1、Designation: D4539 17Standard 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements, see 1.3, 9.1, 9.2.1, 9.3, 9.5,and Annex A1.1.5 This international standard was developed in accor-dance with internationally recognized principles on
7、 standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D97 Test Method for Pour Point of Petrol
8、eum ProductsD975 Specification for Diesel 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for Cloud Point of Petroleum Productsand Liquid FuelsD3117 Test Method for Wax Appearance Point of DistillateFuels (Withdrawn 2010)3D3699 Specification for KerosineD4057 Practice for Ma
9、nual Sampling of Petroleum andPetroleum 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 ThermometersE644 Test Me
10、thods for Testing Industrial Resistance 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
11、.3 Canadian General Standards Board:CAN/CGSB-3.0, No. 14.01-M86, Low Temperature FlowTest (LTFT) for Diesel Fuels51This 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 Propertie
12、s.Current edition approved Dec. 1, 2017. Published January 2018. Originallyapproved in 1985. Last previous edition approved in 2016 as D4539 16. DOI:10.1520/D4539-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual B
13、ook of ASTMStandards 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
14、from CGSB Sales 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 internationall
15、y recognized 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.1NOTE 1CAN/CGSB-3.0, No. 140.1-M86 is essentially equivale
16、nt 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 thermometer (DCT), nan electronicdevice consisting of a digital display and associated tempera-ture sensing probe.3.1.1.1 DiscussionThis d
17、evice consists of a temperaturesensor connected to a measuring instrument; this instrumentmeasures the temperature-dependent quantity of the sensor,computes the temperature from the measured quantity, andprovides a digital output. This digital output goes to a digitaldisplay and/or recording device
18、that may be internal or externalto the 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 s
19、pecimens of fuel islowered at a prescribed 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
20、temperature,expressed as a multiple 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
21、 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 additives.5.2 The test method can be used to sup
22、plement othermeasurements of diesel 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 indicatin
23、g200 mL 6 10 mL and 50 mm to 60 mm ID 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 sto
24、rage 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.6.4 Filter Assembly6, as shown in detail in Fig. 2, for eachsample container (300 mL beaker). 304SS sintered screen7is atwill Dutch weave
25、 mesh with a nominal filtration rating 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.7The sole source of s
26、upply 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 provide this information toASTM International Headquarters. Your comments will receive careful consid
27、er-ation at a meeting of the responsible technical committee1, which you may attend.FIG. 1 LTFT Sample Filtration AssemblyD4539 1726.5 Programmable Cooling System, capable of cooling mul-tiple specimens to the desired temperature at a mean rate of1.0 C per hour between +10 C and 30 C. Absolute devia
28、-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 areacceptable.6.6 Stop Watch or Electric Timer, capable of measuringtenths of a second.6.7 Vacuum System, capable of mainta
29、ining a constantvacuum of 20.0 kPa 6 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.
30、8.1 Liquid-in-glass Temperature Measuring 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 the
31、rmometer with equal or betteraccuracy and equal temperature response.FIG. 2 LTFT Filter AssemblyD4539 1736.8.2 Digital Contact Thermometer Requirements:Parameter RequirementDCT Guide E2877 Class F or betterNominal TemperatureRangeA38 C to +50 C for liquid bath80 C to 20 C for air bathDisplay Resolut
32、ion 0.1 C, minimumAccuracyB500 mK (0.5 C)Sensor Type Platinum Resistance Thermometer (PRT)Sensor SheathC4.2 mm OD maximumSensor LengthDLess than 18 mmImmersion DepthELess than 40 mm per Practice D7962Measurement DriftELess than 500 mK (0.5 C) per yearResponse TimeFLess than or equal to 4 s per Footn
33、ote FCalibration Error Less than 500 mK (0.5 C) over the range of intendeduse.Calibration Range Consistent with temperature range of useCalibration Data Four data points evenly distributed over the calibrationrange that is consistent with the range of use. The cali-bration data is to be included in
34、calibration report.Calibration Report From a calibration laboratory with demonstrated compe-tency in temperature calibration which is traceable to anational calibration laboratory or metrology standardsbody.AThe nominal temperature range may be different from the values shown providedthe calibration
35、 and accuracy criteria are met.BAccuracy is the combined accuracy of the DCT unit which is the display andsensor.CSensor sheath is the tube that holds the sensing element. The value is theoutside diameter of the sheath segment containing the sensor element.DThe physical length of the temperature sen
36、sing element.EAs determined by Practice D7962 or an equivalent procedure.FResponse TimeThe time for a DCT to respond to a step change in temperature.The response time is 63.2 % of the step change time as determined per Section 9of Test Method E644. The step change evaluation begins at 20 C 5 C air t
37、o77 C 5 C with water circulating at 0.9 m s 0.09 m s past the sensor.NOTE 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.NOTE 3When making measurements below 40 C with a PRT,
38、 itmay be necessary to use a 1000 ohm sensor in order to obtain accuratemeasurements.6.8.3 The DCT calibration drift 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 complia
39、nce with 6.8.2.See Practice D7962.NOTE 4When a DCTs calibration drifts in one direction over severalcalibration checks, 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,Gr
40、ade No. 1 (or Grade Low Sulfur No. 1), as specified inSpecification D975, or equivalent liquid that will not separateat 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 w
41、ith Practice D4057,orby Practice D4177.8.2 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 (see Section 4).9. Procedure9.1 Filter a fresh specimen of test fuel at 15 C or hi
42、gher,through dry, lintless filter paper, having a nominal filtrationrating of less than 17 m. (WarningCombustible liquid. SeeA1.3.)NOTE 5The purpose of this filtration step is to remove any contami-nants that interfere with the effectiveness of low temperature flowimprover additives. However, this p
43、re-filtration step may remove contami-nants that affect the low temperature flow properties of the fuel in actualservice. 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 w
44、ill not apply if the pre-filtration stepis not carried out.9.2 Clean and inspect the filter assembly before each test.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 wit
45、h two solvents using avacuum to draw the solvents through the screen. Begin withthree successive washes of at 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
46、.9.2.2 Visually inspect each filter assembly for screen dam-age or the presence of particulates. Discard any 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 manufactur
47、er for verifica-tion; Appendix X1 provides a procedure for checking the filterperformance.9.3 Pour 200 mL of clean, 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 (Poi
48、nt A in Fig. 1) and lidwith aluminum foil to exclude condensation.9.5 Insert a temperature measuring device into 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 liqu
49、id thatwill not phase separate at temperatures down to 30 C.(WarningCombustible liquid. See A1.3.) Place the tempera-ture measuring portion of the device at or near the center of theD4539 174bottle 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 point (Test Method D3117) or cloudpoint (Test Method D2500) of the fuel u
