1、Designation: D5773 15D5773 15aDesignation: IP 446/09Standard Test Method forCloud Point of Petroleum Products (Constant Cooling RateMethod)1This standard is issued under the fixed designation D5773; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se 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 cloud point o
3、fpetroleum 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/IP 219, do not substitute this test method or any othermethod without obt
4、aining comparative data and agreement from the specifier.1. Scope*1.1 This test method covers the determination of the cloud point of petroleum products and biodiesel fuels that are transparentin layers 40 mm in thickness by an automatic instrument using a constant cooling rate.1.2 This test method
5、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 units are to be regarded as standar
6、d. 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 practices and determine the applic
7、ability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D2500 Test Method for Cloud Point of Petroleum ProductsD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petroleum and Petroleum Products2.2 Energy In
8、stitute Standard:3IP 219 Test Method for Cloud Point of Petroleum ProductsIP 446 Determination of the Cloud Point of Petroleum ProductsAutomatic Constant Cooling Rate Method3. Terminology3.1 Definitions:3.1.1 biodiesel, na fuel comprised of mono-alkyl esters of long-chain fatty acids derived from ve
9、getable oils or animal fats,designated B100.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved April 1, 2015Dec. 1, 2015. Published Ap
10、ril 2015February 2016. Originally approved in 1995. Last previous edition approved in 20102015 asD5773 10.D5773 15. DOI: 10.1520/D5773-15.10.1520/D5773-15A.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM
11、 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., http:/www.energyinst.org.uk.This document is not an ASTM standard and is intended only to provide the user of an ASTM standar
12、d 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 that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM i
13、s 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 Conshohocken, PA 19428-2959. United States13.1.1.1 DiscussionBiodiesel is typically produced by a reaction of vegetable oil
14、 or animal fat with an alcohol such as methanol or ethanol in thepresence of a catalyst to yield mono-esters and glycerin. The fuel typically may contain up to 14 different types of fatty acids thatare chemically transformed into fatty acid methyl esters (FAME).3.1.2 biodiesel blend, na blend of bio
15、diesel fuel with petroleum-based diesel fuel designated BXX, where XX is the volumepercentage of biodiesel.3.1.3 cloud point, n in petroleum products and biodiesel fuels, the temperature of a liquid specimen when the smallestobservable cluster of hydrocarbon crystals first occurs upon cooling under
16、prescribed conditions.3.1.3.1 DiscussionThe cloud point occurs when the temperature of the specimen is low enough to cause hydrocarbon crystals to precipitate. In ahomogeneous liquid, the cloud is always noted first at the location in the specimen where the specimen temperature is the lowest.The clo
17、ud point is the temperature at which the crystals first occur, regardless of their location in the specimen, and not afterextensive crystallization has taken place. The hydrocarbon crystals that precipitate at lower temperatures are typically, but notexcluded to, straight chain hydrocarbons commonly
18、 called “wax crystals.”3.1.3.2 DiscussionThe purpose of the cloud point is to measure the wax crystals in the specimen; however, trace amounts of water and inorganiccompounds may also be present. The intent of the cloud point measurement is to capture the temperature at which the liquid fuelin the s
19、pecimen begins to change from a single liquid phase to a two-phase system containing solid and liquid. It is not the intentof this test method to monitor the phase transition of the trace components such as water.3.2 Definitions of Terms Specific to This Standard:3.2.1 automatic cloud point, nthe te
20、mperature 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 crystalformation. The apparatus and the conditio
21、ns 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 constant cooling rate method, n in cloud point test methods, test procedure using prescribed cooling rate, spe
22、cimenreceptacle, and optical system for detection of crystal formation.3.2.2.1 DiscussionThe prescribed cooling rate is described in 4.1; the specimen receptacle is described in Annex A1; and the optical system for thedetection of crystal formation is described in Annex A1.3.2.3 Peltier device, na s
23、olid state thermoelectric device constructed with dissimilar semiconductor materials and configuredin such a way that it will transfer heat to or away from a test specimen dependent on the direction of electric current applied tothe device.3.2.4 D2500/IP 219 equivalent cloud point, nthe temperature
24、of a specimen, in integers, calculated by rounding the resultsof this test method to the next lower integer.3.2.4.1 DiscussionThis test method produces results with 0.1 C resolution. Should the user wish to provide results with a similar format to TestMethod D2500, then this calculation can be perfo
25、rmed. Some apparatus can perform this calculation automatically.4. Summary of Test Method4.1 A prescribed specimen (11.5) is cooled by a Peltier device (A1.1) at a constant rate of 1.5 Cmin 6 0.1 Cmin whilecontinuously being illuminated by a light source (A1.1.4). The specimen is continuously monito
26、red by an array of optical detectors(A1.1.5, Fig. A1.1) for the first appearance of a cloud of wax crystals. The detectors are sufficient in number to ensure that anyD5773 15a2solid phase hydrocarbon crystals that may form are detected. The temperature at which the appearance of a cloud of wax cryst
27、alsis first detected in the specimen is recorded to 0.1 C resolution. When the recorded temperature is rounded to the next lowerinteger temperature, it is designated as the D2500/IP 219 equivalent cloud point per Test Method D5773.5. Significance and Use5.1 The cloud point of petroleum products and
28、biodiesel fuels is an index of the lowest temperature of their utility for certainapplications. Wax crystals of sufficient quantity can plug filters used in some fuel systems.5.2 Petroleum blending operations require a precise measurement of the cloud point.5.3 This test method can determine the tem
29、perature of the test specimen at which wax crystals have formed sufficiently to beobserved as a cloud with a resolution of 0.1 C.5.4 This test method provides results that are equivalent to Test Method D2500.NOTE 1This is based on the Test Method D2500 equivalent cloud point in which the 0.1 C resul
30、t is rounded to the next lower integer.5.5 This test method determines the cloud point in a shorter period of time than Test Method D2500.NOTE 2In cases of samples with cloud points near ambient temperatures, time savings may not be realized.5.6 This test method eliminates most of the operator time
31、required of Test Method D2500.5.7 This test method does not require the use of a mechanical refrigeration apparatus.NOTE 3In certain cases of high ambient temperature, a source of cooling water may be required to measure low temperature cloud points (see 7.1).6. Apparatus6.1 Automatic Apparatus4The
32、automatic cloud point apparatus described in this test method consists of a test chambercontrolled by a microprocessor that is capable of controlling the heating and cooling of the test specimen, optically observing thefirst appearance of a cloud of wax crystals and recording the temperature of the
33、specimen described in detail in Annex A1.6.2 The apparatus shall be equipped with a specimen cup, optical detector array, light source, digital display, Peltier device, anda specimen temperature measuring device.6.3 The Peltier device shall be capable of heating or cooling the test specimen at a con
34、stant rate of 1.5 Cmin 6 0.1 Cmin.6.4 The temperature measuring device in the specimen cup shall be capable of measuring the temperature of the test specimenfrom 40 C to +70 C at a resolution of 0.1 C.6.5 The apparatus shall be equipped with fittings to permit the circulation of a liquid cooling med
35、ium, if required, to removeheat generated by the Peltier device and other electronic components of the apparatus.NOTE 4Some apparatus are designed to use ambient air as a cooling medium. In such cases, a built-in fan is available to provide circulation of airand there is no need for fittings as desc
36、ribed for a liquid cooling medium. The function of the cooling medium is to remove heat from the electroniccomponents. The choice of the cooling medium has no impact whatsoever on the test results.6.6 The apparatus shall be equipped with fittings to permit the circulation of purge gas to purge the t
37、est chamber containing thespecimen cup of any atmospheric moisture.7. Reagents and Materials7.1 Cooling MediumAir, tap water, or other liquid heat exchange medium sufficient to remove heat generated by the Peltierdevice and other electronic components from the apparatus. To achieve specimen cooling
38、to 40 C, supply circulation of liquidcooling medium at +25 C or lower to the apparatus. For an apparatus which relies on air as cooling medium, the ambient airtemperature has to be below +30 C to achieve specimen cooling to 40 C.7.2 Purge GasA gas such as air, nitrogen, helium, or argon with a dew p
39、oint below the lowest operating temperature of theanalyzer. (WarningCompressed gas under high pressure.) (WarningInert gas can be an asphyxiant when inhaled.)7.3 Precision VolumeDispensing Device, capable of dispensing 0.15 mL 6 0.01 mL of sample.7.4 Cotton SwabsPlastic or paper shaft cotton swabs u
40、sed to clean the sample cup. (WarningThe use of swabs with woodenshafts may damage the mirrored surface of the specimen cup.)8. Sampling8.1 Obtain a sample in accordance with Practices D4057 or D4177.4 The sole source of supply of the Phase Technology Cloud PointAnalyzer model series 10, 30, 70, 70V
41、, and 70X known to the committee at this time is Phase Technology,11168 Hammersmith Gate, Richmond, B.C. Canada V7A 5H8. The various model series mentioned above are differentiated by their cooling capacities and user interfaces;however, all of them are capable of covering the entire temperature ran
42、ge specified in the scope. If you are aware of alternative suppliers, please provide this informationto ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.D5773 15a38.2 Samples of very viscous m
43、aterials may be warmed until they are reasonably fluid before they are tested. However, no sampleshould 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 inserting into
44、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 paper,until the oil is perfectly clear, but make such filtration at a temperature at least 14 C above the expected cloud point.NOTE 5Moisture will be noticed in
45、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 Make liquid cooling mediu
46、m connections if required (see Note 4) and ensure that they do not leak.9.3 Make purge gas connections and ensure that they do not leak.9.4 Turn on the liquid cooling medium if required (see Note 4).9.5 Turn on the purge gas.9.6 Turn on the main power switch of the analyzer. After the automatic self
47、 diagnostics startup sequence is completed, theinstrument will display a READY message.10. 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 c
48、an be 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 the specimen cup. Pipette, syringe, or precision positive-displacementdevices are suitable for
49、use in delivering the specimen.11.3 Clean the specimen out of the cup. The cup must be cleaned to the point where no visible droplets of specimen remainin the cup. Non-abrasive absorbent materials such as cotton swabs are suitable for use in cleaning the specimen cup. Cleaningsolvents able to clean the specimen and compatible with the components of the apparatus can also be used. Naphtha, hexane,heptane, and toluene are suitable as cleaning solvents.11.4 Repeat steps 11.2 and 11.3.11.5 Carefully measure 0.15 mL6 0.
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