1、Designation: D4539 10Standard Test Method forFilterability of Diesel Fuels by Low-Temperature Flow Test(LTFT)1This standard is issued under the fixed designation D4539; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of la
2、st 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 equipment at low tempera-tures.1
3、.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 liver damage. Mercury, orits vapor
4、, 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 additional informa-tion. Users shoul
5、d 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 standard to establish appro-priat
6、e 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 ProductsD975 Specification for Diese
7、l Fuel OilsD1655 Specification for Aviation Turbine FuelsD2500 Test Method for Cloud Point of Petroleum ProductsD3117 Test Method for Wax Appearance Point of DistillateFuels3D3699 Specification for KerosineD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automa
8、tic 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 Test42.3 Canadian General Standards Board:CAN/CGSB-3.0, No. 14.01-M86, Low Temperature FlowTes
9、t (LTFT) for Diesel Fuels5NOTE 1CAN/CGSB-3.0, No. 140.1-M86 is essentially equivalent toTest Method D4539, 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 specimens of fuel islowered at a prescribe
10、d 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 temperature,expressed as a multiple of 1C,
11、 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 LowTemperature FlowTest results are indica
12、tive ofthe low temperature flow performance of the test fuel in somediesel vehicles (according to CRC Report No. 528). The test1This test method is under the jurisdiction of Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.07 onFlow Properties.Cu
13、rrent edition approved Oct. 1, 2010. Published November 2010. Originallyapproved in 1985. Last previous edition approved in 2009 as D453909. DOI:10.1520/D4539-10.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book
14、of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Available from Coordinating Research Council, Inc., 219 Perimeter CenterParkway, Atlanta, GA 30346.5Ava
15、ilable from CGSB Sales Centre, Ottawa, Canada K1A 1G6.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.method is especially useful for the evaluation of fuels contain-i
16、ng flow improver additives.4.2 The test method can be used to supplement othermeasurements of diesel fuel low temperature behavior (inaccordance with Test Methods D97, D2500, and D3117).5. Apparatus5.1 Glass Specimen Vessels, (Borosilicate heat-resistantglass or equivalent) several 300-mL, clear, he
17、at resistant,wide-mouthed 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.
18、5.3 Filtering Assembly (see Fig. 1), including a storage lidor some other form of cover, glass tubing, flexible fuel resistanttubing, pinch clamp or valve, and rubber stopper, or othermeans to provide a vacuum seal.5.4 Filter Assembly6, as shown in detail in Fig. 2, for eachsample container (300-mL
19、beaker). 304SS sintered screen7is atwill Dutch weave mesh with a nominal filtration 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 partic
20、les equal to or greater than 17 m.5.5 Programmable Cooling System, capable of cooling 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 sp
21、ecimen. The systemssize and shape are optional. Either liquid or air baths areacceptable.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
22、 each determination.5.8 Temperature Measuring Device (Liquid-in-glassthermometer)Conforming to specifications for ASTM Ther-mometer 114C for air baths or ASTM Thermometer 5C forliquid baths in accordance with Specification E1, or any othertemperature measuring device with equal or better accuracyand
23、 equal temperature response.6. Reagents6.1 Jet A Aviation Turbine FuelAs specified in Specifica-tion D1655, kerosine, as specified in Specification D3699,Grade No. 1 (or Grade Low Sulfur No. 1), as specified inSpecification D975, or equivalent liquid that will not separateat temperatures down to 30C
24、.6.2 HeptaneReagent grade. (WarningFlammable. SeeA1.2.)6.3 AcetoneReagent grade. (WarningFlammable. SeeA1.1.)7. Sampling7.1 Obtain a sample in accordance with Practice D4057,orby Practice D4177.7.2 Each specimen test requires a minimum of 200 mL.Ensure that sufficient sample is obtained to perform t
25、hesubsequent series of test specimens according to the procedurefollowed (see Section 3).6The sole source of supply of the filter assembly known to the committee at thistime is Lawler Manufacturing Corp., Kilmer Ct., Edison, NJ and Alberta ResearchCouncil, Fuels and Lubricants Group, 250 Karl Clark
26、Rd., Edmonton, Alberta,Canada. If you are aware 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.7The sole source of supply of suit
27、able 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, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a
28、 meeting of the responsible technical committee1, which you may attend.FIG. 1 LTFT Sample Filtration AssemblyD4539 1028. 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 liq
29、uid. SeeA1.3.)NOTE 2The purpose of this filtration step is to remove any contami-nants that interfere with the effectiveness of low temperature flowimprover additives. However, this pre-filtration step may remove contami-nants that affect the low temperature flow properties of the fuel in actualserv
30、ice. Users of this test method may find it helpful to run the test withand without the pre-filtration step to compare results and in recognitionthat the precision of the test method will not apply if the pre-filtration stepis not carried out.8.2 Clean and inspect the filter assembly before each test
31、.Filters 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 5
32、0 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
33、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 clean, d
34、ry 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
35、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.FIG. 2 LTFT Filter AssemblyD4539 103(WarningCombustible li
36、quid. SeeA1.3.) Place the tempera-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 leas
37、t 5Cabove the wax appearance point (Test Method D3117) or cloudpoint (Test Method D2500) of the fuel under test. Duringmultiple specimen testing, a sufficient number of temperaturemonitoring vessels (from 8.5) must be distributed throughoutthe cooling bath to insure all test specimen temperaturescon
38、form with precision requirements. The positioning of allbottles or beakers shall permit unimpeded circulation of thecooling 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
39、 desired test temperature,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 below atmo-spheric pressure.8.9.4 Reset the timer.8.10 When the specimen has cooled to the desir
40、ed 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 bath
41、 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 R
42、eapply 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 a
43、 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 3Typically, a volume of approximately 180 mL will becollected in the receiver vessel in a passing result, but this volume mayv
44、ary 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 t
45、hat 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 obtain
46、ed.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 wh
47、ich 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 ap
48、paratusunder 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 results
49、 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 bias inthese test product combinations, no statement of bias can bemade.11. Keywords11.1 diesel fuel; filterability; flow; low temperature; LTFTD4539 104ANNEX(Mandatory Information)A1. WARNING STATEMENTSA1.1 AcetoneA1.1.1
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