1、Designation: D5950 12D5950 12aStandard 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 l
2、ast 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 auto
3、matic apparatus.1. Scope*1.1 This test method covers the determination of pour point of petroleum products by an automatic instrument that tilts the testjar during cooling and detects movement of the surface of the test specimen with an optical device.1.2 This test method is designed to cover the ra
4、nge of temperatures from 66 to +51C; however, the range of temperaturesincluded in the 1992 interlaboratory test program only covered the temperature range from 39 to +6C, and the range oftemperatures included in the 1998 interlaboratory test program was 51 to 11C. (See Section 13.)1.3 Test results
5、from this test method can be determined at 1 or 3C intervals.1.4 This test method is not intended for use with crude oils.NOTE 1The applicability of this test method on residual fuel samples has not been verified. For further information on applicability, refer to 13.4.1.5 The values stated in SI un
6、its are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health p
7、ractices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and P
8、etroleum ProductsD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto 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 pou
9、r point, nin petroleum products, the lowest temperature at which movement of the test specimen is observed underthe prescribed conditions of this test method.3.2 Definitions of Terms Specific to This Standard:1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products an
10、d Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow Properties.Current edition approved April 15, 2012Dec. 1, 2012. Published August 2012March 2013. Originally approved in 1996. Last previous edition approved in 20072012 asD595002(2007).D595012. DOI: 10.1520/D5950-12.10.1520/
11、D5950-12a.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.3 Available from Energy Institute, 61 New Cavendish
12、 St., London, WIG 7AR, U.K., http:/www.energyinst.org.uk.This document is not an ASTM standard and is intended 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
13、 accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current 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 H
14、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2.1 no-flow point, nin petroleum products, the temperature of the test specimen at which a wax crystal structure or viscosityincrease, or both, impedes movement of the surface of the test specimen under the conditions of the
15、 test.3.2.1.1 DiscussionThe no-flow point occurs when, upon cooling, the formation of wax crystal structures or the viscosity increase, or both, hasprogressed to the point where the applied observation device no longer detects movement under the conditions of the test. Thepreceding observation tempe
16、rature, at which flow of the test specimen is last observed, is the pour point.3.2.2 tiltingtilting, vtechnique of movement where the test jar in a vertical position is moved towards a horizontal positionto induce specimen movement.3.2.2.1 DiscussionWhen the test jar is tilted and held in a horizont
17、al position for 5 s without detection of specimen movement, this is the no-flowpoint and the test is complete.4. Summary of Test Method4.1 After preliminary heating, the test specimen is inserted into the automatic pour point apparatus. After starting the program,the specimen is cooled according to
18、the cooling profile listed in Table 1 and examined at either 1 or 3C intervals. The lowesttemperature at which movement of specimen is detected, by the automatic equipment, is displayed as the pour point.NOTE 2If the automatic pour apparatuss preheat option is utilized, place the test specimen into
19、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 the lowest temperature of its utility for certain applications. Flowcharacteristics, like pour point, can be cr
20、itical for the correct operation of lubricating oil systems, fuel systems, and pipelineoperations.5.2 Petroleum blending operations require precise measurement of the pour point.5.3 This test method can determine the pour point of the test specimen with a resolution of 1.0C.5.4 Test results from thi
21、s test method can be determined at either 1 or 3C intervals.5.5 This test method yields a pour point in a format similar to Test Method D97/IP15 when the 3C interval results are reported.TABLE 1 Jacket and Specimen Temperature Cooling ProfileSpecimen Temperature, C Jacket Temperature, C+27 = ST +9 0
22、 0.5+9 = ST 6 18 0.56 = ST 24 33 0.524 = ST 42 51 0.542 = ST 60 69 0.560 = ST 78 87 0.5D5950 12a2NOTE 3Since some users may wish to report their results in a format similar to Test Method D97 (in 3C intervals) the precisions were derived forthe temperatures rounded to the 3C intervals. For statement
23、s on bias relative to Test Method D97, see 13.3.5.6 This test method has better repeatability and reproducibility relative to Test Method D97/IP15 as measured in the 1998interlaboratory test program. (See Section 13.)6. Apparatus6.1 Optical Automatic Pour Point Apparatus4The automatic pour point app
24、aratus described in this test method consists of amicroprocessor controller that is capable of controlling one or more independent test cells. The apparatus shall include provisionsfor independently controlling the temperature of each cell according to the specified cooling profile, monitoring conti
25、nuously thespecimen temperature, and detecting any movement of the specimen during tilting (see Fig. 1). The instrument shall be operatedaccording to the manufacturers instructions.6.2 Temperature Probe, IEC 751 Class A: T =6 (0.15 + 0.002 |T|), capable of measurement from +70 down to 80C. Thetemper
26、ature probe shall be in the center of the test jar and the top of the platinum tip immersed 3 mm below the surface of theoil.6.3 Test Jar, clear cylindrical glass, flat bottom, 34 6 0.5-mm outside diameter, 1.4 6 0.15-mm wall thickness, 120 6 0.5-mmheight, thickness of the bottom 2.0 6 0.5-mm, 2.4-m
27、m maximum, marked with a line to indicate the sample height 54 6 0.5-mmabove the inside bottom.6.4 Jacket, brass, cylindrical, flat bottom, 113 60.2-mm in depth, 45 +0, 0.1-mm inside diameter. It shall be cooled accordingto the cooling profile specified.6.5 Cooling System, either an external system
28、equipped with a circulating pump and capable of maintaining a temperature atleast 10C below the last required jacket temperature level (see Table 1 and Fig. 2), or an internal system capable of maintainingthe required jacket temperatures (see Table 1 and Fig. 2).6.6 Cork Disk, 66 0.2 mm thick to fit
29、 loosely inside the jacket. Felt may be used but special attention must be paid to avoidmoisture in the felt disk. The felt disk must be dried before each test.6.7 Cork Ring, to fit snugly around the outside of the test jar and loosely inside the test cell. Its purpose is to prevent the testjar from
30、 touching the cooling jacket.7. Reagents and Materials7.1 Methyl Alcohol, Anhydrous, for use as cooling medium in circulating bath system, when used.7.2 Cleaning Solvents, suitable for cleaning and drying the test jar and test head, such as petroleum naphtha and hexane.(Warning: Flammable. Liquid ca
31、uses eye burns. Vapor harmful. May be fatal or cause blindness if swallowed or inhaled.)8. Sampling8.1 Obtain a sample in accordance with Practice D4057 or Practice D4177.4 The sole source of supply of the ISL Model CPP97-6, CPP97-2, and CPP-5Gs known to the committee at this time is ISL SA, BP 40,
32、14790 Verson, France. If you areaware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1 which you may attend.FIG. 1 Optical Detection SystemD5950 12a38.2
33、Samples of very viscous materials can be warmed until they are reasonably fluid before they are transferred; however, nosample shall be heated more than is absolutely necessary. The sample shall not be heated and transferred into the test specimenjar unless its temperature is 70C or lower.NOTE 4In t
34、he event the sample has been heated above this temperature, allow the sample to cool until its temperature is at least 70C beforetransferring.9. Preparation of Apparatus9.1 Prepare the instrument for operation in accordance with the manufacturers instructions.9.2 Clean and dry the test head and test
35、 jar using suitable solvents as prescribed by the manufacturer.9.3 Adjust the set-point of the cooling system, when necessary, to the appropriate temperature to cool the jackets to the requiredtemperatures (see Table 1).NOTE 5For most applications, when using an external cooling system, the recircul
36、ating cooler will be set at its lowest operating temperature.10. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions for calibrating, checking, and operating the apparatus are followed.10.1.1 A test head simulator, Part No. V02306, is used to calibrate the equipment
37、. The test head simulator uses precisionresistors in place of the PT 100 temperature probe to calibrate the jacket and specimen temperature electronics. Follow themanufacturers calibration instructions.10.2 A sample with a well documented pour point can be used to verify performance of the apparatus
38、. Alternatively, a samplewhich has been extensively tested in a pour point interlaboratory study can be used.11. Procedure11.1 Pour the sample into the test specimen jar to the scribed mark. When necessary, heat the sample in a water bath or ovenuntil it is just sufficiently fluid to pour the sample
39、 into the test specimen jar. Samples with an expected pour point above 36C orsamples which appear solid at room temperature can be heated above 45C, but should not be heated above 70C (see Note 4).11.2 Subject the test specimen to the following preliminary treatment or use the instruments automatic
40、preheat option.NOTE 6Residual fuels have been known to be sensitive to thermal history. In the case where a residual fuel sample is tested, refer to Test MethodD97 for sample treatment.11.2.1 When the expected pour point (EP) is known to be 33C, heat the test specimen to 45C in a bath or oven mainta
41、inedat 48C.11.2.2 When the expected pour point (EP) is known to be 33C, heat the test specimen to EP + 9C, or at least to 45C butno higher than 70C (see Note 4).11.3 Place a cork disk at the bottom of the jacket in the required cell and fit a cork ring to the test jar. The cork ring shouldbe 25 6 3
42、mm above the bottom of the test jar.11.4 Place the test jar in the selected test cell. Attach the detector head according to the manufacturers instructions.11.5 Select the desired testing interval (1 or 3C).11.6 Enter the expected pour point (EP). If 3C testing intervals are chosen (11.5) you must e
43、nter an expected pour point thatis a multiple of 3C.11.7 Start the test in accordance with the manufacturers instructions.FIG. 2 Test Jar Cooling Chamber and Cooling SystemD5950 12a411.8 At this point, the instrument shall monitor the test specimen with the optical detector, adjusting the jacket tem
44、perature tothe first temperature level (according to Table 1) and measuring the specimen temperature. The instrument shall automaticallychange the jacket temperature in accordance with the specimen temperature (according to Table 1). The time to move the jackettemperature from one level to the next
45、lower level shall not exceed 200 s, for jacket temperatures down to 52C. The instrumentshall start tilting the specimen (without removing it from the jacket) in the prescribed manner when the temperature of the testspecimen is at 9C higher than the expected pour point. If the specimen flows during t
46、he tilting movement, the no-flow point isnot reached and the jacket returns to the waiting vertical position for the next test. The test will continue until the jacket is in acomplete horizontal position and the detector does not detect any movement of the specimen for 5 s. This temperature, the no-
47、flowpoint, plus 1 or 3C (depending on the test interval selected) is the pour point of the oil (see Fig. 1). When the pour point isdetermined, the instrument shall display the pour point result and start to reheat the test specimen.NOTE 7For lower jacket temperatures, the time to move from one jacke
48、t temperature level to the next jacket temperature should not exceed 300 s.Maintain cooling system temperatures as low as possible to attain these jacket temperatures in the shortest time period possible and utilize cooling systemwith cooling capacity capable to achieve the lowest temperature of app
49、lication.11.9 If the instrument detects the no-flow point on the first tilting cycle (EP + 9C), disregard the result and start with 11.1 usinga higher expected pour point.11.10 Record the result as the pour point without any correction.NOTE 8Residual fuels have been known to be sensitive to thermal history. In the case where a residual fuel sample is tested, refer to Test MethodD97 for sample treatment.12. Report12.1 Report the temperature recorded in 11.10 together with the model an
