1、Designation: D4539 16Standard 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, 9.1, 9.2.1, 9.3, 9.5, and AnnexA1.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petroleum ProductsD975 Specification for Dies
7、el Fuel OilsD1655 Specification for Aviation Turbine FuelsD2500 Test Method for Cloud Point of Petroleum Productsand Liquid FuelsD3117 Test Method for Wax Appearance Point of DistillateFuels (Withdrawn 2010)3D3699 Specification for KerosineD4057 Practice for Manual Sampling of Petroleum andPetroleum
8、 ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD7962 Practice for Determination of Minimum ImmersionDepth and Assessment of Temperature Sensor Measure-ment DriftE1 Specification for ASTM Liquid-in-Glass ThermometersE1137 Specification for Industrial Platinum Resista
9、nce Ther-mometersE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision LiquidsE2877 Guide for Digital Contact Thermometers2.2 Coordinating Research Council, Inc.CRC Report No. 528 Diesel Fuel Low-Temperature Oper-ability Field Test42.3 Canadian General Standards Board:
10、CAN/CGSB-3.0, No. 14.01-M86, Low Temperature FlowTest (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. Terminology3.1 Definitions:3.1.1 digital contact the
11、rmometer (DCT), nan electronicdevice consisting of a digital display and associated tempera-ture sensing probe.3.1.1.1 DiscussionThis device consists of a temperaturesensor connected to a measuring instrument; this instrumentmeasures the temperature-dependent quantity of the sensor,computes the temp
12、erature from the measured quantity, andprovides a digital output. This digital output goes to a digital1This test method is under the jurisdiction of Committee D02 on PetroleumProducts, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom-mittee D02.07 on Flow Properties.Current e
13、dition approved Dec. 1, 2016. Published January 2017. Originallyapproved in 1985. Last previous edition approved in 2010 as D4539 10. DOI:10.1520/D4539-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM
14、Standards volume information, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from Coordinating Research Council, Inc., 219 Perimeter CenterParkway, Atlanta, GA 30346.5Available from CGSB S
15、ales Centre, Ottawa, Canada K1A 1G6.*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 StatesThis international standard was developed in accordance with internationally recognize
16、d principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1display and/or recording device that may be internal or externalto t
17、he device. These devices are sometimes referred to as a“digital thermometer.”3.1.1.2 DiscussionPET is an acronym for portable elec-tronic thermometers, a subset of digital contact thermometers(DCT).4. Summary of Test Method4.1 The temperature of a series of test specimens of fuel islowered at a pres
18、cribed cooling rate. Commencing at a desiredtest temperature and at each 1 C 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
19、of 1 C, at which a test specimen canbe filtered in 60 s or less.4.2 Alternatively, a single specimen may be cooled asdescribed under 4.1 and tested at a specified temperature todetermine whether it passes or fails at that temperature.5. Significance and Use5.1 The LowTemperature FlowTest results are
20、 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.5.2 The test method can be used to supplement othermeasurements of diesel
21、fuel low temperature behavior (inaccordance with Test Methods D97, D2500, and D3117).6. Apparatus6.1 Glass Specimen Vessels, (Borosilicate heat-resistantglass or equivalent) several 300 mL, clear, heat resistant,wide-mouthed glass bottles having markings indicating200 mL 6 10 mL and 50 mm to 60 mm I
22、D or clear, heatresistant, tall form beakers with no pour spouts and equivalentdimensions.6.2 Glass Receiver Vessels, clear, heat resistant, glass con-tainers graduated through 180 mL in 10 mL 6 2 mL incre-ments.6.3 Filtering Assembly (see Fig. 1), including a storage lidor some other form of cover,
23、 glass tubing, flexible fuel resistanttubing, pinch clamp or valve, and rubber stopper, or othermeans to provide a vacuum seal.6.4 Filter Assembly6, as shown in detail in Fig. 2, for eachsample container (300 mL beaker). 304SS sintered screen7is atwill Dutch weave mesh with a nominal filtration rati
24、ng of17 m. The mesh is 65 wires/cm by 303/315 wires/cm. Thewire strands have diameters of 0.0071 cm and 0.0046 cm,respectively. The nominal filtration rating indicates a 98 %removal by mass weight of all particles equal to or greater than17 m.6.5 Programmable Cooling System, capable of cooling mul-t
25、iple specimens to the desired temperature at a mean rate of1.0 C per hour between +10 C and 30 C. Absolute devia-tion of any single temperature point along the prescribed rampfunction must not exceed 0.5 C in any specimen.The systemssize and shape are optional. Either liquid or air baths areacceptab
26、le.6.6 Stop Watch or Electric Timer, capable of measuringtenths of a second.7The 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, please prov
27、ide 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 AssemblyD4539 1626.7 Vacuum System, capable of maintaining a constantvacuum of 20.0 kPa 6
28、 0.2 kPa below atmospheric pressure atthe receiver for the duration of each determination.6.8 Temperature Measuring DeviceEither a liquid-in-glass thermometer as described in 6.8.1 or a Digital ContactThermometer (DCT) meeting the requirements described in6.8.2.6.8.1 Liquid-in-glass Temperature Meas
29、uring DeviceConforming to specifications for ASTM Thermometer 114Cfor air baths. For liquid baths use either ASTM Thermometer5C in accordance with Specification E1, or ASTM Thermom-eter S5C in accordance with Specification E2251,oranalternative liquid-in-glass thermometer with equal or betteraccurac
30、y and equal temperature response.6.8.2 Digital Contact Thermometer Requirements:Parameter RequirementDCT Guide E2877 Class F or betterTemperature Range 80 C to 20 CDisplay Resolution 0.1 C, minimumSensor Type Platinum Resistance Thermometer (PRT)Sensor 3 mm o.d. sheath with a sensing element less th
31、an 18mm in lengthMinimum Immersion Less than 40 mm per Practice D7962Accuracy 500 mK (0.5 C) for combined probe and sensorResponse Time Less than or equal to 25 s as defined in SpecificationE1137Drift Less than 500 mK (0.5 C) per yearCalibration Error Less than 500 mK (0.5 C) over the range of inten
32、deduse.Calibration Range 75 C or lower to 0 C or greaterCalibration Data 4 data points evenly distributed over calibration rangewith data included in calibration report.Calibration Report From a calibration laboratory with demonstrated compe-tency in temperature calibration which is traceable to ana
33、tional calibration laboratory or metrology standardsbody.FIG. 2 LTFT Filter AssemblyD4539 163NOTE 2A DCT display mounted on the end to the probes sheath islikely not suitable due to temperature exposure of the electronics. Consultmanufacturer for temperature limitations.6.8.3 The DCT calibration dri
34、ft shall be checked at leastannually by either measuring the ice point or against areference thermometer in a constant temperature bath at theprescribed immersion depth to ensure compliance with 6.8.2.See Practice D7962.NOTE 3When a DCTs calibration drifts in one direction over severalcalibration ch
35、ecks, it may be an indication of deterioration of the DCT.7. Reagents7.1 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 separ
36、ateat temperatures down to 30 C.7.2 HeptaneReagent grade. (WarningFlammable. SeeA1.2.)7.3 AcetoneReagent grade. (WarningFlammable. SeeA1.1.)8. Sampling8.1 Obtain a sample in accordance with Practice D4057,orby Practice D4177.8.2 Each specimen test requires a minimum of 200 mL.Ensure that sufficient
37、sample is obtained to perform thesubsequent series of test specimens according to the procedurefollowed (see Section 4).9. Procedure9.1 Filter a fresh specimen of test fuel at 15 C or higher,through dry, lintless filter paper, having a nominal filtrationrating of less than 17 m. (WarningCombustible
38、liquid. SeeA1.3.)NOTE 4The 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 actuals
39、ervice. 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.9.2 Clean and inspect the filter assembly before each t
40、est.Filters obtained from the manufacturer are already standard-ized. Appendix X1 provides a procedure for checking the filterperformance, if desired.9.2.1 Clean the assembled filter with two solvents using avacuum to draw the solvents through the screen. Begin withthree successive washes of at leas
41、t 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.9.2.2 Visually inspect each filter assembly for screen dam-age or the presence of particulates. Discard any damag
42、ed 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.9.3 Pour 200 mL of clean
43、, dry fuel into each of the several300 mL beakers. (WarningCombustible liquid. See A1.3.)9.4 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.9.5 Insert a temperature measuring device into o
44、ne 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 30 C.(WarningCombustible liquid. See A1.3.) Place the tempe
45、ra-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.9.6 Place the specimen bottles or beaker (from 9.3 through9.5) into the cooling bath at a temperature that is at least 5 Cabove the wax appearance p
46、oint (Test Method D3117) or cloudpoint (Test Method D2500) of the fuel under test. Duringmultiple specimen testing, a sufficient number of temperaturemonitoring vessels (from 9.5) must be distributed throughoutthe cooling bath to insure all test specimen temperaturesconform with precision requiremen
47、ts. The positioning of allbottles or beakers shall permit unimpeded circulation of thecooling medium across their bottoms and sides.9.7 Close the cooling baths door, if it has one.9.8 Start the temperature programmer at a rate of 1.0 Ch.9.9 Before the sample reaches the desired test temperature,chec
48、k the following:9.9.1 Apply the pinch clamp or close the valve at Point B inFig. 1.9.9.2 Place an empty receiver vessel in position.9.9.3 Adjust the vacuum to 20.0 kPa 6 0.2 kPa belowatmospheric pressure.9.9.4 Reset the timer.9.10 When the specimen has cooled to the desired testingtemperature, use t
49、he 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 forfiltration, these steps shall be completed within 1 min.9.11 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
