1、Designation: D5853 17aDesignation: 441/99 (2004)Standard 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.
2、A number 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
3、provides 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 pr
4、oducts canbe 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, kidne
5、y, 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 Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor
6、 addi-tional 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 thi
7、s standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific hazard statements, see Section 7.1.6 This international standard was developed in accor-dance with internationally recognized principl
8、es on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of P
9、etroleum ProductsD130 Test Method for Corrosiveness 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 and
10、Petroleum ProductsD7962 Practice for Determination 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-mometersE644 Test Methods for Testing Industrial Resistanc
11、e Ther-mometersE2251 Specification for Liquid-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 digita
12、l display and associated tempera-ture sensing 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 o
13、utput. This digital output goes to a digitaldisplay and/or recording device that may be internal or external1This 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.C
14、urrent edition approved Dec. 15, 2017. Published February 2018. Originallyapproved in 1995. Last previous edition approved in 2017 as D5853 17. DOI:10.1520/D5853-17A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
15、ook of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary 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 internationa
16、l 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 the World Trade Organization Technical Barriers to Trade (TBT) Committee.
17、1to the device. These devices are sometimes referred 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 subj
18、ected to a pre-scribed treatment designed to enhance 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 solidif
19、ication of the test specimen.3.1.4 pour point, nthe 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 flowc
20、haracteristics. The lowest temperature at which 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 specif
21、ically designedfor crude oils.5.3 The maximum and 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
22、. It is especially useful forthe screening of the 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 to
23、125 mm. The inside diameter of the jar can range 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
24、 clean and free of scratches.6.1.2 Temperature Measuring DeviceEither liquid-in-glass thermometer as described in 6.1.2.1 or digital contactthermometer (DCT) meeting the requirements described in6.1.2.3.6.1.2.1 Liquid-in-Glass Thermometers, having rangesshown in the following table and conforming to
25、 the require-ments prescribed in Specification E1 or Specification E2251for thermometers:NOTE 1All dimensions are stated in millimetres. Positioning of temperature sensing devices are shown in the figure.FIG. 1 Apparatus for Pour Point TestD5853 17a2ThermometerThermometer Temperature RangeNumberASTM
26、 IPHigh cloud and pour 38 C to +50 C 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 usedon
27、ly if they are accurate within 61 C (see Test Method E77).6.1.2.3 Digital Contact Thermometer Requirements forPour Point:3Parameter RequirementDCT Guide E2877 Class F or betterNominal temperature rangeAHigh Pour: 38 C to 50 CLow Pour: 80 C to 20 CMelt Point: 32 C to 127 CDisplay resolution 0.1 C min
28、imumAccuracyB500 mK (0.5 C)Sensor type Platinum resistance thermometer (PRT)Sensor sheathC4.2 mm OD maximumSensor lengthDLess than 10 mmImmersion depthELess than 40 mm per Practice D7962Sample immersion depth Tip of sheath between 10 mm and 15 mmbelow sample meniscusFig. 1Measurement driftELess than
29、 500 mK (0.5 C) per yearResponse timeFLess than or equal to 4 s per footnote FCalibration error Less than 500 mK (0.5 C) over the range ofintended useCalibration range Consistent with temperature range of useCalibration data Four data points evenly distributed over the cali-bration range that is con
30、sistent with the range ofuse. The calibration data is to be included in thecalibration report.Calibration report From a calibration laboratory with demonstratedcompetency in temperature calibration which istraceable to a national calibration laboratory ormetrology standards bodyAThe nominal temperat
31、ure range may be different from the values shown providedthe calibration and accuracy criteria are met.BAccuracy is the combined accuracy of the DCT unit, which is the display andsensor.CSensor sheath is the tube that holds the sensing element. The value is theoutside diameter of the sheath segment
32、containing the sensor element.DThe physical length of the temperature sensing element.EAs determined by Practice D7962 or an equivalent procedure.FResponse TimeThe time for a DCT to respond to a step change in tempera-ture. The response time is 63.2 % of the step change time as determined perSection
33、 9 of Test Methods E644. The step change evaluation begins at 20 C 5 C air to 77 C 5 C with water circulating at 0.9 m s 0.09 m s past thesensor.NOTE 1When making measurements below 40 C with a PRT, itmay be necessary to use a 1000 sensor in order to obtain accuratemeasurements.NOTE 2When the DCT di
34、splay 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 sample
35、tube will improve stability.6.1.2.4 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 6.1.2.3.See Practice D7962.NOTE 3When a DCTs c
36、alibration 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 mm 6 3 mm depth,
37、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 thejacket.6.1.6 Gask
38、et, 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 touching the jacket.6.1.
39、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 (6.1.2) or any ot
40、hertemperature measuring device capable of measuring and dis-playing the designated temperature with the required precisionand accuracy. The required bath temperatures shall either beobtained by refrigeration or by suitable cooling mixtures andshall maintain the designated temperatures to within 61.
41、5 C.Cooling mixtures commonly used for bath temperatures areshown in Table 1.6.2 Water BathThe size 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 tempe
42、rature may be maintainedby any suitable means, provided the temperature can bemonitored and controlled 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 kP
43、a. Alternative designs for the pressurevessel cap and synthetic rubber gasket may be used providedthat the internal dimensions of the pressure vessel are the sameas those shown in Fig. 2.NOTE 4This pressure vessel is identical to the pressure vesseldescribed in Test Method D130.3Supporting data have
44、 been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1826. ContactASTM CustomerService at serviceastm.org.D5853 17a36.4 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 better.7. Reagents
45、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 5Typical petroleum naphtha used for cleaning purposes areVMand P naphthas.7.2 Toluen
46、e, 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 for the cooling ba
47、th.(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 6Sampling is defined as all steps required to
48、 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. Practices D4057 andD
49、4177 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 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
