1、Designation: D97 17Designation: 15/95Standard Test Method forPour Point of Petroleum Products1This standard is issued under the fixed designation D97; the number immediately following the designation indicates the year of originaladoption or, in the case of revision, the year of last revision.Anumbe
2、r in parentheses indicates the year of last reapproval.Asuperscriptepsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method covers and is intended for use on anyp
3、etroleum product.2A procedure suitable for black specimens,cylinder stock, and nondistillate fuel oil is described in 8.8.Thecloud point procedure formerly part of this test method nowappears as Test Method D2500.1.2 Currently there is no ASTM test method for automatedTest Method D97 pour point meas
4、urements.1.3 Several ASTM test methods offering alternative proce-dures for determining pour points using automatic apparatusare available. None of them share the same designation numberas Test Method D97. When an automatic instrument is used,the ASTM test method designation number specific to thete
5、chnique shall be reported with the results. A procedure fortesting the pour point of crude oils is described in Test MethodD5853.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 WARNINGMercury has been designated by manyr
6、egulatory agencies as a hazardous material that can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Saf
7、ety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.6 This standard does not purport to address all of thesafet
8、y 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:3D117 Guide for Sampling, Test Met
9、hods, and Specificationsfor Electrical Insulating Oils of Petroleum OriginD396 Specification for Fuel OilsD2500 Test Method for Cloud Point of Petroleum Productsand Liquid FuelsD5853 Test Method for Pour Point of Crude OilsD6300 Practice for Determination of Precision and BiasData for Use in Test Me
10、thods for Petroleum Products andLubricantsD7962 Practice for Determination of Minimum ImmersionDepth and Assessment of Temperature Sensor Measure-ment DriftE1 Specification for ASTM Liquid-in-Glass ThermometersE644 Test Methods for Testing Industrial Resistance Ther-mometersE1137 Specification for I
11、ndustrial Platinum Resistance Ther-mometersE2877 Guide for Digital Contact Thermometers2.2 Energy Institute Standards:4Specifications for IP Standard Thermometers3. Terminology3.1 Definitions:3.1.1 black oil, nlubricant containing asphaltic materials.Black oils are used in heavy-duty equipment appli
12、cations, suchas mining and quarrying, where extra adhesiveness is desired.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved Jan. 1, 20
13、17. Published January 2017. Originallyapproved in 1927, replacing D47. Last previous edition approved in 2016 asD97 16. DOI: 10.1520/D0097-17.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method was adopted as a joint ASTM-IP Standard in 1965.2State
14、ments defining this test and its significance when applied to electricalinsulating oils of mineral origin will be found in Guide D117.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume info
15、rmation, refer to the standards Document Summary page onthe ASTM website.4Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,U.K., http:/www.energyinst.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box
16、 C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by th
17、e World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.2 cylinder stock, nlubricant for independently lubri-cated 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.
18、1.3 digital contact thermometer (DCT), nan electronicdevice consisting of a digital display and associated tempera-ture sensing probe.3.1.3.1 DiscussionThis device consists of a temperaturesensor connected to a measuring instrument; this instrumentmeasures the temperature-dependent quantity of the s
19、ensor,computes the temperature from the measured quantity, andprovides a digital output. This digital output goes to a digitaldisplay and/or recording device that may be internal or externalto the device. These devices are sometimes referred to as a“digital thermometer”.3.1.3.2 DiscussionPortable el
20、ectronic thermometers(PET) is an acronym sometimes used to refer to a subset of thedevices covered by this definition.3.1.4 pour point, nin petroleum products, the lowesttemperature at which movement of the test specimen isobserved under prescribed conditions of test.3.1.5 residual fuel, na liquid f
21、uel containing bottomsremaining from crude distillation or thermal cracking; some-times referred to as heavy fuel oil.3.1.5.1 DiscussionResidual fuels comprise Grades 4, 5,and 6 fuel oils, as defined in Specification D396.4. Summary of Test Method4.1 After preliminary heating, the sample is cooled a
22、t aspecified rate and examined at intervals of 3 C for flowcharacteristics. The lowest temperature at which movement ofthe specimen is observed is recorded as the pour point.5. Significance and Use5.1 The pour point of a petroleum specimen is an index ofthe lowest temperature of its utility for cert
23、ain applications.6. Apparatus6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 mmto 34.8 mm outside diameter, and 115 mm to 125 mm inheight. The inside diameter of the jar can range from 30.0 mmto 32.4 mm, within the constraint that the wall thickness be nogreater than 1.6 mm. The jar sha
24、ll have a line to indicate asample height 54 mm 6 3 mm above the inside bottom. SeeFig. 1.6.2 Temperature Measuring DeviceEither liquid-in-glassthermometer as described in 6.2.1 or Digital Contact Ther-mometer (DCT) meeting the requirements described in 6.2.2.55Supporting data have been filed at AST
25、M International Headquarters and maybe obtained by requesting Research Report RR:D02-1826. ContactASTM CustomerService at serviceastm.org.NOTE 1Dimensions are in millimetres (not to scale).FIG. 1 Apparatus for Pour Point TestD971726.2.1 Liquid-in-Glass Thermometers, having the followingranges and co
26、nforming to the requirements prescribed inSpecification E1 or Specifications for IP Standard Thermom-eters:Temperature ThermometerNumberThermometer Range ASTM IPHigh cloud and pour 38 C to +50 C 5C 1CLow cloud and pour 80 C to +20 C 6C 2CMelting point +32 C to +127 C 61C 63C6.2.1.1 Since separation
27、of liquid column thermometersoccasionally occurs and may escape detection, thermometersshould be checked immediately prior to the test and used onlyif they prove accurate within 61 C (for example ice point).6.2.2 Digital Contact Thermometer Requirements:Parameter RequirementDCT Guide E2877 Class G o
28、r betterTemperature range 65 C to 90 CDisplay resolution 1 C minimum, preferably 0.1 CSensor type PRT, thermistor, thermocoupleSensor 3 mm OD sheath with a sensing element lessthan 10 mm in lengthMinimum immersion Less than 40 mm per Test Method D7962Sample immersion depth Between 10 mm and 15 mm in
29、 the sample.Fig. 1Display accuracy 500 mK (0.5 C) for combined probe andsensorResponse time less than or equal to 25 s as defined inSpecification E1137Drift less than 500 mK (0.5 C) per yearCalibration error less than 500 mK (0.5 C) over the range ofintended use.Calibration range 40 C or lower to 85
30、 CCalibration data 4 data points evenly distributed over calibrationrange with data included in calibration report.Calibration report From a calibration laboratory with demonstratedcompetency in temperature calibration which istraceable to a national calibration laboratory ormetrology standards body
31、NOTE 1When the DCT display is mounted on the end to the probessheath, the test jar with the probe inserted will be unstable. To resolve this,it is recommended that the probe be less than 30 cm in length but no lessthan 15 cm.A5 cm long stopper, that has a low thermal conductivity, withapproximately
32、half of it inserted in the sample tube will improve stability.6.2.2.1 The DCT calibration drift shall be checked at leastannually by either measuring the ice point or against areference thermometer in a constant temperature bath at theprescribed immersion depth to ensure compliance with 6.2.2.See Te
33、st Method D7962.NOTE 2When a DCTs calibration drifts in one direction over severalcalibration checks, that is, ice point, it may be an indication of deteriora-tion of the DCT.6.3 Cork, to fit the test jar, bored centrally for the testtemperature measuring device.6.4 Jacket, watertight, cylindrical,
34、metal, flat-bottomed,115 mm 6 3 mm depth, with inside diameter of 44.2 mm to45.8 mm. It shall be supported in a vertical position in thecooling bath (see 6.7) so that not more than 25 mm projects outof the cooling medium, and shall be capable of being cleaned.6.5 Disk, cork or felt, 6 mm thick to fi
35、t loosely inside thejacket.6.6 Gasket Ring Form, about 5 mm in thickness, to fitsnugly around the outside of the test jar and loosely inside thejacket. The gasket may be made of rubber, leather, or othermaterial that is elastic enough to cling to the test jar and hardenough to hold its shape. Its pu
36、rpose is to prevent the test jarfrom 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 obtained by refrigeration ifavailable, otherwise by suitable cooling mixtures. Coolingmixtures common
37、ly used for bath temperatures down to thoseshown are in Table 1.7. Reagents and Materials7.1 The following solvents of technical grade are appropri-ate for low-temperature bath media.7.1.1 Acetone, (WarningExtremely flammable).7.1.2 Alcohol, Ethanol (WarningFlammable).7.1.3 Alcohol, Methanol (Warnin
38、gFlammable. Vaporharmful).7.1.4 Petroleum Naphtha, (WarningCombustible. Vaporharmful).7.1.5 Solid Carbon Dioxide, (WarningExtremely cold78.5 C).D971738. 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 t
39、o pour into the test jar.NOTE 3It is known that some materials, when heated to a temperaturehigher than 45 C during 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 sensitivit
40、y tothermal history are residual fuels, black oils, and cylinder stocks.8.1.1 Samples of residual fuels, black oils, and cylinderstocks which have been heated to a temperature higher than45 C during the preceding 24 h, or when the thermal history ofthese sample types is not known, shall be kept at r
41、oomtemperature for 24 h before testing. Samples which are knownby the operator not to be sensitive to thermal history 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 aresear
42、ch report.68.2 In the case of pour points above 36 C, use a higherrange temperature measuring device (6.2) such as IP 63C orASTM 61C, or a digital contact thermometer. Close the test jarwith the cork carrying the test temperature measuring device(6.2). Adjust the position of the cork and temperature
43、 measur-ing device so the cork fits tightly, the temperature measuringdevice and the jar are coaxial, and the temperature measuringdevice is immersed to the correct depth.8.2.1 For liquid-in-glass, the thermometer bulb should beimmersed so the beginning of the capillary is 3 mm below thesurface of t
44、he specimen.8.2.2 For digital contact thermometers, the probe should beimmersed so the end of the probe is 10 mm to 15 mm below thesurface of the specimen.8.3 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 P
45、oints Above 33 CHeatthe specimen without stirring to 9 C above the expected pourpoint, but to at least 45 C, in a bath maintained at 12 C abovethe expected pour point, but at least 48 C. Transfer the test jarto a bath maintained at 24 C 6 1.5 C and commenceobservations for pour point. When using a l
46、iquid bath, ensurethat the liquid level is between the fill mark on the test jar andthe top of the test jar.8.3.2 Specimens Having Pour Points of 33 C andBelowHeat the specimen without stirring to at least 45 C ina bath maintained at 48 C 6 1.5 C. Transfer the test jar to abath maintained at 24 C 6
47、1.5 C. When using a liquid bath,ensure that the liquid level is between the fill mark on the testjar and the top of the test jar. When the specimen temperaturereaches 27 C, and if using liquid-in-glass thermometers,remove the high cloud and pour thermometer, and place thelow cloud and pour thermomet
48、er in position. Transfer the testjar to the cooling bath (see 8.6.1).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 j
49、ar directly into thecooling 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 are expressed in integers that are positive ornegative multiples of 3 C. Begin to examine the appearance ofthe specimen when the temperature of the specimen is 9 Cabove the expected pour
