1、Designation: D97 12D97 15Designation: 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、 Dec. 1, 2012Oct. 1, 2015. Published March 2013November 2015. Originally approved in 1927, replacing D47. Last previous edition approvedin 20112012 as D97D97 12.11. DOI: 10.1520/D0097-12.10.1520/D0097-15.In the IP, this test method is under the jurisdiction of the Standardization Committee. This tes
13、t 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 Service
14、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 previous ve
15、rsion. 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 Changes se
16、ction 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 containing a
17、sphaltic 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 also us
18、ed 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 instrume
19、nt; 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 are so
20、metimesreferred 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 specimen i
21、s 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 D396.
22、4. Summary of Test Method4.1 After preliminary heating, the sample is cooled at a specified rate and examined at intervals of 3C3 C for flowcharacteristics. 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 of
23、 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, 33.233.2 mm to 34.8-mm34.8 mm outside diameter, and 115115 mm to 125mm 125 mm in height. The inside diameter of the jar can range fr
24、om 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 5454 mm 6 3 mm3 mm above the inside bottom. See Fig. 1.6.2 Thermometers, Temperature Measuring Device having the following ranges
25、and conforming to the requirementsprescribed in SpecificationEither liquid-in-glass thermometer as described in 6.2.1 E1 for thermometers:or Digital ContactTemperature ThermometerNumberThermometer Range ASTM IPHigh cloud and pour 38 to +50C 5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 t
26、o +127C 61C 63CThermometer (DCT) meeting the requirements described in 6.2.2.4 Methods forAnalysis and Testing, IP Standards for Petroleum and its Products, Part I, Vol 2.Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,U.K., http:/www.energyinst.org.D97 1526.2.1 Liquid-in-Glas
27、s Thermometers, Since separation of liquid column thermometers occasionally occurs and may escapedetection, thermometers should be checked immediately prior to the test and used only if having the following ranges andconforming to the requirements prescribed in Specification E1 they prove accurate w
28、ithin 61C (for or Specifications for IPStandard Thermometers: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 63Cexample ice point).6.2.1.1 Since separation of liquid column thermomete
29、rs occasionally occurs and may escape detection, thermometers should bechecked immediately prior to the test and used only if they prove accurate within 61 C (for example ice point).6.2.2 Digital Contact Thermometer Requirements:Parameter RequirementDCT E2877 Class G or betterTemperature range 65 C
30、to 90 CDisplay resolution 1 C minimum, preferably 0.1 CSensor type PRT, thermistor, thermocoupleSensor 3 mm OD sheath with a sensing element less than 10 mm in lengthMinimum immersion Less than 40 mm per Test MethodD7962Sample immersion depth Between 10 mm and 15 mm in the sample.Fig. 1Display accur
31、acy 500 mK (0.5 C) for combined probe and sensorResponse time less than or equal to 25 s as defined inSpecification E1137NOTE 1Dimensions are in millimetres (not to scale).FIG. 1 Apparatus for Pour Point TestD97 153Drift less than 500 mK (0.5 C) per yearCalibration error less than 500 mK (0.5 C) ove
32、r 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 demonstrated competency in temperature calibration which istracea
33、ble 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 probe be less than 30 cm in length but no less than 15 cm. A 5
34、cm long stopper, that has a low thermal conductivity, withapproximately half of it inserted in the sample tube will improve stability.6.2.2.1 The DCT calibration drift shall be checked at least annually by either measuring the ice point or against a referencethermometer in a constant temperature bat
35、h at the prescribed immersion depth to ensure compliance with 6.2.2. See Test MethodD7962.NOTE 2When a DCTs calibration drifts in one direction over 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 t
36、he test thermometer.6.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 115115 mm 6 3-mm3 mm depth, with inside diameter of 44.244.2 mmto 45.8 mm. 45.8 mm. It shall be supported in a vertical position in the cooling bath (see 6.7) so that not more than 25 mm 25 mmprojects out of the cooling m
37、edium, and shall be capable of being cleaned.6.5 Disk, cork or felt, 6 mm 6 mm thick to fit loosely inside the jacket.6.6 Gasket, Gasket Ring Form, about 5 mm in thickness, to fit snugly around the outside of the test jar and loosely inside thejacket. The gasket may be made of rubber, leather, or ot
38、her material that is elastic enough to cling to the test jar and hard enoughto hold its shape. Its purpose is to prevent the test jar from touching the jacket.6.7 Bath or Baths, maintained at prescribed temperatures with a firm support to hold the jacket vertical. The required bathtemperatures may b
39、e obtained by refrigeration if available, otherwise by suitable cooling mixtures. Cooling mixtures commonlyused for bath temperatures down to those shown are in Table 1.TABLE 1 Cooling Mixtures and Bath TemperaturesCooling Mixture BathTemperatureIce and water 0 1.5CIce and water 0 C 1.5 CCrushed ice
40、 and sodium chloride crystals orAcetone or petroleum naphtha, or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature18 1.5CCrushed ice and sodium chloride crystals orAcetone or petroleum naphtha, or methanol or ethanol (seeSection 7) with solid carbon di
41、oxide 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 1.5CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the d
42、esiredtemperature33 C 1.5 CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature51 1.5CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature51 C 1.5
43、 CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature69 1.5CAcetone or petroleum naphtha or methanol or ethanol (seeSection 7) with solid carbon dioxide added to give the desiredtemperature69 C 1.5 CD97 1547. Reagents and
44、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 ha
45、rmful).7.1.5 Solid Carbon Dioxide, (WarningExtremely cold 78.5C).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
46、to a temperature higher than 45C45 C during the preceding 24 h, 24 h, do not yield the samepour point results as when they are kept at room temperature for 24 h 24 h prior to testing. Examples of materials which are known to show sensitivityto thermal history are residual fuels, black oils, and cyli
47、nder stocks.8.1.1 Samples of residual fuels, black oils, and cylinder stocks which have been heated to a temperature higher than 45C45 Cduring the preceding 24 h, 24 h, or when the thermal history of these sample types is not known, shall be kept at room temperaturefor 24 h 24 h before testing. Samp
48、les which are known by the operator not to be sensitive to thermal history need not be kept atroom temperature for 24 h before testing.8.1.2 Experimental evidence supporting elimination of the 24-h24 h waiting period for some sample types is contained in aresearch report.58.2 Close the test jar with
49、 the cork carrying the high-pour thermometer (5.2). In the case of pour points above 36C, 36 C, usea higher range thermometer such as IP 63C or ASTM 61C. Close the test jar with the cork carrying the test thermometer (6.2).Adjust the position of the cork and thermometer so the cork fits tightly, the thermometer and the jar are coaxial, and thethermometer bulb is immersed is immersed to the correct depth. For liquid-in-glass, the thermometer bulb should be immersed soth
