1、Designation: D5773 171Designation: IP 446/09Standard Test Method forCloud Point of Petroleum Products and Liquid Fuels(Constant Cooling Rate Method)1This standard is issued under the fixed designation D5773; the number immediately following the designation indicates the year oforiginal adoption or,
2、in the case 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.1NOTESubsection 13.1.3 was revised editorially in September 2017.INTRODUCTIONThis test method
3、 describes an alternative procedure for the determination of cloud point ofpetroleum products Test Method D2500/IP 219 using an automatic apparatus. The temperature resultsfrom this test method have been found to be equivalent to Test Method D2500/IP 219. Whenspecification requires Test Method D2500
4、/IP 219, do not substitute this test method or any othermethod without obtaining comparative data and agreement from the specifier.1. Scope*1.1 This test method covers the determination of the cloudpoint of petroleum products and biodiesel fuels that aretransparent in layers 40 mm in thickness by an
5、 automaticinstrument using a constant cooling rate.1.2 This test method covers the range of temperatures from60 C to +49 C with temperature resolution of 0.1 C,however, the range of temperatures included in the 1997interlaboratory cooperative test program only covered thetemperature range of 56 C to
6、 +34 C.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 theresponsibility of the user of this standard to establi
7、sh appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment
8、 of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D2500 Test Method for Cloud Point of Petroleum Productsand Liquid FuelsD4057 Practice for Manual Sampling of Petroleum
9、 andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products2.2 Energy Institute Standard:3IP 219 Test Method for Cloud Point of Petroleum ProductsIP 446 Determination of the Cloud Point of PetroleumProductsAutomatic Constant Cooling Rate Method3. Terminology3.1 Def
10、initions:3.1.1 biodiesel, na fuel comprised of 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 alcohol such asmethanol or ethanol in the presenc
11、e 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).1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubric
12、ants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved May 1, 2017. Published May 2017. Originallyapproved in 1995. Last previous edition approved in 2015 as D5773 15a. DOI:10.1520/D5773-17E01.2For referenced ASTM standards, visit the ASTM website, ww
13、w.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 Summary of
14、 Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in th
15、e Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13.1.2 biodiesel blend, na blend of biodiesel fuel withpetroleum-based diesel fuel designated BXX, where XX is thevolu
16、me percentage of biodiesel.3.1.3 cloud point, nin petroleum products and biodieselfuels, the temperature of a liquid specimen when the smallestobservable cluster of wax crystals first occurs upon coolingunder prescribed conditions.3.1.3.1 DiscussionThe cloud point occurs when the tem-perature of the
17、 specimen is low enough to cause wax crystalsto precipitate. In a homogeneous liquid, the cloud is alwaysnoted first at the location in the specimen where the specimentemperature is the lowest. The cloud point is the temperature atwhich the crystals first occur, regardless of their location in thesp
18、ecimen, and not after extensive crystallization has takenplace. The wax crystals that precipitate at lower temperaturesare typically, but not excluded to, straight-chain hydrocarbonsand lipids.3.1.3.2 DiscussionThe purpose of the cloud point is tomeasure the wax crystals in the specimen; however, tr
19、aceamounts of water and inorganic compounds may also bepresent.The intent of the cloud point measurement is to capturethe temperature at which the liquid fuel in the specimen beginsto change from a single liquid phase to a two-phase systemcontaining solid and liquid. It is not the intent of this tes
20、tmethod to monitor the phase transition of the trace componentssuch as water.3.2 Definitions of Terms Specific to This Standard:3.2.1 automatic cloud point, nthe temperature of aspecimen, when the appearance of the cloud is determinedunder the conditions of this test method.3.2.1.1 DiscussionThe clo
21、ud point in this test method isdetermined by an automatic instrument using an optical devicefor detection of the crystal formation. The apparatus and theconditions are different from those established for Test MethodD2500, although according to interlaboratory examination, theresults have been deter
22、mined to be equivalent to Test MethodD2500.3.2.2 constant cooling rate method, nin cloud point testmethods, test procedure using prescribed cooling rate, speci-men receptacle, and optical system for detection of crystalformation.3.2.2.1 DiscussionThe prescribed cooling rate is de-scribed in 4.1, the
23、 specimen receptacle is described in AnnexA1, and the optical system for the detection of crystal forma-tion is described in Annex A1.3.2.3 Peltier device, na solid-state thermoelectric deviceconstructed with dissimilar semiconductor materials and con-figured in such a way that it will transfer heat
24、 to or away froma test specimen dependent on the direction of electric currentapplied to the device.3.2.4 D2500/IP 219 equivalent cloud point, nthe tempera-ture of a specimen, in integers, calculated by rounding theresults of this test method to the next lower integer.3.2.4.1 DiscussionThis test met
25、hod produces results with0.1 C resolution. Should the user wish to provide results witha similar format to Test Method D2500, then this calculationcan be performed. Some apparatus can perform this calculationautomatically.4. Summary of Test Method4.1 A prescribed specimen (11.5) is cooled by a Pelti
26、erdevice (A1.1) at a constant rate of 1.5 Cmin 6 0.1 Cminwhile continuously being illuminated by a light source(A1.1.4). The specimen is continuously monitored by an arrayof optical detectors (A1.1.5, Fig. A1.1) for the first appearanceof a cloud of wax crystals. The detectors are sufficient innumbe
27、r to ensure that any solid-phase hydrocarbon crystalsthat may form are detected. The temperature at which theappearance of a cloud of wax crystals is first detected in thespecimen is recorded to 0.1 C resolution. When the recordedtemperature is rounded to the next lower integer temperature, itis des
28、ignated as the D2500/IP 219 equivalent cloud point perTest Method D5773.5. 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 sufficient quantity canplug filters used in some
29、 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 resolution of 0.1 C.5.4 This test method provides re
30、sults that are equivalent toTest Method D2500.NOTE 1This is based on the Test Method D2500 equivalent cloudpoint in which the 0.1 C result is rounded to the next lower integer.5.5 This test method determines the cloud point in a shorterperiod of time than Test Method D2500.NOTE 2In cases of samples
31、with cloud points near ambienttemperatures, time savings may not be realized.5.6 This test method eliminates most of the operator timerequired of Test Method D2500.5.7 This test method does not require the use of a mechani-cal refrigeration apparatus.NOTE 3In certain cases of high ambient temperatur
32、e, a source ofcooling water may be required to measure low-temperature cloud points(see 7.1).D5773 17126. Apparatus6.1 Automatic Apparatus4The automatic cloud point ap-paratus described in this test method consists of a test chambercontrolled by a microprocessor that is capable of controllingthe hea
33、ting and cooling of the test specimen, optically observ-ing the first appearance of a cloud of wax crystals andrecording the temperature of the specimen described in detailin Annex A1.6.2 The apparatus shall be equipped with a specimen cup,optical detector array, light source, digital display, Pelti
34、erdevice, and a specimen temperature measuring device.6.3 The Peltier device shall be capable of heating or coolingthe test specimen at a constant rate of 1.5 Cmin 60.1 Cmin.6.4 The temperature-measuring device in the specimen cupshall be capable of measuring the temperature of the testspecimen from
35、 40 C to +70 C at a resolution of 0.1 C.6.5 The apparatus shall be equipped with fittings to permitthe circulation of a liquid cooling medium, if required, toremove heat generated by the Peltier device and other elec-tronic components of the apparatus.NOTE 4Some apparatus are designed to use ambient
36、 air as a coolingmedium. In such cases, a built-in fan is available to provide circulation ofair and there is no need for fittings as described for a liquid coolingmedium. The function of the cooling medium is to remove heat from theelectronic components. The choice of the cooling medium has no impa
37、ctwhatsoever on the test results.6.6 The apparatus shall be equipped with fittings to permitthe circulation of purge gas to purge the test chamber contain-ing the specimen cup of any atmospheric moisture.7. Reagents and Materials7.1 Cooling MediumAir, tap water, or other liquid heatexchange medium s
38、ufficient to remove heat generated by thePeltier device and other electronic components from theapparatus. To achieve specimen cooling to 40 C, supplycirculation of liquid cooling medium at +25 C or lower to theapparatus. For an apparatus which relies on air as coolingmedium, the ambient air tempera
39、ture has to be below +30 C toachieve specimen cooling to 40 C.7.2 Purge GasA gas such as air, nitrogen, helium, orargon with a dew point below the lowest operating temperatureof the analyzer. (WarningCompressed gas under high pres-sure.) (WarningInert gas can be an asphyxiant when in-haled.)7.3 Prec
40、ision Volume Dispensing Device, capable of dis-pensing 0.15 mL 6 0.01 mL of sample.7.4 Cotton SwabsPlastic or paper shaft cotton swabs usedto clean the sample cup. (WarningThe use of swabs withwooden shafts may damage the mirrored surface of thespecimen cup.)8. Sampling8.1 Obtain a sample in accorda
41、nce with Practice D4057 orD4177.8.2 Samples of very viscous materials may be warmed untilthey are reasonably fluid before they are tested. However, nosample should be heated more than absolutely necessary.8.3 The sample shall not be heated above 70 C. When thesample is heated above 70 C, allow the s
42、ample to cool below70 C before filtering 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 oil is perfectly clear, but make suchfiltration at a temperature at least 14 C above the
43、 expectedcloud point.NOTE 5Moisture 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 man
44、ufacturers instructions.9.2 Make liquid cooling medium connections if required(see Note 4) and ensure that they do not leak.9.3 Make purge gas connections and ensure that they do notleak.9.4 Turn on the liquid cooling medium if required (see Note4).9.5 Turn on the purge gas.9.6 Turn on the main powe
45、r switch of the analyzer.After theautomatic self diagnostics startup sequence is completed, theinstrument will display a READY message.10. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions forcalibrating, checking, and operating the apparatus are fol-lowed.10.2 A
46、sample with a mutually agreed upon cloud point canbe used to verify performance of the apparatus.11. Procedure11.1 Inspect the specimen cup to ensure it is clean and dry.If not, clean the cup (see 11.3).11.2 Deliver 0.15 mL 6 0.01 mL of specimen into thespecimen cup. Pipette, syringe, or precision p
47、ositive-displacement devices are suitable for use in delivering thespecimen.11.3 Clean the specimen out of the cup. The cup must becleaned to the point where no visible droplets of specimenremain in the cup. Non-abrasive absorbent materials such as4The sole source of supply of the PhaseTechnology Cl
48、oud PointAnalyzer modelseries 10, 30, 70, 70V, and 70X known to the committee at this time is PhaseTechnology, 11168 Hammersmith Gate, Richmond, B.C. Canada V7A 5H8. Thevarious model series mentioned above are differentiated by their cooling capacitiesand user interfaces; however, all of them are ca
49、pable of covering the entiretemperature range specified in the scope. If you are aware of alternative suppliers,please provide this information to ASTM International Headquarters. Your com-ments will receive careful consideration at a meeting of the responsible technicalcommittee,1which you may attend.D5773 1713cotton swabs are suitable for use in cleaning the specimen cup.Cleaning solvents able to clean the specimen and compatiblewith the components of the apparatus can also be used.Naphtha, hexane, heptane, and t
