lubri-cated
10、 engine cylinders, such as those of steam engines and aircompressors. Cylinder stock are also used for lubrication ofvalves and other elements in the cylinder area.3.1.3 pour point, nin petroleum products, the lowesttemperature at which movement of the test specimen isobserved under prescribed condi
11、tions of test.3.1.4 residual fuel, na liquid fuel containing bottomsremaining from crude distillation or thermal cracking; some-times referred to as heavy fuel oil.3.1.4.1 DiscussionResidual fuels comprise Grades 4, 5,and 6 fuel oils, as defined in Specification D 396.4. Summary of Test Method4.1 Af
12、ter preliminary heating, the sample is cooled at aspecified rate and examined at intervals of 3C for flowcharacteristics. The lowest temperature at which movement ofthe specimen is observed is recorded as the pour point.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Pr
13、oducts and Lubricants and is the direct responsibility of SubcommitteeD02.07.0D on Wax-Related Viscometric Properties of Fuels and Oils.Current edition approved Nov. 1, 2006. Published November 2006. Originallyapproved in 1927, replacing D 47. Last previous edition approved in 2005 asD 9705a.In the
14、IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was adopted as a joint ASTM-IP Standard in 1965.2Statements defining this test and its significance when applied to electricalinsulating oils of mineral origin will be found in Guide D117.3For referenced
15、 ASTM standards, visit the 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.4Withdrawn.5Methods forAnalysis and Testing, IP Standards for Petroleum and
16、its Products,Part I, Vol 2.1*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.5. Significance and Use5.1 The pour point of a petroleum specimen is an index ofthe lowest t
17、emperature of its utility for certain applications.6. Apparatus6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 to34.8-mm outside diameter, and 115 to 125 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 greate
18、r than1.6 mm. The jar shall have a line to indicate a sample height 546 3 mm above the inside bottom. See Fig. 1.6.2 Thermometers, having the following ranges and con-forming to the requirements prescribed in Specification E1forthermometers:Temperature ThermometerNumberThermometer Range ASTM IPHigh
19、cloud and pour 38 to +50C 5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 to +127C 61C 63C6.2.1 Since separation of liquid column thermometers occa-sionally occurs and may escape detection, thermometersshould be checked immediately prior to the test and used onlyif they prove accurate with
20、in 61C (for example ice point).6.3 Cork, to fit the test jar, bored centrally for the testthermometer.6.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 1156 3-mm depth, with inside diameter of 44.2 to 45.8 mm. Itshall be supported in a vertical position in the cooling bath (see6.7) so that
21、not more than 25 mm projects out of the coolingmedium, and shall be capable of being cleaned.6.5 Disk, cork or felt, 6 mm thick to fit loosely inside thejacket.6.6 Gasket, to fit snugly around the outside of the test jarand loosely inside the jacket. The gasket may be made ofrubber, leather, or othe
22、r material that is elastic enough to clingto the test jar and hard enough to hold its shape. Its purpose isto prevent the test jar from touching the jacket.6.7 Bath or Baths, maintained at prescribed temperatureswith a firm support to hold the jacket vertical. The requiredbath temperatures may be ob
23、tained by refrigeration if avail-able, otherwise by suitable freezing mixtures. Freezing mix-tures commonly used for temperatures down to those shownare as follows:For Tempera-tures DownIce and water 9CCrushed ice and sodium chloride crystals 12CCrushed ice and calcium chloride crystals 27CAcetone o
24、r petroleum naphtha (see Section 7) chilledin a covered metal beaker with an ice-salt mixture to 12Cthen with enough solid carbon dioxide to give the desired tem-perature.57C7. Reagents and Materials7.1 The following solvents of technical grade are appropri-ate for low-temperature bath media.7.1.1 A
25、cetone,(WarningExtremely flammable).7.1.2 Alcohol, Ethanol (WarningFlammable).NOTEDimensions are in millimetres (not to scale).FIG. 1 Apparatus for Pour Point TestD970627.1.3 Alcohol, Methanol (WarningFlammable. Vaporharmful).7.1.4 Petroleum Naphtha,(WarningCombustible. Vaporharmful).7.1.5 Solid Car
26、bon Dioxide,(WarningExtremely cold78.5C).8. Procedure8.1 Pour the specimen into the test jar to the level mark.When necessary, heat the specimen in a bath until it is justsufficiently fluid to pour into the test jar.NOTE 1It is known that some materials, when heated to a temperaturehigher than 45C d
27、uring the preceding 24 h, do not yield the same pourpoint results as when they are kept at room temperature for 24 h prior totesting. Examples of materials which are known to show sensitivity tothermal history are residual fuels, black oils, and cylinder stocks.8.1.1 Samples of residual fuels, black
28、 oils, and cylinderstocks which have been heated to a temperature higher than45C during the preceding 24 h, or when the thermal history ofthese sample types is not known, shall be kept at roomtemperature for 24 h before testing. Samples which are knownby the operator not to be sensitive to thermal h
29、istory need notbe kept at room temperature for 24 h before testing.8.1.2 Experimental evidence supporting elimination of the24-h waiting period for some sample types is contained in aresearch report.68.2 Close the test jar with the cork carrying the high-pourthermometer (5.2). In the case of pour po
30、ints above 36C, usea higher range thermometer such as IP 63C or ASTM 61C.Adjust the position of the cork and thermometer so the cork fitstightly, the thermometer and the jar are coaxial, and thethermometer bulb is immersed so the beginning of the capillaryis 3 mm below the surface of the specimen.8.
31、3 For the measurement of pour point, subject the speci-men in the test jar to the following preliminary treatment:8.3.1 Specimens Having Pour Points Above 33CHeatthe specimen without stirring to 9C above the expected pourpoint, but to at least 45C, in a bath maintained at 12C abovethe expected pour
32、point, but at least 48C. Transfer the test jarto a bath maintained at 24 6 1.5C and commence observa-tions for pour point. When using a liquid bath, ensure that theliquid level is between the fill mark on the test jar and the topof the test jar.8.3.2 Specimens Having Pour Points of 33C andBelowHeat
33、the specimen without stirring to 45C in a bathmaintained at 48 6 1.5C and cool to 15C in a bathmaintained at 6 6 1.5C. Remove the high cloud and pourthermometer, and place the low cloud and pour thermometer inposition. When using a liquid bath, ensure that the liquid levelis between the fill mark on
34、 the test jar and the top of the test jar.8.4 See that the disk, gasket, and the inside of the jacket areclean and dry. Place the disk in the bottom of the jacket. Placethe gasket around the test jar, 25 mm from the bottom. Insertthe test jar in the jacket. Never place a jar directly into thecooling
35、 medium.8.5 After the specimen has cooled to allow the formation ofparaffin wax crystals, take great care not to disturb the mass ofspecimen nor permit the thermometer to shift in the specimen;any disturbance of the spongy network of wax crystals willlead to low and erroneous results.8.6 Pour points
36、 are expressed in integers that are positive ornegative multiples of 3C. Begin to examine the appearance ofthe specimen when the temperature of the specimen is 9Cabove the expected pour point (estimated as a multiple of 3C).At each test thermometer reading that is a multiple of 3Cbelow the starting
37、temperature remove the test jar from thejacket. To remove condensed moisture that limits visibilitywipe the surface with a clean cloth moistened in alcohol(ethanol or methanol). Tilt the jar just enough to ascertainwhether there is a movement of the specimen in the test jar. Ifmovement of specimen i
38、n the test jar is noted, then replace thetest jar immediately in the jacket and repeat a test for flow atthe next temperature, 3C lower. Typically, the completeoperation of removal, wiping, and replacement shall requirenot more than 3 s.8.6.1 If the specimen has not ceased to flow when itstemperatur
39、e has reached 27C, transfer the test jar to a jacket ina cooling bath maintained at 0 6 1.5C. As the specimencontinues to get colder, transfer the test jar to a jacket in thenext lower temperature cooling bath in accordance with Table1.8.6.2 If the specimen in the jar does not show movementwhen tilt
40、ed, hold the jar in a horizontal position for 5 s, asnoted by an accurate timing device, and observe the specimencarefully. If the specimen shows any signs of movement before5 s has passed, replace the test jar immediately in the jacket andrepeat a test for flow at the next temperature, 3C lower.8.7
41、 Continue in this manner until a point is reached at whichthe specimen shows no movement when the test jar is held ina horizontal position for 5 s. Record the observed reading ofthe test thermometer.8.8 For black specimen, cylinder stock, and nondistillatefuel specimen, the result obtained by the pr
42、ocedure describedin 8.1 through 8.7 is the upper (maximum) pour point. Ifrequired, determine the lower (minimum) pour point by heat-ing the sample while stirring, to 105C, pouring it into the jar,and determining the pour point as described in 8.4 through 8.7.8.9 Some specifications allow for a pass/
43、fail test or havepour point limits at temperatures not divisible by 3C. In thesecases, it is acceptable practice to conduct the pour pointmeasurement according to the following schedule: Begin toexamine the appearance of the specimen when the temperatureof the specimen is 9C above the specification
44、pour point.Continue observations at 3C intervals as described in 8.6 and6Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021377.TABLE 1 Bath and Sample Temperature RangesBath Bath TemperatureSetting, CSample TemperatureRange, C
45、106 1.5 Start to 92-186 1.5 9 to -63-36 1.5 -6to-244-56 1.5 -24 to -425-96 1.5 -42 to -60D970638.7 until the specification temperature is reached. Report thesample as passing or failing the specification limit.9. Calculation and Report9.1 Add 3C to the temperature recorded in 8.7 and reportthe resul
46、t as the Pour Point, ASTM D 97. For black oil, and soforth, add 3C to the temperature recorded in 8.7 and report theresult as Upper Pour Point, ASTM D 97, or Lower Pour Point,ASTM D 97, as required.10. Precision and Bias10.1 PrecisionThe precision of this test method as deter-mined by the statistica
47、l examination of the interlaboratory testresults is as follows:10.1.1 Lubricating Oil7:10.1.1.1 RepeatabilityThe difference between successivetest results, obtained by the same operator using the sameapparatus under constant operating conditions on identical testmaterial would, in the long run, in t
48、he normal and correctoperation of this test method, exceed 6C only in one case intwenty. Differences greater than this should be consideredsuspect.10.1.1.2 ReproducibilityThe difference between twosingle and independent test results, obtained by differentoperators working in different laboratories o
49、n identical testmaterial would, in the long run, in the normal and correctoperation of this test method, exceed 9C only in one case intwenty. Differences greater than this should be consideredsuspect.10.1.1.3 The precision statements7were derived from a1998 interlaboratory test program using Practice D 6300.Participants analyzed five sets of duplicate base oils, three setsof duplicate multigrade lubricating oils, and one set each ofduplicate hydraulic oils and automatic transmission fluid in thetemperature range of
