1、Designation: D 4539 09An American National StandardStandard Test Method forFilterability of Diesel Fuels by Low-Temperature Flow Test(LTFT)1This standard is issued under the fixed designation D 4539; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase 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 estimating the filterability ofdiesel fuels in some automotive e
3、quipment at low tempera-tures.1.2 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.3 WarningMercury has been designated by EPA andmany state agencies as a hazardous material that can causecentral nervous system, kidney, and liv
4、er damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury-containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAs website(http:/www.epa.gov/mercury/faq.htm) for addit
5、ional informa-tion. Users should be aware that selling mercury or mercury-containing products, or both, in your state may be prohibited bystate law.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 st
6、andard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 1.3, 8.1, 8.2.1, 8.3, 8.5, andAnnexA1.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum Produ
7、ctsD 975 Specification for Diesel Fuel OilsD 1655 Specification for Aviation Turbine FuelsD 2500 Test Method for Cloud Point of Petroleum ProductsD3117 Test Method for WaxAppearance Point of DistillateFuelsD 3699 Specification for KerosineD 4057 Practice for Manual Sampling of Petroleum andPetroleum
8、 ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Coordinating Research Council, Inc.CRC Report No. 528 Diesel Fuel Low-Temperature Oper-ability Field Test32.3 Canadian General Standards Board:CAN/CGSB-3.0, No.
9、 14.01-M86, Low Temperature FlowTest (LTFT) for Diesel Fuels4NOTE 1CAN/CGSB-3.0, No. 140.1-M86 is essentially equivalent toTest Method D 4539, but the differences in apparatus and procedures mayor may not yield different results.3. Summary of Test Method3.1 The temperature of a series of test specim
10、ens of fuel islowered at a prescribed cooling rate. Commencing at a desiredtest temperature and at each 1C interval thereafter, a separatespecimen from the series is filtered through a 17-m screenuntil a minimum LTFT pass temperature is obtained. Theminimum LTFT pass temperature is the lowest temper
11、ature,expressed as a multiple of 1C, at which a test specimen can befiltered in 60 s or less.3.2 Alternatively, a single specimen may be cooled asdescribed under 3.1 and tested at a specified temperature todetermine whether it passes or fails at that temperature.4. Significance and Use4.1 The LowTem
12、perature FlowTest results are indicative ofthe low temperature flow performance of the test fuel in somediesel vehicles (according to CRC Report No. 528). The testmethod is especially useful for the evaluation of fuels contain-ing flow improver additives.4.2 The test method can be used to supplement
13、 othermeasurements of diesel fuel low temperature behavior (inaccordance with Test Methods D 97, D 2500, and D 3117).1This test method is under the jurisdiction of Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow Properties.Current edit
14、ion approved April 15, 2009. Published May 2009. Originallyapproved in 1985. Last previous edition approved in 2003 as D 4539031.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informati
15、on, refer to the standards Document Summary page onthe ASTM website.3Available from Coordinating Research Council, Inc., 219 Perimeter CenterParkway, Atlanta, GA 30346.4Available from CGSB Sales Centre, Ottawa, Canada K1A 1G6.1*A Summary of Changes section appears at the end of this standard.Copyrig
16、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Apparatus5.1 Glass Specimen Vessels, (Borosilicate heat-resistantglass or equivalent) several 300-mL, clear, heat resistant,wide-mouthed glass bottles having markings indicating 200 610 mL a
17、nd 5060 mm ID or clear, heat resistant, tall formbeakers with no pour spouts and equivalent dimensions.5.2 Glass Receiver Vessels, clear, heat resistant, glass con-tainers graduated through 180 mL in 10 6 2 mL increments.5.3 Filtering Assembly (see Fig. 1), including a storage lidor some other form
18、of cover, glass tubing, flexible fuel resistanttubing, pinch clamp or valve, and rubber stopper, or othermeans to provide a vacuum seal.5.4 Filter Assembly5, as shown in detail in Fig. 2, for eachsample container (300-mL beaker). 304SS sintered screen6is atwill Dutch weave mesh with a nominal filtra
19、tion rating of 17m. The mesh is 65 wires/cm by 303/315 wires/cm. The wirestrands have diameters of 0.0071 cm and 0.0046 cm, respec-tively. The nominal filtration rating indicates a 98 % removalby mass weight of all particles equal to or greater than 17 m.5.5 Programmable Cooling System, capable of c
20、ooling mul-tiple specimens to the desired temperature at a mean rate of1.0C per hour between +10C and 30C. Absolute deviationof any single temperature point along the prescribed rampfunction must not exceed 0.5C in any specimen. The systemssize and shape are optional. Either liquid or air baths area
21、cceptable.5.6 Stop Watch or Electric Timer, capable of measuringtenths of a second.5.7 Vacuum System, capable of maintaining a constantvacuum of 20.0 6 0.2 kPa below atmospheric pressure at thereceiver for the duration of each determination.5.8 Temperature Measuring Device (Liquid-in-glassthermomete
22、r)Conforming to specifications for ASTM Ther-mometer 114C for air baths or ASTM Thermometer 5C forliquid baths in accordance with Specification E 1, or any othertemperature measuring device with equal or better accuracyand equal temperature response.6. Reagents6.1 Jet A Aviation Turbine FuelAs speci
23、fied in Specifica-tion D 1655, kerosine, as specified in Specification D 3699,Grade No. 1 (or Grade Low Sulfur No. 1), as specified inSpecification D 975, or equivalent liquid that will not separateat temperatures down to 30C.6.2 HeptaneReagent grade. (WarningFlammable. SeeA1.2.)6.3 AcetoneReagent g
24、rade. (WarningFlammable. SeeA1.1.)7. Sampling7.1 Obtain a sample in accordance with Practice D 4057,orby Practice D 4177.7.2 Each specimen test requires a minimum of 200 mL.Ensure that sufficient sample is obtained to perform thesubsequent series of test specimens according to the procedurefollowed
25、(see Section 3).8. Procedure8.1 Filter a fresh specimen of test fuel at 15C or higher,through dry, lintless filter paper, having a nominal filtrationrating of less than 17 m. (WarningCombustible liquid. SeeA1.3.)5The sole source of supply of the filter assembly known to the committee at thistime is
26、Lawler Manufacturing Corp., Kilmer Ct., Edison, NJ and Alberta ResearchCouncil, Fuels and Lubricants Group, 250 Karl Clark Rd., Edmonton, Alberta,Canada. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful c
27、onsider-ation at a meeting of the responsible technical committee1, which you may attend.6The sole source of supply of suitable filter cloth known to the committee at thistime is PallAerospace Co., PallAeropower Corp., 6301 49thSt. N, Pinellas Park, FL33781. If you are aware of alternative suppliers
28、, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.FIG. 1 LTFT Sample Filtration AssemblyD45390928.2 Clean and inspect the filter assembly before each test.F
29、ilters obtained from the manufacturer are already standard-ized. Appendix X1 provides a procedure for checking the filterperformance, if desired.8.2.1 Clean the assembled filter with two solvents using avacuum to draw the solvents through the screen. Begin withthree successive washes of at least 50
30、mL of heptane(WarningFlammable. See A1.2). Follow with three succes-sive washes of at least 50 mL of acetone (WarningExtremely flammable. See A1.1). Air dry the filters afterwashing.8.2.2 Visually inspect each filter assembly for screen dam-age or the presence of particulates. Discard any damaged fi
31、lterscreens. Reclean any filter screens containing particulates. Ifthe standardization of the filter is suspect, obtain a new filter.Alternately, return the filter to the manufacturer for verifica-tion; Appendix X1 provides a procedure for checking the filterperformance.8.3 Pour 200 mL of clean, dry
32、 fuel into each of the several300-mL beakers. (WarningCombustible liquid. See A1.3.)8.4 Insert the clean filter assembly into each specimencontainer and tightly cover the joint (Point A in Fig. 1) and lidwith aluminum foil to exclude condensation.8.5 Insert a temperature measuring device into one or
33、 moreseparate, identical glass specimen bottles or beaker(s) contain-ing 200 mL of Jet A aviation turbine fuel kerosine, or GradeNo. 1 (or Grade Low Sulfur No. 1) or equivalent liquid thatwill not phase separate at temperatures down to 30C.(WarningCombustible liquid. SeeA1.3.) Place the tempera-ture
34、 measuring portion of the device at or near the center of thebottle or beaker approximately half way between the top andthe bottom of the liquid.8.6 Place the specimen bottles or beaker (from 8.3 through8.5) into the cooling bath at a temperature that is at least 5Cabove the wax appearance point (Te
35、st Method D3117)orcloud point (Test Method D 2500) of the fuel under test.During multiple specimen testing, a sufficient number oftemperature monitoring vessels (from 8.5) must be distributedthroughout the cooling bath to insure all test specimen tem-peratures conform with precision requirements. Th
36、e position-ing of all bottles or beakers shall permit unimpeded circulationof the cooling medium across their bottoms and sides.8.7 Close the cooling baths door, if it has one.8.8 Start the temperature programmer at a rate of 1.0C/h.8.9 Before the sample reaches the desired test temperature,check th
37、e following:FIG. 2 LTFT Filter AssemblyD45390938.9.1 Apply the pinch clamp or close the valve at Point B inFig. 1.8.9.2 Place an empty receiver vessel in position.8.9.3 Adjust the vacuum to 20.0 6 0.2 kPa below atmo-spheric pressure.8.9.4 Reset the timer.8.10 When the specimen has cooled to the desi
38、red testingtemperature, use the filter assembly stem to gently stir (15revolutions at approximately 1 turn/s) the specimen to disperseany settled wax crystals. Remove the aluminum foil andconnect the filtration apparatus joint at Point A in Fig. 1.Ifthespecimen has to be removed from the cooling bat
39、h forfiltration, these steps shall be completed within 1 min.8.11 Filter the specimen by removing the pinch clamp oropen the valve at Point B in Fig. 1 while simultaneouslystarting the timer. If necessary, adjust the vacuum system tomaintain a vacuum of 20.0 + 0.2 kPa below atmosphericpressure.8.12
40、Reapply the pinch clamp or close the valve at Point Bin Fig. 1 at precisely 60 s or when suction is lost, whicheveroccurs first. Record the volume of specimen filtered in millili-tres and the testing temperature in degrees Celsius.8.13 PassFail Criteria:8.13.1 Passing ResultThe result is considered
41、a pass ifmost of the specimen has been siphoned into the receivervessel within 60 s, and suction is lost due to the low level ofspecimen remaining in the specimen vessel.NOTE 2Typically, a volume of approximately 180 mL will becollected in the receiver vessel in a passing result, but this volume may
42、vary due to differences in specimen vessel dimensions and thetemperature/volume characteristics of the fuel.8.13.2 Failing ResultThe result is considered a fail ifsuction is not lost within 60 s.8.14 To determine the minimum LTFT pass temperature,repeat 8.9 through 8.12 on subsequent test specimens
43、that havebeen cooled 1C lower than the previous test temperature, untilat least one passing result and one failing result are obtained(see 8.13.1 and 8.13.2).8.15 Alternatively, cool a single specimen to a desiredtemperature and determine whether a passing (8.13.1)orafailing (8.13.2) result is obtai
44、ned.9. Report9.1 Report the temperature of the last passing result re-corded in 8.14 as:Minimum LTFT Pass Temperature =_C.9.2 Alternatively, report the result recorded in Step 8.15 as:Pass or Fail at _C.10. Precision and Bias10.1 PrecisionThe precision data were obtained in acooperative program in w
45、hich fuels were investigated over thetemperature range from 10 to 25C. The precision of thistest method as determined by the statistical examination ofinterlaboratory test results is as follows:10.1.1 RepeatabilityThe difference between successiveresults obtained by the same operator with the same a
46、pparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and correct operation ofthe test method exceed the following value only in one case intwenty.Repeatability 5 2C (1)10.1.2 ReproducibilityThe difference between two singleand independent result
47、s obtained by different operators work-ing in different laboratories on identical test material would, inthe long run, in the normal and correct operation of the testmethod, exceed the following value only in one case in twenty.Reproducibility 5 4C (2)10.2 BiasThere being no criteria for measuring b
48、ias inthese test product combinations, no statement of bias can bemade.11. Keywords11.1 diesel fuel; filterability; flow; low temperature; LTFTANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 AcetoneA1.1.1 (WarningExtremely flammable.)A1.1.2 (WarningVapors may cause flash fire.)A1.1.3 (Warning
49、Keep away from heat, sparks, and openflame.)A1.1.4 (WarningKeep container closed.)A1.1.5 (WarningUse with adequate ventilation.)A1.1.6 (WarningAvoid buildup of vapors, and eliminateall sources of ignition, especially non-explosion proof electri-cal apparatus and heaters.)A1.1.7 (WarningAvoid prolonged breathing of vapor orspray mist.)A1.1.8 (WarningAvoid contact with eyes or skin.)A1.2 n-HeptaneA1.2.1 (WarningFlammable. Harmful if inhaled.)A1.2.2 (WarningKeep away from heat, sparks, and openflame.)A1.2.3 (Wa
