ASTM D5985-2002(2014) 2011 Standard Test Method for Pour Point of Petroleum Products &40 Rotational Method&41 《石油产品倾点40 旋转法41的标准试验方法》.pdf

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1、Designation: D5985 02 (Reapproved 2014)Standard Test Method forPour Point of Petroleum Products (Rotational Method)1This standard is issued under the fixed designation D5985; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year

2、 of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThis test method covers an alternative procedure for the determination of pour point of petroleumproducts using an

3、 automatic apparatus.1. Scope1.1 This test method covers the determination of pour pointof petroleum products by an automatic instrument that con-tinuously rotates the test specimen against a suspended detec-tion device during cooling of the test specimen.1.2 This test method is designed to cover th

4、e range oftemperatures from 57 to +51C; however, the range oftemperatures included in the 1992 interlaboratory programonly covered the temperature range of 39 to +6C (see 13.4).1.3 This test method determines the no-flow point of petro-leum products by detection of the crystal structure or viscosity

5、increase, or both, in the sample that is sufficient to impede flowof the specimen.1.4 This test method is not intended for use with crude oils.NOTE 1The applicability of this test method on residual fuel sampleshas not been verified. For further information on applicability, refer to13.4.1.5 The val

6、ues stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 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 standard to establish appro-priate sa

7、fety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling

8、of Petroleum andPetroleum Products2.2 Energy Institute Standards:3IP 15 Test Method for Pour Point of Petroleum Products3. Terminology3.1 Definitions:3.1.1 pour point, nin petroleum products, the lowesttemperature at which movement of the test specimen isobserved under prescribed conditions of test.

9、3.2 Definitions of Terms Specific to This Standard:3.2.1 no-flow point, nin petroleum products, the tempera-ture of the test specimen at which a wax crystal structure orviscosity increase, or both, impedes movement of the surfaceof the test specimen under the conditions of the test.3.2.2 DiscussionT

10、he no-flow point occurs when, uponcooling, the formation of wax crystal structures or viscosityincrease, or both, have progressed to the point where theapplied observation device no longer detects movement underthe conditions of the test. The preceding observationtemperature, at which flow of the te

11、st specimen is lastobserved, is the pour point.3.2.3 pour point at 3C testing intervals, nin petroleumproducts, the temperature calculated by rounding the no-flowpoint of the test specimen to the next higher integer which is amultiple of 3C.1This test method is under the jurisdiction of ASTM Committ

12、ee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1996. Last previous edition approved in 2008 as D598502(2008).DOI: 10.1520/D5985-0

13、2R14.2For 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.3Available from Energy Institute, 61 New Cavendish St.,

14、London, WIG 7AR,U.K., http:/www.energyinst.org.uk.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.4 DiscussionThe no-flow point can be measured witha resolution of 0.1C in this test method. In Test Method D97observations for no-fl

15、ow are in 3C intervals and when resultswith a similar format to Test Method D97 are required, thiscalculation shall be performed. Some apparatus can performthis calculation automatically.3.2.5 rotational, nin this standard, the technique of turn-ing the test specimen jar in an upright position upon

16、a turntablewith a stationary positioned, temperature sensor containingpendulum, inserted into the test specimen.3.2.6 DiscussionUpon cooling of the test specimen, theresultant crystal formation or viscosity increase in the speci-men exerts force upon the pendulum, offsetting the stationaryposition a

17、nd causing detection of the no-flow point.4. Summary of Test Method4.1 After inserting the test specimen into the automatic pourpoint apparatus, and initiation of the program, the test speci-men is heated and then cooled by maintaining a constanttemperature differential between the cooling block and

18、 thesample. The test specimen is continuously tested for flowcharacteristics by rotating the test specimen cup at approxi-mately 0.1 rpm against a stationary, counter-balanced, sphere-shaped pendulum. The temperature of the test specimen atwhich a crystal structure or a viscosity increase, or both,

19、withinthe test specimen causes the displacement of the pendulum isrecorded with a resolution of 0.1C. The test specimen is thenheated to the original starting temperature.5. Significance and Use5.1 The pour point of a petroleum product is an index of thelowest temperature of its utility for certain

20、applications. Flowcharacteristics, such as pour point, can be critical for thecorrect operation of lubricating systems, fuel systems, andpipeline operations.5.2 Petroleum blending operations require precise measure-ment of the pour point.5.3 This test method can determine the temperature of thetest

21、specimen with a resolution of 0.1C at which eithercrystals have formed or viscosity increases sufficiently toimpede movement of the petroleum product.5.4 This test method yields a pour point in a format similarto Test Method D97/IP15 when the 3C interval results arereported.NOTE 2Since some users ma

22、y wish to report their results in a formatsimilar to Test Method D97 (in 3C intervals) the precisions were derivedfor the temperatures rounded to the 3C intervals. For statements on biasrelative to Test Method D97, see 13.3.5.5 This test method has better repeatability and comparablereproducibility

23、relative to Test Method D97 as measured in the1992 interlaboratory program. (See Section 13.)6. Apparatus6.1 Automatic Apparatus4The automatic pour point appa-ratus described in the Annex A1 consists of a microprocessorcontrolled measuring unit that is capable of heating, cooling,rotating, and recor

24、ding the temperature of the test specimen.The apparatus shall be equipped with a digital display, cooling/heating block assembly, turntable, test specimen cup andmeasuring head containing a counter-balanced pendulum andtemperature measuring device.6.2 Test Specimen CupThe test specimen cup is a flat

25、bottom aluminum cup with the dimensions in A1.2. To indicatethe required fill level, the inside of the test cup is scribed at aheight of 36 6 0.2 mm above the inside bottom. The outsidebottom of the test cup has two indentions to facilitate therotation of the test cup.6.3 Circulating BathRefrigerati

26、on unit equipped with acirculating pump capable of maintaining a temperature at least20C colder than the lowest expected pour point to bemeasured.7. Reagents and Material7.1 Methyl Alcohol, anhydrous, for use as cooling mediumin circulating bath.7.2 Cleaning Solvents, suitable for cleaning and dryin

27、g thespecimen cup and pendulum, such as petroleum naptha andacetone. (WarningFlammable. Liquid causes eye burns.Vapor harmful. May be fatal or cause blindness if swallowed orinhaled.)8. Sampling8.1 Obtain a sample in accordance with Practices D4057 orby D4177.8.2 Samples of very viscous materials ca

28、n be warmed untilthey are reasonably fluid before they are transferred; however,no sample shall be heated more than is absolutely necessary.The sample shall not be heated and transferred into the testspecimen cup unless its temperature is 70C or lower.NOTE 3In the event the sample has been heated ab

29、ove thistemperature, allow the sample to cool until its temperature is at least 70Cbefore transferring.9. Preparation of Apparatus9.1 Prepare the instrument for operation in accordance withthe manufacturers instructions.9.2 Clean and dry the test specimen cup and the coolingwell using suitable solve

30、nts as prescribed by the apparatusmanufacturer.4The sole source of supply of the instrument known to the committee at this timeis Herzog Model MC 850, available from Walter Herzog, Lauda, Germany. If youare aware of alternative suppliers, please provide this information to ASTMInternational Headquar

31、ters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.D5985 02 (2014)29.3 Prepare the refrigerated circulating bath for operation inaccordance with the manufacturers instructions and allow it toattain a temperature at least 20

32、C lower than the expected pourpoint of the sample.10. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions forcalibrating, checking, and operating the apparatus are fol-lowed.10.2 Adjust the position of the measuring pendulum, whennecessary, according to the manufact

33、urers instructions.10.3 A sample with a well documented pour point can beused to verify performance of the apparatus. Alternatively, asample which has been extensively tested in a pour pointinterlaboratory study can be used.11. Procedure11.1 Transfer the specimen into the test specimen cup to thescr

34、ibed mark. When necessary, heat the sample in a water bathor oven until it is just sufficiently fluid to transfer into the testspecimen cup. Samples with an expected pour point above36C or which appear solid at room temperature can be heatedabove 45C but shall not be heated above 70C (see Note 3).NO

35、TE 4Residual fuels have been known to be sensitive to thermalhistory. In the case where a residual fuel sample is tested, refer to TestMethod D97 for sample treatment.11.2 Make sure that the cooling well is free of moisture. Ifit is not, remove all moisture by wiping with a dry cloth. Insertthe test

36、 specimen cup into the cooling well. Bring the measur-ing head into position over the test specimen cup and lower itinto the test specimen.11.3 Start the test program following the manufacturersinstructions.11.4 When the expected pour point is known to be higherthan 33C, preselect a starting tempera

37、ture which is at least9C higher than the expected pour point, but at least 45C. Thehighest starting temperature that can be programmed is 70C.11.5 When the expected pour point is known to be at orbelow 33C, the test duration can be shortened by preselect-ing a starting temperature which is at least

38、9C higher than theexpected pour point. The lowest starting temperature that canbe programmed is 20C.11.6 When the expected pour point is not known and thesample appears to be liquid, preselect a starting temperature of45C. The apparatus automatically heats the test specimen toapproximately 45C when

39、a starting temperature is not se-lected. When the expected pour point is not known and thesample needs to be heated before transferring into the testspecimen cup, preselect a starting temperature of 70C.11.7 Initially, the test specimen is heated to approximately45C, or to the starting temperature p

40、reselected by the operatorbetween 20 and 70C. The test specimen cup is continuouslyrotated at approximately 0.1 rpm and flow of the cooling fluidfrom the circulating bath is regulated to maintain the coolingblock at a temperature approximately 8C lower than the testspecimen temperature. The test spe

41、cimen temperature is con-tinuously displayed. At the detection of the last flow point, thetemperature the test specimen attained is held on the digitaldisplay until reset by the operator. The test specimen is thenheated to approximately 45C, or to the preselected tempera-ture.11.8 The test specimen

42、temperature rounded up to the next3C integer is also displayed.12. Report12.1 Report the temperature recorded in 11.7, with resolu-tion of 0.1C, as the no-flow point in accordance with TestMethod D5985 (rotational method).12.2 Report the temperature recorded in 11.8 as the pourpoint at 3C testing in

43、tervals in accordance with Test MethodD5985.13. Precision and Bias13.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults is as follows:513.1.1 Pour Point at 3C Testing Intervals (RotationalMethod):13.1.1.1 RepeatabilityThe dif

44、ference between successivetest results, obtained by the same operator using the sameapparatus under constant operating conditions on identical testmaterial, would in the long run, in the normal and correctoperation of this test method, exceed the following only in onecase in twenty.2.3C13.1.1.2 Repr

45、oducibilityThe difference between twosingle and independent test results, obtained by differentoperators working in different laboratories on identical testmaterial, would in the long run, in normal and correct operationof this test method, exceed the following only in one case intwenty.8.7C13.1.2 N

46、o-Flow PointRepeatabilityThe difference be-tween successive test results, obtained by the same operatorusing the same apparatus under constant operating conditionson identical test material, would in the long run, in the normaland correct operation of this test method, exceed the followingonly in on

47、e case in twenty.1.18C13.2 BiasSince there is no accepted reference materialsuitable for determining the bias for the procedure in this testmethod, bias has not been determined.13.3 Relative Bias:13.3.1 Pour points at 3C testing intervals were compared tothe results from Test Method D97. Relative bi

48、as5amongcertain samples was observed; however, the observed bias doesnot appear to be of a systematic nature. Biases relative to Test5Supporting data (results of the 1992 interlaboratory cooperative test program)have been filed at ASTM International Headquarters and may be obtained byrequesting Rese

49、arch Report RR:D02-1312.D5985 02 (2014)3Method D97/IP15 may conceivably occur for sample types notincluded in the laboratory test program.NOTE 5Large differences in results were observed between methodsfor one sample in the Interlaboratory Test Study. The sample was ahigh-sulfur winter diesel. When cooled during the performance of a testmethod, this sample formed thin, but very large crystals, that could bedescribed as large plates. These crystals formed wherever sample-glasscontact was made as well as cover