1、Designation: D 4539 03e1An 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
2、 case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.e1NOTEFootnote 9 was corrected editorially in August 2004.1. Scope*1.1 This test method covers est
3、imating the filterability ofdiesel fuels in some automotive equipment at low tempera-tures.1.2 The values stated in SI units are to be regarded as thestandard. The values in parentheses are for information only.1.3 This standard does not purport to address all of thesafety concerns, if any, associat
4、ed with its use. It is theresponsibility 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. For specificwarning statements, see 8.1, 8.2.1, 8.3, 8.5, and Annex A1.2. Referenced Documents2.1 ASTM
5、Standards:D97 Test Method for Pour Point of Petroleum Oils2D 975 Specification for Diesel Fuel Oils2D 1655 Specification for Aviation Turbine Fuels2D 2500 Test Method for Cloud Point of Petroleum Prod-ucts2D3117 Test Method for WaxAppearance Point of DistillateFuels2D 3699 Specification for Kerosine
6、3D 4057 Practice for Manual Sampling of Petroleum andPetroleum Products3D 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3E1 Specification for ASTM Thermometers42.2 Coordinating Research Council, Inc.CRC Report No. 528 Diesel Fuel Low-Temperature Oper-ability Field Test52.3 C
7、anadian General Standards Board:CAN/CGSB-3.0, No. 14.01-M86, Low Temperature FlowTest (LTFT) for Diesel Fuels6NOTE 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 Met
8、hod3.1 The temperature of a series of test specimens 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. Them
9、inimum LTFT pass temperature is the lowest temperature,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
10、temperature.4. Significance and Use4.1 The LowTemperature 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 additi
11、ves.4.2 The test method can be used to supplement othermeasurements of diesel fuel low temperature behavior (inaccordance with Test Methods D 97, D 2500, and D 3117).5. Apparatus5.1 Glass Specimen Vessels, (Borosilicate heat-resistantglass or equivalent) several 300-mL, clear, heat resistant,wide-mo
12、uthed glass bottles having markings indicating 200 610 mL and 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.1This test method is
13、 under the jurisdiction of Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow Properties.Current edition approved May 10, 2003. Published June 2003. Originallyapproved in 1985. Last previous edition approved in 2002 as D 453902.2Annual Bo
14、ok of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 05.02.4Annual Book of ASTM Standards, Vol 14.03.5Available from Coordinating Research Council, Inc., 219 Perimeter CenterParkway, Atlanta, GA 30346.6Available from CGSB Sales Centre, Ottawa, Canada K1A 1G6.1*A Summary of Changes sec
15、tion appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 Filtering Assembly (see Fig. 1), including a storage lidor some other form of cover, glass tubing, flexible fuel resistanttubing, pinch clamp
16、 or valve, and rubber stopper, or othermeans to provide a vacuum seal.5.4 Filter Assembly7, as shown in detail in Fig. 2, for eachsample container (300-mL beaker). 304SS sintered screen8is atwill Dutch weave mesh with a nominal filtration rating of 17m. The mesh is 65 wires/cm (165 wires/in.) X 303/
17、315wires/cm (770/800 wires/in.). The wire strands have diametersof 0.0071 cm (0.0028 in.) and 0.0046 cm (0.0018 in.),respectively. The nominal filtration rating indicates a 98 %removal by mass weight of all particles equal to or greater than17 m.5.5 Programmable Cooling System, capable of cooling mu
18、l-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 areacceptable
19、.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 (150 6 1.5 mm Hg) belowatmospheric pressure at the receiver for the duration of eachdetermination.5.8 Temperature Measuring Device (Liquid-in-glassth
20、ermometer)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 Fuel
21、As specified 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 AcetoneR
22、eagent grade. (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 proceduref
23、ollowed (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.)8.2 Clean and inspect the filter assembly before each test.Filters obtained from
24、 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 with7The sole source of supply of the filter assembly known to
25、the committee at thistime is 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 co
26、mments will receive careful consider-ation at a meeting of the responsible technical committee1, which you may attend.8The 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 a
27、ware of alternative suppliers, 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 AssemblyD453903e12three successive washes of at
28、 least 50 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
29、damaged filterscreens. 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
30、clean, dry 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 i
31、nto one or 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 te
32、mpera-ture 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
33、 point (Test 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 requir
34、ements. The 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 temperatur
35、e,check the following:8.9.1 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 (150 + 1.5 mmHg) below atmospheric pressure.8.9.4 Reset the timer.FIG. 2 LTFT Filter AssemblyD453903e138.10 When the spe
36、cimen has cooled to the desired 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
37、removed from the cooling bath 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 (15
38、0 + 1.5 mm Hg) belowatmospheric pressure.8.12 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:
39、8.13.1 Passing ResultThe result is considered 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 v
40、essel in a passing result, but this volume mayvary 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
41、8.9 through 8.12 on subsequent test specimens 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 passi
42、ng (8.13.1)orafailing (8.13.2) result is obtained.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 d
43、ata were obtained in acooperative program in which 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
44、 obtained by the same operator with the same apparatusunder 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 diffe
45、rence between two singleand independent results 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
46、.2 BiasThere being no criteria for measuring bias 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 (Warni
47、ngVapors may cause flash fire.)A1.1.3 (WarningKeep 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 appar
48、atus 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 (WarningKeep container closed.)A1.2.4 (Warni
49、ngUse with adequate ventilation.)A1.2.5 (WarningAvoid prolonged breathing of vapor orspray mist.)A1.2.6 (WarningAvoid prolonged or repeated skin con-tact.)A1.3 Combustible LiquidA1.3.1 (WarningCombustible. Vapor harmful.)A1.3.2 (WarningKeep away from heat, sparks, and openflame.)D453903e14A1.3.3 (WarningKeep container closed.)A1.3.4 (WarningUse with adequate ventilation.)A1.3.5 (WarningAvoid prolonged breathing of vapor orspray mist.)A1.3.6 (WarningAvoid prolonged or repeated skin con-tact.)A1.4 Mercury
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