1、Designation: D5853 16D5853 17Designation: 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 rev
2、ision. 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 determination of the pour point temperatures of crude oils down to 36 C.Proced
3、ure A provides a measure of the maximum (upper) pour point temperature and is described in 9.1. Procedure B providesa measure of the minimum (lower) pour point temperature and is described in 9.2.1.2 The use of this test method is limited to use for crude oils. Pour point temperatures of other petro
4、leum products can bedetermined by Test Method D97.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous sys
5、tem, 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 product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury
6、/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products in your state or country may be prohibited by law.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the
7、 user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazard statements, see Section 7.1.6 This international standard was developed in accordance with internationally recognized principles on s
8、tandardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum
9、ProductsD130 Test Method for Corrosiveness to Copper from Petroleum Products by Copper Strip TestD323 Test Method for Vapor Pressure of Petroleum Products (Reid Method)D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petrole
10、um ProductsD7962 Practice for Determination of Minimum Immersion Depth and Assessment of Temperature Sensor Measurement DriftE1 Specification for ASTM Liquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of ThermometersE1137 Specification for Industrial Platinum Resistance The
11、rmometersE2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision LiquidsE2877 Guide for Digital Contact Thermometers3. Terminology3.1 Definitions of Terms Specific to This Standard:1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Li
12、quid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved Dec. 1, 2016May 1, 2017. Published January 2017May 2017. Originally approved in 1995. Last previous edition approved in 20112016 asD5853 11.D5853 16. DOI: 10.1520/D5853-16.10
13、.1520/D5853-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service 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 i
14、ntended only to provide the user of an ASTM standard an indication of what changes have been made to the previous 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 cu
15、rrent versionof the standard as published by ASTM is to be considered the official document.*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 States13.1.1 digital contact thermom
16、eter (DCT), nan electronic device consisting of a digital display and associated temperaturesensing probe.3.1.1.1 DiscussionThis device consists of a temperature sensor connected to a measuring instrument; this instrument measures the temperature-dependent quantity of the sensor, computes the temper
17、ature 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 sometimesreferred to as a “digital thermometer.”3.1.1.2 DiscussionPET is an acronym for portable ele
18、ctronic thermometers, a subset of digital contact thermometers (DCT).3.1.2 maximum (upper) pour point, nthe pour point obtained after the test specimen has been subjected to a prescribedtreatment designed to enhance gelation of wax crystals and solidification of the test specimen.3.1.3 minimum (lowe
19、r) pour point, nthe pour point obtained after the test specimen has been subjected to a prescribedtreatment designed to delay gelation of wax crystals and solidification of the test specimen.3.1.4 pour point, nthe lowest temperature at which movement of the test specimen is observed under the condit
20、ions of thetest.4. Summary of Test Method4.1 After preliminary heating, the test specimen is cooled at a specified rate and examined at intervals of 3 C for flowcharacteristics. The lowest temperature at which movement of the test specimen is observed is recorded as the pour point.5. Significance an
21、d Use5.1 The pour point of a crude oil is an index of the lowest temperature of handleability for certain applications.5.2 This is the only pour point method specifically designed for crude oils.5.3 The maximum and minimum pour point temperatures provide a temperature window where a crude oil, depen
22、ding on itsthermal history, might appear in the liquid as well as the solid state.5.4 The test method can be used to supplement other measurements of cold flow behavior. It is especially useful for thescreening of the effect of wax interaction modifiers on the flow behavior of crude oils.6. Apparatu
23、s6.1 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 125 mm.The inside diameter of the jar can range from 30.0 mm to 32.4 mm, within the constraint that the wall thickness shall be n
24、o greaterthan 1.6 mm. The jar shall have a line to indicate a sample height 54 mm 6 3 mm above the inside bottom. The inside of the testjar (up to the mark) shall be visibly clean and free of scratches.6.1.2 Temperature Measuring DeviceEither liquid-in-glass thermometer as described in 6.1.2.1 or di
25、gital contact thermometer(DCT) meeting the requirements described in 6.1.2.3 and 6.1.2.4.6.1.2.1 Liquid-in-Glass Thermometers, having ranges shown in the following table and conforming to the requirementsprescribed in Specification E1 or Specification E2251 for thermometers:ThermometerThermometer Te
26、mperature Range NumberASTM 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 thermometers occasionally occurs and may escape detection, the ice point of thethermometers shall be checked p
27、rior to the test and used only if they are accurate within 61 C (see Test Method E77).6.1.2.3 Digital contact thermometer requirements for pour point:3Parameter RequirementDCT Guide E2877 Class G or better3 Supporting data have been filed at ASTM International Headquarters and may be obtained by req
28、uesting Research Report RR:D02-1826. Contact ASTM CustomerService at serviceastm.org.D5853 172Temperature 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 element less than 10 mm in lengthMinimum Immersion Less
29、than 40 mm per Practice D7962Length of Sheath in Sample Tip of sheath between 10 mm and 15 mm below sample meniscus (Fig. 1).Accuracy 500 mK (0.5 C) for combined probe and sensorResponse Time Less than or equal to 25 s as defined in Specification E1137Drift Less than 500 mK (0.5 C) per yearCalibrati
30、on Error Less than 500 mK (0.5 C) over the range of intended use.Calibration Range 40 C or lower to 50 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 t
31、emperature calibration whichis traceable to a national calibration laboratory or metrology standards body.6.1.2.4 Digital contact thermometer requirements for melting point:Parameter RequirementDCT Guide E2877 Class E or betterTemperature Range 32 C to 130 CDisplay Resolution 0.1 C minimumSensor Typ
32、e Platinum Resistance Thermometer (PRT)NOTE 1All dimensions are stated in millimetres. Positioning of temperature sensing devices are shown in the figure.FIG. 1 Apparatus for Pour Point TestD5853 173Sensor 3 mm o.d. sheath with a sensing element less than 24 mm in lengthMinimum Immersion Less than 4
33、0 mm per Practice D7962Length of Sheath in Sample Tip of sheath between 10 mm and 15 mm below sample meniscus (Fig. 1).Accuracy 500 mK (0.5 C) for combined probe and sensorResponse Time Less than or equal to 25 s as defined in Specification E1137Drift Less than 500 mK (0.5 C) per yearCalibration Err
34、or Less than 500 mK (0.5 C) over the range of intended use.Calibration Range 32 C or lower to 130 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 temper
35、ature calibration whichis traceable to a national calibration laboratory or metrology standards body.NOTE 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 between 15 cm and 30
36、cm in length. A 5 cm long stopper that has a low thermal conductivity with approximately halfof it inserted in the sample tube will improve stability.6.1.2.5 The DCT calibration drift shall be checked at least annually by either measuring the ice point or against a referencethermometer in a constant
37、 temperature bath at the prescribed immersion depth to ensure compliance with 6.1.2.3 or 6.1.2.4. SeePractice D7962.NOTE 2When a DCTs calibration drifts in one direction over several calibration checks, it is an indication of a change in the DCT, thus a fullrecalibration is necessary.6.1.3 Cork, to
38、fit the test jar, center bored for the test thermometer.6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed, 115 mm 6 3 mm depth, with inside diameter of 44.2 mm to 45.8 mm.It shall be supported in a vertical position in the cooling bath (6.1.7) so that no more than 25 mm projects out of the
39、 coolingmedium. The jacket shall be capable of being cleaned.6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside the jacket.6.1.6 Gasket, to fit snugly around the outside of the test jar and loosely inside the jacket. The gasket shall be made of rubber,leather, or other material that is suffi
40、ciently elastic to cling to the test jar and hard enough to hold its shape. Its purpose is to preventthe test jar from touching the jacket.6.1.7 Cooling Bath or Baths, of a type suitable for obtaining the required temperatures. The size and shape of the bath areoptional, but a support to hold the ja
41、cket firmly in a vertical position is essential.The bath temperature shall be monitored by meansof the appropriate thermometer (6.1.2) or any other temperature measuring device capable of measuring and displaying thedesignated temperature with the required precision and accuracy. The required bath t
42、emperatures shall either be obtained byrefrigeration or by suitable cooling mixtures and shall maintain the designated temperatures to within 61.5 C. Cooling mixturescommonly used for bath temperatures are shown in Table 1.TABLE 1 Cooling Mixtures and Bath TemperaturesBath TemperatureIce and water 0
43、 C 1.5CCrushed ice and sodium chloride crystals orAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature18 C 1.5CAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the de
44、sired temperature33 C 1.5CAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature51 C 1.5CAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature69 C 1.
45、5CD5853 1746.2 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 position is required. The required bath temperature may be maintained byany suitable means, provided the temp
46、erature can be monitored and controlled to the designated temperature (61 C (9.1.4; 9.2.4).6.3 Pressure Vessel, constructed of stainless steel according to the dimensions given in Fig. 2, and capable of withstanding atest pressure of 700 kPa. Alternative designs for the pressure vessel cap and synth
47、etic rubber gasket may be used provided thatthe internal dimensions of the pressure vessel are the same as those shown in Fig. 2.NOTE 3This pressure vessel is identical to the pressure vessel described in Test Method D130.6.4 Timing Device, capable of measuring up to 30 s with a resolution of at lea
48、st 0.1 s and an accuracy of 60.2 s or better.FIG. 2 Pressure VesselD5853 1757. Reagents and Materials7.1 The following solvents of technical grade are appropriate for low-temperature bath media.7.1.1 Acetone, (WarningExtremely flammable.)7.1.2 Petroleum Naphtha, (WarningCombustible. Vapor harmful.)N
49、OTE 4Typical petroleum naphtha used for cleaning purposes are VM and P naphthas.7.2 Toluene, technical grade (WarningFlammable. Vapor harmful.).7.3 Solid Carbon Dioxide, (WarningExtremely cold (78.5 C).)7.4 Sodium Chloride CrystalsCommercial or technical grade sodium chloride is suitable.7.5 Ethanol or Ethyl AlcoholA commercial or technical grade of dry ethanol is suitable for the cooling bath. (WarningFlammable. Denatured. Cannot be made nontoxic.)7.6 Methanol or Methyl AlcoholA co
