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Standard Test Method for Pour Point of Petroleum Products1

Designation: D 97 05 Designation: 15/95An American National StandardStandard Test Method forPour Point of Petroleum Products1 This 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, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) indicates an editorial change since the last revision or Standard has been approved for use by agencies of the Department of Scope* This test Method is intended for use on any procedure suitable for black specimens, cylinderstock, and nondistillate fuel oil is described A procedurefor testing the fluidity of a residual fuel oil at a specifiedtemperature is described inAppendix Several ASTM test methods offering alternative proce-dures for determining pour points using automatic apparatusare available.

5. Significance and Use 5.1 The pour point of a petroleum specimen is an index of the lowest temperature of its utility for certain applications.

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Transcription of Standard Test Method for Pour Point of Petroleum Products1

1 Designation: D 97 05 Designation: 15/95An American National StandardStandard Test Method forPour Point of Petroleum Products1 This 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, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscriptepsilon (e) indicates an editorial change since the last revision or Standard has been approved for use by agencies of the Department of Scope* This test Method is intended for use on any procedure suitable for black specimens, cylinderstock, and nondistillate fuel oil is described A procedurefor testing the fluidity of a residual fuel oil at a specifiedtemperature is described inAppendix Several ASTM test methods offering alternative proce-dures for determining pour points using automatic apparatusare available.

2 None of them share 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 Standard does not 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 Referenced Standards: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 Pumpability of Industrial Fuel OilsD 5853 Test Method for pour Point of Crude OilsE1 Specification for ASTM Liquid-in-Glass Institute Standards.

3 Specifications for IP Standard Thermometers53. oil,n lubricant containing asphaltic oils are used in heavy-duty equipment applications, suchas mining and quarrying, where extra adhesiveness is stock,n lubricant 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 Point ,n in Petroleum products, the lowesttemperature at which movement of the test specimen isobserved under prescribed conditions of fuel,n a liquid fuel containing bottomsremaining from crude distillation or thermal cracking; some-times referred to as heavy fuel Residual fuels comprise Grades 4, 5,and 6 fuel oils, as defined in SpecificationD Summary of Test After preliminary heating, the sample is cooled at aspecified rate and examined at intervals of 3 C for flowcharacteristics.

4 The lowest temperature at which movement ofthe specimen is observed is recorded as the pour test Method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of on Flow edition approved June 1, 2005. Published July 2005. Originally approvedin 1927, replacing D 47. Last previous edition approved in 2004 as D 97 the IP, this test Method is under the jurisdiction of the StandardizationCommittee. This test Method was adopted as a joint ASTM-IP Standard in defining this test and its significance when applied to electricalinsulating oils of mineral origin will be found in Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC.

5 For suggestions on the testing of reagents notlisted by the American Chemical Society, seeAnnual Standards for LaboratoryChemicals,BDH Ltd., Poole, Dorset, , and theUnited States Pharmacopeiaand National Formulary, Pharmacopeial Convention, Inc. (USPC), Rockville, for Analysis and Testing,IP Standards for Petroleum and its Products,Part I, Vol *A Summary of Changes section appears at the end of this ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Significance and The pour Point of a Petroleum specimen is an index ofthe lowest temperature of its utility for certain Jar, cylindrical, of clear glass, flat bottom, outside diameter, and 115 to 125 mm in height.

6 Theinside diameter of the jar can range from to mm,within the constraint that the wall thickness be no greater mm. The jar shall have a line to indicate a sample height 5463 mm above the inside bottom. SeeFig. , having the following ranges and con-forming to the requirements prescribed in SpecificationE1forthermometers:Temperatu reThermometerNumberThermometerRangeASTMI PHigh cloud and pour 38 to +50 C5C1 CLow cloud and pour 80 to +20 C6C2 CMelting Point +32 to +127 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 within61 C (for example ice Point ).

7 , to fit the test jar, bored centrally for the , watertight, cylindrical, metal, flat-bottomed, 11563-mm depth, with inside diameter of to mm. Itshall be supported in a vertical position in the cooling bath ( ) so that not more than 25 mm projects out of the coolingmedium, and shall be capable of being , cork or felt, 6 mm thick to fit loosely inside , to fit snugly around the outside of the test jarand loosely inside the jacket. The gasket may be made ofrubber, leather, or other 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 or Baths, maintained at prescribed temperatureswith a firm support to hold the jacket vertical.

8 The requiredbath temperatures may be obtained 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 water9 CCrushed ice and sodium chloride crystals 12 CCrushed ice and calcium chloride crystals 27 CAcetone or Petroleum naphtha (see Section6) chilledin a covered metal beaker with an ice-salt mixture to 12 Cthen with enough solid carbon dioxide to give the desired tem-perature. 57 C7. Reagents and The following solvents of technical grade are appropri-ate for low-temperature bath ,(Warning Extremely flammable). , Ethanol(Warning Flammable).

9 NOTE Dimensions are in millimetres (not to scale).FIG. 1 Apparatus for pour Point TestD97 , Methanol(Warning Flammable. Vaporharmful). Naphtha,(Warning Combustible. Vaporharmful). Carbon Dioxide,(Warning Extremely cold C).8. pour the specimen into the test jar to the level necessary, heat the specimen in a water bath until it isjust sufficiently fluid to pour into the test It 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 sensitivity tothermal history are residual fuels, black oils, and cylinder 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 roomtemperature for 24 h before testing.

10 Samples which are knownby the operator not to be sensitive to thermal history need notbe kept at room temperature for 24 h before Experimental evidence supporting elimination of the24-h waiting period for some sample types is contained in aresearch Close the test jar with the cork carrying the high-pourthermometer ( ). In the case of pour points above 36 C, usea higher range thermometer such as IP 63C or ASTM 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 For the measurement of pour Point , subject the speci-men in the test jar to the following preliminary Having pour points Above 33 C Heatthe 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.


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