1、Designation: D5950 14Standard Test Method forPour Point of Petroleum Products (Automatic Tilt Method)1This standard is issued under the fixed designation D5950; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. 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 automatic app
3、aratus.1. Scope*1.1 This test method covers the determination of pour pointof petroleum products by an automatic instrument that tilts thetest jar during cooling and detects movement of the surface ofthe test specimen with an optical device.1.2 This test method is designed to cover the range oftempe
4、ratures from 66 C to +51 C; however, the range oftemperatures included in the 1992 interlaboratory test programonly covered the temperature range from 39 C to +6 C, andthe range of temperatures included in the 1998 interlaboratorytest program was 51 C to 11 C. (See Section 13.)1.3 Test results from
5、this test method can be determined at1 C or 3 C intervals.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 values stated in SI units a
6、re 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 safety and health practice
7、s 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 of Petroleum andPetroleu
8、m ProductsD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a Material2.2 Energy Institute Standard:3IP 15 Test Method for Pour Point of Petroleum Products3. Terminology3.1 Definitions:3.1.1 pour point,
9、 nin petroleum products, the lowesttemperature at which movement of the test specimen isobserved under the prescribed conditions of this test method.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 cr
10、ystal structure orviscosity increase, or both, impedes movement of the surfaceof the test specimen under the conditions of the test.3.2.1.1 DiscussionThe no-flow point occurs when, uponcooling, the formation of wax crystal structures or the viscosityincrease, or both, has progressed to the point whe
11、re the appliedobservation device no longer detects movement under theconditions of the test. The preceding observation temperature,at which flow of the test specimen is last observed, is the pourpoint.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuel
12、s, and Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved May 1, 2014. Published June 2014. Originallyapproved in 1996. Last previous edition approved in 2012 as D5950 12a. DOI:10.1520/D5950-14.2For referenced ASTM standards, visit the ASTM
13、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., London, WIG 7AR,U.K., http:/www.energyinst.org.uk.*A
14、 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 States13.2.2 tilting, vtechnique of movement where the test jar ina vertical position is moved towards a horizontal position toind
15、uce specimen movement.3.2.2.1 DiscussionWhen the test jar is tilted and held in ahorizontal position for 5 s without detection of specimenmovement, this is the no-flow point and the test is complete.4. Summary of Test Method4.1 After preliminary heating, the test specimen is insertedinto the automat
16、ic pour point apparatus. After starting theprogram, the specimen is cooled according to the coolingprofile listed in Table 1 and examined at either 1 C or 3 Cintervals. The lowest temperature at which movement ofspecimen is detected, by the automatic equipment, is displayedas the pour point.NOTE 2If
17、 the automatic pour apparatuss preheat option is utilized,place the test specimen into the apparatus. After starting the program, theapparatus will automatically carry out the preliminary heating.5. Significance and Use5.1 The pour point of a petroleum product is an index of thelowest temperature of
18、 its utility for certain applications. Flowcharacteristics, like pour point, can be critical for the correctoperation of lubricating oil systems, fuel systems, and pipelineoperations.5.2 Petroleum blending operations require precise measure-ment of the pour point.5.3 This test method can determine t
19、he pour point of the testspecimen with a resolution of 1.0 C.5.4 Test results from this test method can be determined ateither 1 C or 3 C intervals.5.5 This test method yields a pour point in a format similarto Test Method D97/IP15 when the 3 C interval results arereported.NOTE 3Since some users may
20、 wish to report their results in a formatsimilar to Test Method D97 (in 3 C intervals) the precisions were derivedfor the temperatures rounded to the 3 C intervals. For statements on biasrelative to Test Method D97, see 13.3.5.6 This test method has better repeatability and reproduc-ibility relative
21、 to Test Method D97/IP15 as measured in the1998 interlaboratory test program. (See Section 13.)6. Apparatus6.1 Optical Automatic Pour Point Apparatus4The auto-matic pour point apparatus described in this test methodconsists of a microprocessor controller that is capable ofcontrolling one or more ind
22、ependent test cells. The apparatusshall include provisions for independently controlling thetemperature of each cell according to the specified coolingprofile, monitoring continuously the specimen temperature,and detecting any movement of the specimen during tilting (seeFig. 1). The instrument shall
23、 be operated according to themanufacturers instructions.6.2 Temperature Probe, IEC 751 Class A: T=6(0.15 + 0.002 |T|), capable of measurement from +70 C downto 80 C. The temperature probe shall be in the center of thetest jar and the top of the platinum tip immersed 3 mm belowthe surface of the oil.
24、6.3 Test Jar, clear cylindrical glass, flat bottom, 34 mm 60.5 mm outside diameter, 1.4 mm 6 0.15 mm wall thickness,120 mm 6 0.5 mm height, thickness of the bottom 2.4 mmmaximum, marked with a line to indicate the sample height54 mm 6 0.5 mm above the inside bottom.6.4 Jacket, brass, cylindrical, fl
25、at bottom, 113 mm 60.2 mmin depth, 45 +0, 0.1 mm inside diameter. It shall be cooledaccording to the cooling profile specified.4The sole source of supply of the ISL Model CPP97-6, CPP97-2, and CPP-5Gsknown to the committee at this time is ISL SA, BP 40, 14790 Verson, France. If youare aware of alter
26、native suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.TABLE 1 Jacket and Specimen Temperature Cooling ProfileSpecimen Temperature, C Jacket Tempera
27、ture, C+27=ST+9 00.5+9=ST6 180.56=ST24 330.524=ST42 510.542=ST60 690.560=ST78 870.5FIG. 1 Optical Detection SystemD5950 1426.5 Cooling System, either an external system equipped witha circulating pump and capable of maintaining a temperature atleast 10 C below the last required jacket temperature le
28、vel(see Table 1 and Fig. 2), or an internal system capable ofmaintaining the required jacket temperatures (see Table 1 andFig. 2).6.6 Cork Disk, 6mm6 0.2 mm thick to fit loosely insidethe jacket. Felt may be used but special attention must be paidto avoid moisture in the felt disk. The felt disk mus
29、t be driedbefore each test.6.7 Cork Ring, to fit snugly around the outside of the test jarand loosely inside the test cell. Its purpose is to prevent the testjar from touching the cooling jacket.6.8 Ultrasonic Bath, Unheated(optional)with an oper-ating frequency between 25 kHz to 60 kHz and a typica
30、l poweroutput of 100 W, of suitable dimensions to hold container(s)placed inside of bath, for use in effectively dissipating andremoving air or gas bubbles that can be entrained in viscoussample types prior to analysis. It is permissible to use ultra-sonic baths with operating frequencies and power
31、outputsoutside this range, however it is the responsibility of thelaboratory to conduct a data comparison study to confirm thatresults determined with and without the use of such ultrasonicbaths does not materially impact results.7. Reagents and Materials7.1 Methyl Alcohol, Anhydrous, for use as coo
32、ling mediumin circulating bath system, when used.7.2 Cleaning Solvents, suitable for cleaning and drying thetest jar and test head, such as petroleum naphtha and hexane.(WarningFlammable. Liquid causes eye burns. Vapor harm-ful. May be fatal or cause blindness if swallowed or inhaled.)8. Sampling8.1
33、 Obtain a sample in accordance with Practice D4057 orPractice D4177.8.2 Samples of very viscous materials can 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
34、the testspecimen jar unless its temperature is 70 C or lower.NOTE 4In the event the sample has been heated above thistemperature, allow the sample to cool until its temperature is at least 70 Cbefore transferring.8.3 For some sample types, such as viscous lube oils that areprone to having entrained
35、air or gas bubbles present in thesample, the use of an ultrasonic bath (see 6.8) without theheater turned on (if so equipped), has been found effective indissipating bubbles typically within 5 min.9. Preparation of Apparatus9.1 Prepare the instrument for operation in accordance withthe manufacturers
36、 instructions.9.2 Clean and dry the test head and test jar using suitablesolvents as prescribed by the manufacturer.9.3 Adjust the set-point of the cooling system, whennecessary, to the appropriate temperature to cool the jackets tothe required temperatures (see Table 1).NOTE 5For most applications,
37、 when using an external cooling system,the recirculating cooler will be set at its lowest operating temperature.10. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions forcalibrating, checking, and operating the apparatus are fol-lowed.10.1.1 A test head simulator,
38、Part No. V02306, is used tocalibrate the equipment. The test head simulator uses precisionresistors in place of the PT 100 temperature probe to calibratethe jacket and specimen temperature electronics. Follow themanufacturers calibration instructions.10.2 A sample with a well documented pour point c
39、an 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 Pour the sample into the test specimen jar to the scribedmark. When necessary, heat the sample in a water bath or ovenuntil it
40、 is just sufficiently fluid to pour the sample into the testspecimen jar. Samples with an expected pour point above36 C or samples which appear solid at room temperature canbe heated above 45 C, but should not be heated above 70 C(see Note 4).11.2 Subject the test specimen to the following prelimina
41、rytreatment or use the instruments automatic preheat option.FIG. 2 Test Jar Cooling Chamber and Cooling SystemD5950 143NOTE 6Residual 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.11.2.1 When
42、the expected pour point (EP) is known to be33 C, heat the test specimen to 45 C in a bath or ovenmaintained at 48 C.11.2.2 When the expected pour point (EP) is known to be33 C, heat the test specimen to EP + 9 C, or at least to45 C but no higher than 70 C (see Note 4).11.3 Place a cork disk at the b
43、ottom of the jacket in therequired cell and fit a cork ring to the test jar. The cork ringshould be 25 mm 6 3 mm above the bottom of the test jar.11.4 Place the test jar in the selected test cell. Attach thedetector head according to the manufacturers instructions.11.5 Select the desired testing int
44、erval (1 C or 3 C).11.6 Enter the expected pour point (EP). If 3 C testingintervals are chosen (11.5) you must enter an expected pourpoint that is a multiple of 3 C.11.7 Start the test in accordance with the manufacturersinstructions.11.8 At this point, the instrument shall monitor the testspecimen
45、with the optical detector, adjusting the jacket tem-perature to the first temperature level (according to Table 1)and measuring the specimen temperature. The instrument shallautomatically change the jacket temperature in accordancewith the specimen temperature (according to Table 1).The timeto move
46、the jacket temperature from one level to the next lowerlevel shall not exceed 200 s, for jacket temperatures down to52 C. The instrument shall start tilting the specimen (withoutremoving it from the jacket) in the prescribed manner when thetemperature of the test specimen is at 9 C higher than theex
47、pected pour point. If the specimen flows during the tiltingmovement, the no-flow point is not reached and the jacketreturns to the waiting vertical position for the next test. The testwill continue until the jacket is in a complete horizontalposition and the detector does not detect any movement of
48、thespecimen for 5 s.This temperature, the no-flow point, plus 1 Cor 3 C (depending on the test interval selected) is the pourpoint of the oil (see Fig. 1). When the pour point is determined,the instrument shall display the pour point result and start toreheat the test specimen.NOTE 7For lower jacket
49、 temperatures, the time to move from onejacket temperature level to the next jacket temperature should not exceed300 s. Maintain cooling system temperatures as low as possible to attainthese jacket temperatures in the shortest time period possible and utilizecooling system with cooling capacity capable to achieve the lowesttemperature of application.11.9 If the instrument detects the no-flow point on the firsttilting cycle (EP + 9 C), disregard the result and start with11.1 using a
