1、Designation: D5853 16Designation: 441/99Standard Test Method forPour Point of Crude Oils1This standard is issued under the fixed designation D5853; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers two procedures for the deter-mination of the pour point temperatures of crude oils down to36 C. Procedure A provides
3、 a measure of the maximum(upper) pour point temperature and is described in 9.1. Proce-dure B provides a measure of the minimum (lower) pour pointtemperature and is described in 9.2.1.2 The use of this test method is limited to use for crudeoils. Pour point temperatures of other petroleum products c
4、anbe determined by Test Method D97.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kidney, and l
5、iver 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 Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-ti
6、onal information. Users should be aware that selling mercuryand/or mercury containing products in your state or countrymay be prohibited by law.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standa
7、rd to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD130 Test Method for Corrosive
8、ness to Copper from Petro-leum Products by Copper Strip TestD323 Test Method for Vapor Pressure of Petroleum Products(Reid Method)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD7962 Practice for Determinat
9、ion of Minimum ImmersionDepth and Assessment of Temperature Sensor Measure-ment DriftE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther-mometersE1137 Specification for Industrial Platinum ResistanceTher-mometersE2251 Specification for Liquid
10、-in-Glass ASTM Thermom-eters with Low-Hazard Precision LiquidsE2877 Guide for Digital Contact Thermometers3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 digital contact thermometer (DCT), nan electronicdevice consisting of a digital display and associated tempera-ture sensing
11、 probe.3.1.1.1 DiscussionThis device consists of a temperaturesensor connected to a measuring instrument; this instrumentmeasures the temperature-dependent quantity of the sensor,computes the temperature from the measured quantity, andprovides a digital output. This digital output goes to a digital1
12、This 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 Dec. 1, 2016. Published January 2017. Originallyapproved in 1995. Last previous editi
13、on approved in 2011 as D5853 11. DOI:10.1520/D5853-16.2For referenced 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.*A Summ
14、ary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established
15、 in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1display and/or recording device that may be internal or externalto the device. These devices are sometimes refe
16、rred to as a“digital thermometer.”3.1.1.2 DiscussionPET is an acronym for portable elec-tronic thermometers, a subset of digital contact thermometers(DCT).3.1.2 maximum (upper) pour point, nthe pour point ob-tained after the test specimen has been subjected to a pre-scribed treatment designed to enh
17、ance gelation of wax crystalsand solidification of the test specimen.3.1.3 minimum (lower) pour point, nthe pour point ob-tained after the test specimen has been subjected to a pre-scribed treatment designed to delay gelation of wax crystalsand solidification of the test specimen.3.1.4 pour point, n
18、the lowest temperature at which move-ment of the test specimen is observed under the conditions ofthe test.4. Summary of Test Method4.1 After preliminary heating, the test specimen is cooled ata specified rate and examined at intervals of 3 C for flowcharacteristics. The lowest temperature at which
19、movement ofthe test specimen is observed is recorded as the pour point.5. Significance and Use5.1 The pour point of a crude oil is an index of the lowesttemperature of handleability for certain applications.5.2 This is the only pour point method specifically designedfor crude oils.5.3 The maximum an
20、d minimum pour point temperaturesprovide a temperature window where a crude oil, depending onits thermal history, might appear in the liquid as well as thesolid state.5.4 The test method can be used to supplement othermeasurements of cold flow behavior. It is especially useful forthe screening of th
21、e effect of wax interaction modifiers on theflow behavior of crude oils.6. Apparatus6.1 Pour Point Test Apparatus Assembly (see Fig. 1):6.1.1 Test Jar, cylindrical, of clear glass, flat bottomed,outside diameter 33.2 mm to 34.8 mm, and height 115 mm to125 mm. The inside diameter of the jar can range
22、 from30.0 mm to 32.4 mm, within the constraint that the wallthickness shall be no greater than 1.6 mm. The jar shall have aline to indicate a sample height 54 mm 6 3 mm above theinside bottom. The inside of the test jar (up to the mark) shallbe visibly clean and free of scratches.6.1.2 Temperature M
23、easuring DeviceEither liquid-in-glass thermometer as described in 6.1.2.1 or digital contactthermometer (DCT) meeting the requirements described in6.1.2.3 and 6.1.2.4.NOTE 1All dimensions are stated in millimetres. Positioning of temperature sensing devices are shown in the figure.FIG. 1 Apparatus f
24、or Pour Point TestD5853 1626.1.2.1 Liquid-in-Glass Thermometers, having rangesshown in the following table and conforming to the require-ments prescribed in Specification E1 or Specification E2251for thermometers:ThermometerThermometer Temperature RangeNumberASTM IPHigh cloud and pour 38 C to +50 C
25、5C, S5C 1CLow cloud and pour 80 C to +20 C 6C 2CMelting point +32 C to +127 C 61C 63C6.1.2.2 Since separation of liquid column thermometersoccasionally occurs and may escape detection, the ice point ofthe thermometers shall be checked prior to the test and usedonly if they are accurate within 61 C (
26、see Test Method E77).6.1.2.3 Digital contact thermometer requirements for pourpoint:3Parameter RequirementDCT Guide E2877 Class G or betterTemperature Range 80 C to 50 CDisplay Resolution 0.1 C minimumSensor Type Platinum Resistance Thermometer (PRT)Sensor 3 mm o.d. sheath with a sensing elementless
27、 than 10 mm in lengthMinimum Immersion Less than 40 mm per Practice D7962Length of Sheath in Sample Tip of sheath between 10 mm and 15 mmbelow sample meniscus (Fig. 1).Accuracy 500 mK (0.5 C) for combined probe andsensorResponse Time Less than or equal to 25 s as defined inSpecification E1137Drift L
28、ess 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 50 CCalibration Data 4 data points evenly distributed over calibra-tion range with data included in calibrationreport.Calibration Report From a calibration labo
29、ratory with demon-strated competency in temperature calibra-tion which is traceable to a national calibra-tion laboratory or metrology standards body.6.1.2.4 Digital contact thermometer requirements for melt-ing point:Parameter RequirementDCT Guide E2877 Class E or betterTemperature Range 32 C to 13
30、0 CDisplay Resolution 0.1 C minimumSensor Type Platinum Resistance Thermometer (PRT)Sensor 3 mm o.d. sheath with a sensing elementless than 24 mm in lengthMinimum Immersion Less than 40 mm per Practice D7962Length of Sheath in Sample Tip of sheath between 10 mm and 15 mmbelow sample meniscus (Fig. 1
31、).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 32 C or lower to 130 CCalibration Data 4 da
32、ta points evenly distributed over calibra-tion range with data included in calibrationreport.Calibration Report From a calibration laboratory with demon-strated competency in temperature calibra-tion which is traceable to a national calibra-tion laboratory or metrology standards body.NOTE 1When the
33、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 between 15 cm and 30 cm in length.A 5 cm long stopper that has a low thermal conductivity with approxi-mately half of it inserted in the s
34、ample tube will improve stability.6.1.2.5 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 6.1.2.3or 6.1.2.4. See Practice D7962.NO
35、TE 2When a DCTs calibration drifts in one direction over severalcalibration checks, it is an indication of a change in the DCT, thus a fullrecalibration is necessary.6.1.3 Cork, to fit the test jar, center bored for the testthermometer.6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed,115
36、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 (6.1.7) so that no more than 25 mm projects outof the cooling medium. The jacket shall be capable of beingcleaned.6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
37、jacket.6.1.6 Gasket, to fit snugly around the outside of the test jarand loosely inside the jacket. The gasket shall be made ofrubber, leather, or other material that is sufficiently elastic tocling to the test jar and hard enough to hold its shape. Itspurpose is to prevent the test jar from touchin
38、g the jacket.6.1.7 Cooling Bath or Baths, of a type suitable for obtainingthe required temperatures. The size and shape of the bath areoptional, but a support to hold the jacket firmly in a verticalposition is essential. The bath temperature shall be monitoredby means of the appropriate thermometer
39、(6.1.2) or any othertemperature measuring device capable of measuring and dis-playing the designated temperature with the required precisionand accuracy. The required bath temperatures shall either be3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting
40、 Research Report RR:D02-1826. ContactASTM CustomerService at serviceastm.org.D5853 163obtained by refrigeration or by suitable cooling mixtures andshall maintain the designated temperatures to within 61.5 C.Cooling mixtures commonly used for bath temperatures areshown in Table 1.6.2 Water BathThe si
41、ze and shape of the bath are optional,but a support to hold the test jar immersed in the bath to abovethe sample height in the test jar and in a firm vertical positionis required. The required bath temperature may be maintainedby any suitable means, provided the temperature can bemonitored and contr
42、olled to the designated temperature (61C(9.1.4; 9.2.4).6.3 Pressure Vessel, constructed of stainless steel accordingto the dimensions given in Fig. 2, and capable of withstandinga test pressure of 700 kPa. Alternative designs for the pressurevessel cap and synthetic rubber gasket may be used provide
43、dthat the internal dimensions of the pressure vessel are the sameas those shown in Fig. 2.NOTE 3This pressure vessel is identical to the pressure vesseldescribed in Test Method D130.6.4 Timing Device, capable of measuring up to 30 s with aresolution of at least 0.1 s and an accuracy of 60.2 s or bet
44、ter.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 Petroleum Naphtha, (WarningCombustible. Vaporharmful.)NOTE 4Typical petroleum naphtha used for cleaning purposes areVMand P nap
45、hthas.7.2 Toluene, technical grade (WarningFlammable. Vaporharmful.).7.3 Solid Carbon Dioxide, (WarningExtremely cold(78.5 C).)7.4 Sodium Chloride CrystalsCommercial or technicalgrade sodium chloride is suitable.7.5 Ethanol or Ethyl AlcoholA commercial or technicalgrade of dry ethanol is suitable fo
46、r the cooling bath.(WarningFlammable. Denatured. Cannot be made non-toxic.)7.6 Methanol or Methyl AlcoholA commercial or techni-cal grade of dry methanol is suitable for the cooling bath.(WarningFlammable. Vapor harmful.)8. Sampling, Test Samples, and Test SpecimensNOTE 5Sampling is defined as all s
47、teps required to obtain a portion ofthe contents of any pipe, tank, or other system and to place the sample intothe laboratory test container.8.1 Laboratory SampleIt is essential that the samplereceived by the laboratory is representative of the batch or lotof crude oil from which it was taken. Prac
48、tices D4057 andD4177 provide guidance for obtaining such representativesamples.8.2 Preparation of Test SamplesThe pour point of crudeoils is very sensitive to trace amounts of high melting waxes.Exercise meticulous care to ensure such waxes, if present, areeither completely melted or, if volatility
49、constraints preventheating to complete melting, homogeneously suspended in thesample (Appendix X1). Inspect the walls of the originalcontainer to ensure that no high melting point material is leftsticking to the wall.NOTE 6It is not possible to define universal mandatory rules for thepreparation of crude oil test samples. Guidelines for sample handling forthe most common situations are given in Appendix X1.9. Procedure9.1 Procedure A for Maximum (Upper) Pour Point:9.1.1 Pour the test sample into the test jar
