1、Designation: D97 15D97 16Designation: 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.
2、Anumber 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 o
3、n any petroleum product.2 A procedure suitable for black specimens,cylinder stock, and nondistillate fuel oil is described in 8.8. The cloud point procedure formerly part of this test method nowappears as Test Method D2500.1.2 Currently there is no ASTM test method for automated Test Method D97 pour
4、 point measurements.1.3 Several ASTM test methods offering alternative procedures for determining pour points using automatic apparatus areavailable. None of them share the same designation number asTest Method D97.When an automatic instrument is used, theASTMtest method designation number specific
5、to the technique shall be reported with the results. A procedure for testing the pour pointof crude oils is described in Test Method D5853.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 WARNINGMercury has been designa
6、ted 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. Cautionshould be taken when handling mercury and mercury containing products. See the applicable produc
7、t 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 your state or country may be prohibited by law.1.6 This standard does not purport to address a
8、ll 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 regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D117 Guide for Sampli
9、ng, Test Methods, and Specifications for Electrical Insulating Oils of Petroleum OriginD396 Specification for Fuel OilsD2500 Test Method for Cloud Point of Petroleum ProductsD5853 Test Method for Pour Point of Crude OilsD6300 Practice for Determination of Precision and Bias Data for Use in Test Meth
10、ods for Petroleum Products and LubricantsD7962 Practice for Determination of Minimum Immersion Depth and Assessment of Temperature Sensor Measurement DriftE1 Specification for ASTM Liquid-in-Glass ThermometersE644 Test Methods for Testing Industrial Resistance ThermometersE1137 Specification for Ind
11、ustrial Platinum Resistance ThermometersE2877 Guide for Digital Contact Thermometers1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved
12、 Oct. 1, 2015Jan. 1, 2016. Published November 2015February 2016. Originally approved in 1927, replacing D47. Last previous edition approvedin 20122015 as D97 12.D97 15. DOI: 10.1520/D0097-15.10.1520/D0097-16.In the IP, this test method is under the jurisdiction of the Standardization Committee. This
13、 test method was adopted as a joint ASTM-IP Standard in 1965.2 Statements defining this test and its significance when applied to electrical insulating oils of mineral origin will be found in Guide D117.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Serv
14、ice at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM 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 previou
15、s version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult 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 Change
16、s section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.2 Energy Institute Standards:4Specifications for IP Standard Thermometers3. Terminology3.1 Definitions:3.1.1 black oil, nlubricant containi
17、ng asphaltic materials. Black oils are used in heavy-duty equipment applications, such asmining and quarrying, where extra adhesiveness is desired.3.1.2 cylinder stock, nlubricant for independently lubricated engine cylinders, such as those of steam engines and aircompressors. Cylinder stock are als
18、o used for lubrication of valves and other elements in the cylinder area.3.1.3 digital contact thermometer (DCT), nan electronic device consisting of a digital display and associated temperaturesensing probe.3.1.3.1 DiscussionThis device consists of a temperature sensor connected to a measuring inst
19、rument; this instrument measures the temperature-dependent quantity of the sensor, computes the temperature from the measured quantity, and provides a digital output. This digitaloutput goes to a digital display and/or recording device that may be internal or external to the device. These devices ar
20、e sometimesreferred to as a “digital thermometer”.3.1.3.2 DiscussionPortable electronic thermometers (PET) is an acronym sometimes used to refer to a subset of the devices covered by this definition.3.1.4 pour point, nin petroleum products, the lowest temperature at which movement of the test specim
21、en is observed underprescribed conditions of test.3.1.5 residual fuel, na liquid fuel containing bottoms remaining from crude distillation or thermal cracking; sometimesreferred to as heavy fuel oil.3.1.5.1 DiscussionResidual fuels comprise Grades 4, 5, and 6 fuel oils, as defined in Specification D
22、396.4. Summary of Test Method4.1 After preliminary heating, the sample is cooled at a specified rate and examined at intervals of 3 C for flow characteristics.The lowest temperature at which movement of the specimen is observed is recorded as the pour point.5. Significance and Use5.1 The pour point
23、of a petroleum specimen is an index of the lowest temperature of its utility for certain applications.6. Apparatus6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 mm to 34.8 mm outside diameter, and 115 mm to 125 mm in height.The inside diameter of the jar can range from 30.0 mm to 32.4
24、mm, within the constraint that the wall thickness be no greater than1.6 mm. The jar shall have a line to indicate a sample height 54 mm 6 3 mm above the inside bottom. See Fig. 1.6.2 Temperature Measuring DeviceEither liquid-in-glass thermometer as described in 6.2.1 or Digital Contact Thermometer(D
25、CT) meeting the requirements described in 6.2.2.56.2.1 Liquid-in-Glass Thermometers, having the following ranges and conforming to the requirements prescribed inSpecification E1 or Specifications for IP Standard Thermometers:Temperature ThermometerNumberThermometer Range ASTM IPHigh cloud and pour 3
26、8 C to +50 C 5C 1CLow cloud and pour 80 C to +20 C 6C 2CMelting point +32 C to +127 C 61C 63C4 Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR, U.K., http:/www.energyinst.org.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting
27、 Research Report RR:D02-1377RR:D02-1826. Contact ASTMCustomer Service at serviceastm.org.D97 1626.2.1.1 Since separation of liquid column thermometers occasionally occurs and may escape detection, thermometers should bechecked immediately prior to the test and used only if they prove accurate within
28、 61 C (for example ice point).6.2.2 Digital Contact Thermometer Requirements:Parameter RequirementDCT Guide E2877 Class G or 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 less
29、than 10 mm in lengthMinimum immersion Less than 40 mm per Test Method D7962Sample immersion depth Between 10 mm and 15 mm in the sample.Fig. 1Display accuracy 500 mK (0.5 C) for combined probe and sensorResponse time less than or equal to 25 s as defined inSpecification E1137Drift less than 500 mK (
30、0.5 C) per yearCalibration error less than 500 mK (0.5 C) over the range of intended use.Calibration range 40 C or lower to 85 CCalibration data 4 data points evenly distributed over calibration range with data included in calibration report.Calibration report From a calibration laboratory with demo
31、nstrated competency in temperature calibration which istraceable to a national calibration laboratory or metrology standards bodyNOTE 1When the DCT display is mounted on the end to the probes sheath, the test jar with the probe inserted will be unstable. To resolve this, itis recommended that the pr
32、obe be less than 30 cm in length but no less than 15 cm. A 5 cm long stopper, that has a low thermal conductivity, withNOTE 1Dimensions are in millimetres (not to scale).FIG. 1 Apparatus for Pour Point TestD97 163approximately half of it inserted in the sample tube will improve stability.6.2.2.1 The
33、 DCT calibration drift shall be checked at least annually by either measuring the ice point or against a referencethermometer in a constant temperature bath at the prescribed immersion depth to ensure compliance with 6.2.2. See Test MethodD7962.NOTE 2When a DCTs calibration drifts in one direction o
34、ver several calibration checks, that is, ice point, it may be an indication of deteriorationof the DCT.6.3 Cork, to fit the test jar, bored centrally for the test thermometer.6.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 115 mm 6 3 mm depth, with inside diameter of 44.2 mm to 45.8 mm.It
35、 shall be supported in a vertical position in the cooling bath (see 6.7) so that 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 the jacket.6.6 Gasket Ring Form, about 5 mm in thickness, to fit snug
36、ly around the outside of the test jar and loosely inside the jacket.The gasket may be made of rubber, leather, or other material that is elastic enough to cling to the test jar and hard enough to holdits shape. Its purpose is to prevent the test jar from touching the jacket.6.7 Bath or Baths, mainta
37、ined at prescribed temperatures with a firm support to hold the jacket vertical. The required bathtemperatures may be obtained by refrigeration if available, otherwise by suitable cooling mixtures. Cooling mixtures commonlyused for bath temperatures down to those shown are in Table 1.7. Reagents and
38、 Materials7.1 The following solvents of technical grade are appropriate for low-temperature bath media.7.1.1 Acetone, (WarningExtremely flammable).7.1.2 Alcohol, Ethanol (WarningFlammable).7.1.3 Alcohol, Methanol (WarningFlammable. Vapor harmful).7.1.4 Petroleum Naphtha, (WarningCombustible. Vapor h
39、armful).7.1.5 Solid Carbon Dioxide, (WarningExtremely cold 78.5 C).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 just sufficientlyfluid to pour into the test jar.NOTE 3It is known that some materials, when heated to a t
40、emperature higher than 45 C during the preceding 24 h, do not yield the same pour pointresults as when they are kept at room temperature for 24 h prior to testing. Examples of materials which are known to show sensitivity to thermal historyare residual fuels, black oils, and cylinder stocks.8.1.1 Sa
41、mples of residual fuels, black oils, and cylinder stocks which have been heated to a temperature higher than 45 Cduring the preceding 24 h, or when the thermal history of these sample types is not known, shall be kept at room temperature for24 h before testing. Samples which are known by the operato
42、r not to be sensitive to thermal history need not be kept at roomtemperature for 24 h before testing.TABLE 1 Cooling Mixtures and Bath TemperaturesCooling Mixture BathTemperatureIce and water 0 C 1.5 CCrushed ice and sodium chloride crystals orAcetone or petroleum naphtha, or methanol or ethanol (se
43、eSection 7) with solid carbon dioxide added to give the desiredtemperature18 C 1.5 CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature33 C 1.5 CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid
44、 carbon dioxide added to give the desiredtemperature51 C 1.5 CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature69 C 1.5 CD97 1648.1.2 Experimental evidence supporting elimination of the 24 h waiting period for some sampl
45、e types is contained in a researchreport.68.2 In the case of pour points above 36 C, use a higher range thermometer such as IP 63C or ASTM 61C. Close the test jarwith the cork carrying the test thermometer (6.2). Adjust the position of the cork and thermometer so the cork fits tightly, thethermomete
46、r and the jar are coaxial, and the thermometer is immersed to the correct depth. For liquid-in-glass, the thermometerbulb should be immersed so the beginning of the capillary is 3 mm below the surface of the specimen. For digital contactthermometers, the probe should be immersed so the end of the pr
47、obe is 10 mm to 15 mm below the surface of the specimen.8.3 For the measurement of pour point, subject the specimen in the test jar to the following preliminary treatment:8.3.1 Specimens Having Pour Points Above 33 CHeat the specimen without stirring to 9 C above the expected pour point,but to at le
48、ast 45 C, in a bath maintained at 12 C above the expected pour point, but at least 48 C. Transfer the test jar to a bathmaintained at 24 C 6 1.5 C and commence observations for pour point. When using a liquid bath, ensure that the liquid levelis between the fill mark on the test jar and the top of t
49、he test jar.8.3.2 Specimens Having Pour Points of 33 C and BelowHeat the specimen without stirring to at least 45 C in a bathmaintained at 48 C 6 1.5 C. Transfer the test jar to a bath maintained at 24 C 6 1.5 C. When using a liquid bath, ensure thatthe liquid level is between the fill mark on the test jar and the top of the test jar. When the specimen temperature reaches 27 C,remove the high cloud and pour thermometer, and place the low cloud and pour thermometer in position. Tr
