ASTM D7397-2008 459 Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method).pdf

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1、Designation: D 7397 08An American National StandardStandard Test Method forCloud Point of Petroleum Products (Miniaturized OpticalMethod)1This standard is issued under the fixed designation D 7397; the number immediately following the designation indicates the year oforiginal adoption or, in the cas

2、e of revision, the year 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.1. Scope*1.1 This test method covers the determination of the cloudpoint of petroleum products and biod

3、iesel fuels that aretransparent in layers 40 mm in thickness by an automaticinstrument.1.2 This test method covers the range of temperatures from60 to +20C with temperature resolution of 0.1C; however,the range of temperatures included in the 2006 interlaboratorycooperative test program only covered

4、 the temperature range of35 to +12C. See Section 13.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsib

5、ility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 2500 Test Method for Cloud Point of Petroleum ProductsD 4057 Practice for Manual Sampling of P

6、etroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 5773 Test Method for Cloud Point of Petroleum Products(Constant Cooling Rate Method)2.2 Energy Institute Standards:3IP 219 Test Method for Cloud Point of Petroleum ProductsIP 446 Test Method for

7、Cloud Point of Petroleum Products3. Terminology3.1 Definitions:3.1.1 biodiesel, nfuel comprising mono-alkyl esters oflong-chain fatty acids derived from vegetable oils or animalfats, designated B100.3.1.1.1 DiscussionBiodiesel is typically produced by areaction of vegetable oil or animal fat with an

8、 alcohol such asmethanol or ethanol in the presence of a catalyst to yieldmono-esters and glycerin. The fuel typically may contain up to14 different types of fatty acids that are chemically transformedinto fatty acid methyl esters (FAME).3.1.2 biodiesel blend (BXX), nblend of biodiesel fuel withpetr

9、oleum-based diesel fuel designated BXX, where XX is thevolume percentage (as a whole number without the percentagesign) of biodiesel.3.1.3 cloud point, nin petroleum products and biodieselfuels, the temperature of a liquid specimen when the smallestobservable cluster of hydrocarbon crystals first oc

10、curs uponcooling under prescribed conditions.3.1.3.1 DiscussionThe cloud point occurs when the tem-perature of the specimen is low enough to cause hydrocarboncrystals to precipitate. In a homogeneous liquid, the cloud isalways noted first at the location in the specimen where thespecimen temperature

11、 is the lowest. The cloud point is thetemperature at which the crystals first occur, regardless of theirlocation in the specimen, and not after extensive crystallizationhas taken place. The hydrocarbon crystals that precipitate atlower temperatures are typically, but not excluded to, straightchain h

12、ydrocarbons commonly called “wax crystals.”3.2 Definitions of Terms Specific to This Standard:1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.07.0D on Wax-Related Viscometric Properties of Fuels

13、 and Oils.Current edition approved Oct. 15, 2008. Published November 2008. Originallyapproved in 2007. Last previous edition approved in 2007 as D 739707.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS

14、tandards 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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100

15、Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2.1 automatic cloud point, ntemperature of a specimen,when the appearance of the cloud is determined under theconditions of this test method.3.2.1.1 DiscussionThe cloud point in this test method isdetermined by an auto

16、matic instrument using a miniaturizedtest receptacle equipped with two optical fibers, one to bringlight into the test receptacle and the other to receive lightscattered from the specimen.3.2.2 D 2500/IP 219 equivalent cloud point, ntemperatureof a specimen, in integers, calculated by applying a bia

17、s androunding the result to the next lower integer (see 12.2).3.2.2.1 DiscussionThis test method produces results with0.1C resolution. Should the user wish to provide results witha similar format to Test Method D 2500, then this calculationcan be performed (see 12.2). Some apparatus can perform this

18、calculation automatically.3.2.3 Peltier device, nsolid state thermoelectric deviceconstructed with dissimilar semiconductor materials and con-figured in such a way that it will transfer heat to or away froma test specimen dependent on the direction of electric currentapplied to the device.44. Summar

19、y of Test Method4.1 A specimen is cooled by a Peltier device at a rate of 306 5C/min, while continuously being illuminated by a lightsource. The specimen is continuously monitored by an opticaldetector for the first appearance of a cloud of wax crystals.Once crystals are first detected, as manifeste

20、d by an increase inlight level received by the optical detector, the specimen iswarmed at a rate of 15 6 5C/min. As soon as all the crystalshave re-dissolved into the liquid specimen, warming is haltedand the specimen is cooled again; but this time at a slower rateof 6 6 3C/min. When crystals first

21、appear under this slowercooling rate, the temperature of the specimen is recorded to0.1C resolution as cloud point.5. Significance and Use5.1 The cloud point of petroleum products and biodieselfuels is an index of the lowest temperature of their utility forcertain applications. Wax crystals of suffi

22、cient quantity canplug filters used in some fuel systems.5.2 Petroleum blending operations require a precise mea-surement of the cloud point.5.3 This test method can determine the temperature of thetest specimen at which wax crystals have formed sufficiently tobe observed as a cloud with a resolutio

23、n of 0.1C.5.4 This test method provides results that are equivalent toTest Method D 5773/IP 446. The temperature results of thistest method have been found to be warmer than those of TestMethod D 2500/IP 219 by an average of 0.49C; however, nosample specific bias was observed.5.5 Similar to Test Met

24、hod D 5773/IP 446, this test methoddetermines cloud point in a shorter period of time than TestMethod D 2500/IP 219.NOTE 1In cases of samples with cloud points near ambient tempera-tures, time savings may not be realized.NOTE 2This test method eliminates most of the operator timerequired of Test Met

25、hod D 2500/IP 219.NOTE 3The only utility required by the apparatus described in thistest method is electricity with power consumption of approximately 20watts. The electric power can come from an alternating current source(wall receptacle) or direct current source such as a battery or a cigarettelig

26、hter plug in a vehicle.NOTE 4The apparatus described by this test method can be mademuch smaller and lighter than that of Test Methods D 5773/IP 446 andD 2500/IP 219, allowing full portability.NOTE 5The apparatus used in the 2006 interlaboratory study weighedapproximately 1 kg and occupied the space

27、 of a small lunch box. SeeSection 13.6. Apparatus6.1 Automatic Apparatus4,5The automatic cloud pointapparatus described in this test method consists of a testchamber controlled by a microprocessor that is capable ofcontrolling the heating and cooling of the test specimen,optically observing the firs

28、t appearance of a cloud of waxcrystals and recording the temperature of the specimen de-scribed in detail in Annex A1.6.2 The apparatus shall be equipped with a specimenreceptacle, optical detector, light source, optical fibers, digitaldisplay, Peltier device, and a specimen temperature measuringdev

29、ice.6.3 The Peltier device shall be capable of heating or coolingthe test specimen at a rate of 3 to 35C/min.6.4 The temperature measuring device in the specimenreceptacle shall be capable of measuring the temperature of thetest specimen from 60 to +20C at a resolution of 0.1C.4NOTE 6The apparatus d

30、escribed above is covered by patents. If youare aware of an alternative(s) to the patented items, please attach to yourballot return a description of the alternative(s). All suggestions will beconsidered by the committee.7. Reagents and Materials7.1 Disposable syringe that is capable of dispensing a

31、t least10 6 0.5 mL per full discharge of sample into the specimenreceptacle.NOTE 7The apparatus can also be connected to a sample supply lineto receive new sample. The amount of sample required per analysis is thesame as that for the syringe injection procedure (that is, 20 6 1.0 mL peranalysis). In

32、 such cases, a disposable syringe would not be needed.8. Sampling8.1 Obtain a sample in accordance with Practices D 4057 orD 4177.8.2 Samples of very viscous materials may be warmed untilthey are reasonably fluid before they are tested. However, nosample should be heated more than absolutely necessa

33、ry.4The Peltier device is covered by a patent. Interested parties are invited to submitinformation regarding the identification of an alternative(s) to this patented item tothe ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technica

34、l committee.5The sole source of supply of the apparatus known to the committee at this timeis Phase Technology Miniature Cloud Point Analyzer available from PhaseTechnology, 11168 Hammersmith Gate, Richmond, B.C., Canada V7A-5H8. If youare aware of alternative suppliers, please provide this informat

35、ion to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.D73970828.3 The sample shall not be heated above 70C. When thesample is heated above 70 C, allow the sample to cool below70C before filteri

36、ng or inserting into the apparatus.8.4 When moisture is present in the sample, remove themoisture by a method, such as filtration through dry lint-freefilter paper, until the specimen is perfectly clear, but make suchfiltration at a temperature at least 14C above the expectedcloud point.NOTE 8Moistu

37、re will be noticed in the sample as a separate phase oras a haze throughout the entire sample. Generally, a slight haze will notinterfere with the detection of the wax cloud.9. Preparation of Apparatus9.1 Prepare the instrument for operation in accordance withthe manufacturers instructions.9.2 Turn

38、on the main power switch of the analyzer.10. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions forcalibrating, checking, and operating the apparatus are fol-lowed.10.2 A sample with a mutually agreed upon cloud point canbe used to verify performance of the apparat

39、us.11. Procedure11.1 Draw 10 6 0.5 mL of bubble-free sample into a newdisposable syringe. Connect the syringe to the inlet port, andinject the full charge of sample into the test receptacle. Thespecimen excess will flow into a waste-receiving container.11.2 Draw another 10 6 0.5 mL of bubble-free sa

40、mple intothe syringe. Connect the syringe to the inlet port, and inject thefull charge of sample into the test receptacle. The specimenexcess will flow into a waste-receiving container. The totalamount of sample (that is, 20 6 1.0 mL) is sufficient inquantity to flush out any previous sample in the

41、specimenreceptacle and fill it with the fresh sample.NOTE 9Follow manufacturers instructions for sample injection if thespecimen receptacle is connected to a sample supply line as described inNote 7.11.3 Start the operation of the apparatus according to themanufacturers instructions. From this point

42、 on, the apparatusautomatically controls the procedure.11.4 Cool the sample at a rate of 30 6 5C/min, whilecontinuously illuminating the sample with the light source.Monitor the specimen continuously with the optical detector.Once crystals are first detected, as manifested by an increase inlight lev

43、el received by the optical detector, warm the specimenat a rate of 15 6 5C/min. As soon as all the crystals havere-dissolved into the liquid specimen in accordance with thistest method, stop the warming and cool the specimen again ata slower rate of 6 6 3C/min. When crystals first appear underthis s

44、lower cooling rate, record the temperature of the speci-men as the cloud point.11.5 The measurement is automatically terminated once thecloud point is detected.11.6 When the measurement is complete, the cloud pointvalue per Test Method D 7397 will be displayed by theapparatus.12. Calculation or Inte

45、rpretation of Results12.1 Report the temperature recorded in 11.6 as the auto-matic cloud point Test Method D 7397.12.2 When specified, correct the temperature recorded in11.6 with the relative bias in accordance with 13.3, round theresult to the next lower integer (a colder temperature), andreport

46、as the Test Method D 2500/IP 219 equivalent cloudpoint per Test Method D 7397.13. Precision and Bias613.1 PrecisionThe precision of this test method as deter-mined by the statistical examination of the interlaboratory testresults is as follows:13.1.1 RepeatabilityThe difference between successivetes

47、t 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:0.26E201 3 31.0 X!Cwhere X = cloud point in C only in one case in twenty. SeeTable 1.1

48、3.1.2 ReproducibilityThe difference between two singleand independent test results, obtained by different operatorsworking in different laboratories on identical test material,would in the long run, in normal and correct operation of thistest method, exceed:0.34E201 3 31.0 X!C6Supporting data (the r

49、esults of the 2006 Interlaboratory Cooperative TestProgram) have been filed at ASTM International Headquarters and may be obtainedby requesting Research Report RR: D02-1627.TABLE 1 Typical Repeatability at Different Cloud PointsCloud Point C Repeatability C15 0.410 0.550.7008-5 0.9-10 1.1-15 1.2-20 1.3-25 1.5-30 1.6-35 1.7TABLE 2 Typical Reproducibility at Different Cloud PointsCloud Point C Reproducibility C15 0.510 0.750.9011-5 1.2-10 1.4-15 1.6-20 1.7-25 1.9-30 2.1-35 2.2D7397083where X = cloud point in C) only in on