1、Designation: D5772 15D5772 17Designation: IP 445/09Standard Test Method forCloud Point of Petroleum Products and Liquid Fuels (LinearCooling Rate Method)1This standard is issued under the fixed designation D5772; the number immediately following the designation indicates the year oforiginal adoption
2、 or, 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.INTRODUCTIONThis test method describes an alternative procedure for the determination of
3、 cloud point ofpetroleum products of Test Method D2500/IP 219 using an automatic apparatus. The temperatureresults from this test method have been found to be equivalent to Test Method D2500/IP 219. Whenspecification requires Test Method D2500/IP 219, do not substitute this test method or any otherm
4、ethod without obtaining comparative data and agreement from the specifier.1. Scope*1.1 This test method covers the description of the determination of the cloud point of petroleum products and biodiesel fuelsthat are transparent in layers 40 mm in thickness by an automatic instrument using a linear
5、cooling rate.1.2 This test method covers the range of temperatures from 60 C to 49 C with temperature resolution of 0.1 C, however,the range of temperatures included in the 1997 interlaboratory cooperative test program only covered the temperature range of56 C to +34 C.1.3 The values stated in SI un
6、its are to be regarded as standard. No other units of measurement are included in this standard.1.4 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.1.5 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and
8、 Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D2500 Test Method for Cloud Point of Petroleum Products and Liquid FuelsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice f
9、or Automatic Sampling of Petroleum and Petroleum Products2.2 Energy Institute Standard:IP 219 Test Method for Cloud Point of Petroleum Products33. Terminology3.1 Definitions:1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is t
10、he direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved April 1, 2015May 1, 2017. Published April 2015May 2017. Originally approved in 1995. Last previous edition approved in 20102015 asD5772 10.D5772 15. DOI: 10.1520/D5772-15.10.1520/D5772-17.2 For referencedASTM
11、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 St., London, WIG 7AR, U.K., ht
12、tp:/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 accurately, ASTM recommends th
13、at 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 Harbor Drive, PO Box C700, West
14、Conshohocken, PA 19428-2959. United States13.1.1 biodiesel, na fuel comprised of mono-alkyl esters of long-chain fatty acids derived from vegetable oils or animal fats,designated B100.3.1.1.1 DiscussionBiodiesel is typically produced by a reaction of vegetable oil or animal fat with an alcohol such
15、as methanol or ethanol in thepresence of a catalyst to yield-mono-esters yield mono-esters and glycerin. The fuel typically may contain up to 14 different typesof fatty acids that are chemically transformed into fatty acid methyl esters (FAME).3.1.2 biodiesel blend, na blend of biodiesel fuel with p
16、etroleum-based diesel fuel designated BXX, where XX is the volumepercentage of biodiesel.3.1.3 cloud point, nin petroleum products and biodiesel fuels, the temperature of a liquid specimen when the smallestobservable cluster of hydrocarbonwax crystals first occurs upon cooling under prescribed condi
17、tions.3.1.3.1 DiscussionThe cloud point occurs when the temperature of the specimen is low enough to cause hydrocarbonwax crystals to precipitate. Ina homogeneous liquid, the cloud is always noted first at the location in the specimen where the specimen temperature is the lowest.The cloud point is t
18、he temperature at which the crystals first occur, regardless of their location in the specimen, and not afterextensive crystallization has taken place. The hydrocarbonwax crystals that precipitate at lower temperatures are typically, but notexcluded to, straight chain hydrocarbons commonly called “w
19、ax crystals.”straight-chain hydrocarbons and lipids.3.1.3.2 DiscussionThe purpose of the cloud point method is to detect the presence of the wax crystals in the specimen; however, trace amounts ofwater and inorganic compounds may also be present. The intent of the cloud point method is to capture th
20、e temperature at whichthe liquid fuel in the specimen begins to change from a single liquid phase to a two-phase system containing solid and liquid. Itis not the intent of this test method to monitor the phase transition of the trace components, such as water.3.2 Definitions of Terms Specific to Thi
21、s Standard:3.2.1 automatic cloud point, nthe temperature 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 is determined by an automatic instrument using an optical device for detection of the cr
22、ystalformation. The apparatus and the conditions are different from those established for Test Method D2500, although, according tointerlaboratory examination, the results have been determined to be equivalent to Test Method D2500.3.2.2 linear cooling rate method, nin cloud point test methods, test
23、procedure using prescribed cooling rate, specimenreceptacle, and optical system for detection of crystal formation.3.2.2.1 DiscussionThe prescribed cooling rate is described in 11.6; the specimen receptacle is described in Annex A1, and the optical system for thedetection of crystal formation is des
24、cribed in Annex A1.3.2.3 D2500/IP 219 equivalent cloud point, nthe temperature of a specimen, in integers, calculated by rounding the resultsof this test method to the next lower integer.3.2.3.1 DiscussionThis test method produces results with 0.1 C resolution. Should the user wish to provide result
25、s with a similar format to TestMethod D2500, then this calculation can be performed. Some apparatus can perform this calculation automatically.D5772 1724. Summary of Test Method4.1 After insertion of the specimen into the apparatus and initiation of the program, the prescribed specimen test cell (An
26、nexA1) is heated and then linearly cooled at a specified rate (11.6). The specimen is continuously monitored by an opposing opticallight barrier (Annex A1 and Fig. A1.3) for the crystal structure formation. The temperature, when the crystallization of the waxin the specimen is detected by the optica
27、l barrier, is recorded with a resolution of 0.1 C.The specimen is then heated to the originalstarting temperature.5. Significance and Use5.1 For petroleum products and diesel fuels, the cloud point is an index of the lowest temperature of its utility for certainapplications. Wax crystals of sufficie
28、nt quantity can plug filters used in some fuel systems.5.2 Petroleum blending operations require precise measurement of the cloud point.5.3 This test method can determine the temperature of the test specimen at which wax crystals have formed sufficiently to beobserved as a cloud, with a resolution o
29、f 0.1 C.5.4 This test method provides results that when rounded to the next lower integer are equivalent to Test Method D2500.5.5 This test method is more precise than Test Method D2500.6. Apparatus6.1 Automatic Apparatus4The automatic cloud point apparatus described in AnnexA1 consists of a micropr
30、ocessor-controlledmeasuring unit that is capable of heating, cooling, optically observing the appearance of the automatic cloud point, and recordingthe temperature of the specimen. The apparatus shall be equipped with a digital display, cooling/heating block assembly, opticallight barrier assembly,
31、and a test cell of the approximate dimensions listed in Annex A1, and contain a temperature measuringdevice.6.2 Beaker, glass or plastic (disposable) (50 mL), for containing the sample prior to introduction into the test cell.6.3 Circulating Bath, a refrigeration unit equipped with a circulating pum
32、p capable of maintaining a temperature at least 20 Clower than the lowest expected cloud point to be measured.7. Reagents and Materials7.1 Cleaning Solvents, suitable for cleaning and drying the test cell, such as petroleum naphtha and acetone. (WarningFlammable. Liquid causes eye burns. Vapor is ha
33、rmful. May be fatal or cause blindness if swallowed or inhaled.)7.2 Methyl Alcohol, anhydrous, for use as cooling medium in circulating bath.7.3 Lint-free filter paper may be used as a drying medium.8. Sampling8.1 Obtain a sample in accordance with PracticesPractice D4057 or D4177.8.2 Samples of ver
34、y viscous materials may be warmed until they are reasonably fluid before they are sampled. However, nosample should be heated more than absolutely necessary.8.3 The sample shall not be heated above 70 C. When the sample is heated above 70 C, allow the sample to cool below 70 Cbefore filtering or ins
35、erting into the apparatus.8.4 When moisture is present in the sample, remove the moisture by a method such as filtration through dry, lint-free filter paperuntil the oil is perfectly clear. Make such filtration at a temperature at least 14 C above the expected cloud point.NOTE 1Moisture will be noti
36、ced in the sample as a separate phase or as a haze throughout the entire sample. Generally, a slight haze will not interferewith the detection of the wax cloud.9. Preparation of Apparatus9.1 Prepare the instrument for operation in accordance with the manufacturers instructions.9.2 Clean and dry the
37、test cell using suitable solvents as prescribed by the manufacturer.9.3 Prepare the refrigerated circulating bath for operation in accordance with the manufacturers instructions and allow it toattain a temperature at least 20 C lower than the expected cloud point of the sample.4 The sole source of s
38、upply of the Herzog Model SC 815 and SC 819 known to the committee at this time is Walter Herzog, Lauda, Germany. If you are aware of alternativesuppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the respons
39、ible technicalcommittee,1 which you may attend.D5772 17310. Calibration and Standardization10.1 Ensure that all of the manufacturers instructions for calibrating, checking, and operating the apparatus are followed.10.2 A sample with a mutually agreed upon cloud point can be used to verify performanc
40、e of the apparatus.11. Procedure11.1 Pour at least 20 mL of the sample into the beaker. When necessary, heat the sample in a water bath or oven until it is justsufficiently fluid to pour into the beaker.11.2 Place the beaker under the entrance of the test cell and start the test in accordance with t
41、he manufacturers instructions.11.3 When the expected cloud point is known to be above 25 C, preselect a starting temperature which is at least 14 C abovethe expected cloud point. The highest starting temperature that can be programmed is 70 C.11.4 When the expected cloud point is known to be at or b
42、elow 25 C, the test duration can be shortened by preselecting astarting temperature which is at least 14 C above the expected cloud point. The lowest starting temperature that can beprogrammed is 20 C.11.5 When the expected cloud point is not known, preselect a starting temperature of 40 C. The appa
43、ratus automatically heatsthe test specimen to approximately 40 C when a starting temperature is not selected. When the expected cloud point is not knownand the sample needs to be heated before transferring into the test specimen beaker, preselect a starting temperature of 70 C.11.6 A portion of the
44、sample is drawn into the test cell. Initially, the specimen is heated to 40 C or to a starting temperaturepreselected by the operator between 20 C and 70 C. The flow of the cooling fluid from the circulating bath is then regulated tomaintain the rate of cooling of the specimen at 1 C 6 0.2 C per min
45、 (see Note 2). The specimen is continuously monitored bythe optical light barrier and the specimen temperature is continuously displayed.At the detection of the automatic cloud point, thetemperature the specimen attained, to within 0.1 C resolution, is held on the digital display until cleared by th
46、e operator. Thespecimen is then heated to 40 C or to the preselected starting temperature.NOTE 2Although the apparatus is capable of faster cooling rates of 2 C or 3 C min, the interlaboratory program does not address the equivalencyand precision of results using these cooling rates.11.7 Clean the t
47、est cell by flushing solvents through the cell and then dry with clean air according to the manufacturersinstructions.NOTE 3Some apparatus is capable of automatic cleaning of the test cell and automatic sample changing.12. Report12.1 Report the temperature recorded in 11.6 as the automatic cloud poi
48、nt Test Method D5772.12.2 When specified, round the temperature recorded in 11.6 to the next lower integer and report as the Test Method D2500equivalent cloud point in accordance with Test Method D5772.13. Precision and Bias13.1 PrecisionThe precision of this test method as determined by the statist
49、ical examination of the interlaboratory testresults5,6 is as follows:13.1.1 RepeatabilityThe difference between successive test results obtained by the same operator using the same apparatusunder constant operating conditions on identical test material would in the long run, in the normal and correct operation of thistest method, exceed 1.3 C only in one case in twenty.13.1.2 ReproducibilityThe difference between two single and independent test results obtained by different operators workingin different laboratories
