1、Designation: D5853 11Designation: 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 to36C. 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 ca
4、nbe 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 liv
5、er 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-tion
6、al information. Users should be aware that selling mercuryand/or mercury containing products into 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 Pe-troleum Products by Copper Strip TestD323 Test Method for Vapor Pressure of Petroleum Prod-ucts (Reid Method)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM L
9、iquid-in-Glass ThermometersE77 Test Method for Inspection and Verification of Ther-mometers3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 maximum (upper) pour point, nthe pour point ob-tained after the test specimen has been subjected to a pre-scribed treatment designed to en
10、hance gelation of wax crystalsand solidification of the test specimen.3.1.2 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.3.1.3 pour point,
11、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 3C for flow1This test method is under the jurisdiction of AS
12、TM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved June 1, 2011. Published July 2011. Originally approvedin 1995. Last previous edition approved in 2009 as D585309. DOI: 10.1520/D5853-11.2For referen
13、ced 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.1*A Summary of Changes section appears at the end of this standard.Copyri
14、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.characteristics. 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
15、the lowesttemperature of handleability for certain applications.5.2 This is the only pour point method specifically 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
16、 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 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 T
17、est Jar, cylindrical, of clear glass, flat bottomed,outside diameter 33.2 to 34.8 mm, and height 115 to 125 mm.The inside diameter of the jar can range from 30.0 to 32.4 mm,within the constraint that the wall thickness shall be no greaterthan 1.6 mm. The jar shall have a line to indicate a samplehei
18、ght 54 6 3 mm above the inside bottom. The inside of thetest jar (up to the mark) shall be visibly clean and free ofscratches.6.1.2 Thermometers, having ranges shown in the followingtable and conforming to the requirements prescribed in Speci-fication E1 for thermometers:ThermometerThermometer Tempe
19、rature RangeNumberASTM IPHigh cloud and pour 38 to +50C 5C 1CLow cloud and pour 80 to +20C 6C 2CMelting point +32 to +127C 61C 63C6.1.2.1 Since separation of liquid column thermometersoccasionally occurs and may escape detection, the ice point ofthe thermometers shall be checked prior to the test an
20、d usedonly if they are accurate within 61C (see Test Method E77).6.1.3 Cork, to fit the test jar, center bored for the testthermometer.6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed,115 6 3 mm depth, with inside diameter of 44.2 to 45.8 mm.It shall be supported in a vertical position in
21、 the cooling bath(6.1.7) so that no more than 25 mm projects out of the coolingmedium. The jacket shall be capable of being cleaned.6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside thejacket.6.1.6 Gasket, to fit snugly around the outside of the test jarand loosely inside the jacket. The ga
22、sket 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.6.1.7 Cooling Bath or Baths, of a type suitable for obtainingthe required temperatures. The s
23、ize and shape of the bath areoptions, 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 otherNOTEAll dimensions are stated in millimetres.FIG. 1 Apparatus for Pour Point TestD5853
24、112temperature 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.
25、5C.Cooling mixtures commonly used for bath temperatures areshown in Table 1.6.2 Water BathThe size and shape of the bath are op-tional, but a support to hold the test jar immersed in the bath toabove the sample height in the test jar and in a firm verticalposition is required. The required bath temp
26、erature may bemaintained by any suitable means, provided the temperaturecan be monitored 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 k
27、Pa. 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 1This pressure vessel is identical to the pressure vesseldescribed in Test Method D130.6.4 Timing Device, c
28、apable 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 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,(WarningComb
29、ustible. Vaporharmful.)NOTE 2Typical petroleum naphtha used for cleaning purposes areVM and P naphthas.7.2 Toluene, technical grade (WarningFlammable. Vaporharmful.).7.3 Solid Carbon Dioxide,(WarningExtremely cold(78.5C).)7.4 Sodium Chloride CrystalsCommercial or technicalgrade sodium chloride is su
30、itable.7.5 Ethanol or Ethyl AlcoholA commercial or technicalgrade of dry ethanol is suitable for 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.
31、 Vapor harmful.)8. Sampling, Test Samples, and Test SpecimensNOTE 3Sampling is defined as all steps 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
32、 the laboratory is representative of the batch or lotof crude oil from which it was taken. Practices 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 m
33、eticulous 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
34、to the wall.NOTE 4It 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
35、test jar to the level mark.If necessary, reheat the test sample to a temperature at least20C above the expected pour point (8.2 andAppendix X1) butnot higher than a temperature of 60C (WarningThe vaporpressure of crude oils at temperatures higher than 60C willusually exceed 100 kPa. Under these circ
36、umstances the samplecontainer may rupture. Opening of the container may inducefoaming with resultant loss of sample and possible injury topersonnel.)TABLE 1 Cooling Mixtures and Bath TemperaturesBath TemperatureIce and water 0 6 1.5CCrushed ice and sodium chloride crystals orAcetone or petroleum nap
37、htha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature18 6 1.5CAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature33 6 1.5CAcetone or petroleum naphtha or methanol or etha
38、nol(see Section 7) with solid carbon dioxide added togive the desired temperature51 6 1.5CAcetone or petroleum naphtha or methanol or ethanol(see Section 7) with solid carbon dioxide added togive the desired temperature69 6 1.5CD5853 1139.1.2 Immediately close the test jar with the cork carryingthe
39、high cloud and pour thermometer, or, if the expected pourpoint is above 36C, the melting point thermometer.Adjust theposition of the cork and thermometer so the cork fits tightly, thethermometer and the jar are coaxial, and the thermometer bulbis immersed to a depth that places the beginning of thec
40、apillary 3 mm below the surface of the test specimen.9.1.3 Keep the test jar with the test specimen at roomtemperature (between 18 and 24C) for at least 24 h.NOTE 5The pour point of a crude oil is dependent on the state ofcrystallization of the wax in the test specimen. In crude oils, achievingequil
41、ibrium between crystallized wax and dissolved wax is a rather slowprocess. However, experience has shown that in a majority of cases, suchan equilibrium is reached within 24 h.9.1.4 If the expected pour point is greater than 36C, heatthe sample to 9C above the expected pour point. If theexpected pou
42、r point is less than 36C, heat the sample to atemperature of 45 6 1C. Maintain the water bath (6.2) to heatthe sample at 48 6 1C or at a temperature 12C higher thanthe expected pour point, whichever is higher.FIG. 2 Pressure VesselD5853 1149.1.4.1 As soon as the test specimen has reached therequired
43、 temperature, remove the cork carrying the thermom-eter and stir the test specimen gently with a spatula or similardevice. Put the cork carrying the thermometer back in place(see 9.1.2).9.1.5 Ensure that the disk, gasket, and the inside of thejacket are clean and dry. Place the disk in the bottom of
44、 thejacket. Place the disk and jacket in the cooling medium aminimum of 10 min before the test jar is inserted. The use ofa jacket cover, while the empty jacket is cooling, is permitted.Remove the test jar from the water bath and dry with a tissue.Place the gasket around the test jar, 25 mm from the
45、 bottom.Insert the test jar into the jacket in the first bath maintained at21C and commence observations for pour point. Never placea test jar directly into the cooling medium.9.1.6 Exercise care not to disturb the mass of test specimennor permit the thermometer to shift in the test specimen; anydis
46、turbance of the spongy network of wax crystals will lead toa lower pour point and erroneous results (Note 5).NOTE 6With dark colored materials, such as crude oils, it is imprac-tical to observe, in the test jar, the onset of crystallization and networkformation in the test specimen. Hence, it is pre
47、sumed that networkformation will begin at the very early stages of the cooling sequence.9.1.7 Pour points are expressed in temperatures which arepositive or negative multiples of 3C. Begin to examine theappearance of the test specimen when the temperature of thetest specimen is 9C above the expected
48、 pour point (estimatedas a multiple of 3C). At each test thermometer reading whichis a multiple of 3C below the starting temperature, remove thetest jar from the jacket. When necessary, remove moisture thatlimits visibility of the test specimen by wiping the surface ofthe test jar with a clean cloth
49、 moistened in alcohol atapproximately the temperature of the test specimen in the jar.Then tilt the jar just enough to ascertain whether there ismovement of the test specimen in the jar. When movement isobserved, immediately return the test jar into the jacket. Ifmovement of the specimen in the test jar is noted, then replacethe test jar immediately in the jacket, and repeat a test for flowat the next temperature, 3C lower. Typically the completeoperation of removal, wiping, and replacement shall requirenot more
