ASTM D4539-22

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Designation: D4539 − 17 D4539 − 22
Standard Test Method for
Filterability of Diesel Fuels by Low-Temperature Flow Test
(LTFT)
This standard is issued under the fixed designation D4539; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers estimating the filterability of diesel fuels in some automotive equipment at low temperatures.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 Warning—Mercury has been designated by EPA and many stateregulatory agencies as a hazardous materialsubstance that can
cause central nervous system, kidney, and liver damage. serious medical issues. Mercury, or its vapor, may has been demonstrated
to be hazardous to health and corrosive to materials. Caution should be taken Use caution when handling mercury and
mercury-containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website
(http://www.epa.gov/mercury/faq.htm) for additional information. Users should be aware (SDS) for additional information. The
potential exists that selling mercury or mercury-containing products, or both, in your state may be prohibited by state law.is
prohibited by local or national law. Users must determine legality of sales in their location.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine 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 accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D97 Test Method for Pour Point of Petroleum Products
D975 Specification for Diesel Fuel
D1655 Specification for Aviation Turbine Fuels
D2500 Test Method for Cloud Point of Petroleum Products and Liquid Fuels
D3117 Test Method for Wax Appearance Point of Distillate Fuels (Withdrawn 2010)
D3699 Specification for Kerosine
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
This test method is under the jurisdiction of Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee D02.07
on Flow Properties.
Current edition approved Dec. 1, 2017Dec. 1, 2022. Published January 2018December 2022. Originally approved in 1985. Last previous edition approved in 20162017
as D4539 – 16.D4539 – 17. DOI: 10.1520/D4539-17.10.1520/D4539-22.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
*A Summary of Changes section appears at the end of this standard
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D4539 − 22
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
D7962 Practice for Determination of Minimum Immersion Depth and Assessment of Temperature Sensor Measurement Drift
E1 Specification for ASTM Liquid-in-Glass Thermometers
E644 Test Methods for Testing Industrial Resistance Thermometers
E2251 Specification for Liquid-in-Glass ASTM Thermometers with Low-Hazard Precision Liquids
E2877 Guide for Digital Contact Thermometers
2.2 Coordinating Research Council, Inc.
CRC Report No. 528 Diesel Fuel Low-Temperature Operability Field Test
2.3 Canadian General Standards Board:
CAN/CGSB-3.0, No. 14.01-M86,140.1-M86, Low Temperature Flow Test (LTFT) for Diesel Fuels
NOTE 1—CAN/CGSB-3.0, No. 140.1-M86 is essentially equivalent to Test Method D4539, but the differences in apparatus and procedures may or may
not yield different results.
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, refer to Terminology D4175.
3.1.2 digital contact thermometer (DCT), n—an electronic device consisting of a digital display and associated temperature
sensing probe.
3.1.2.1 Discussion—
This device consists of a temperature sensor connected to a measuring instrument; this instrument measures the temperature-
dependent quantity of the sensor, computes the temperature from the measured quantity, and provides a digital output. This digital
output goes to a digital display and/or recording device that may be internal or external to the device. These devices are sometimes
referred to as a “digital thermometer.”
3.1.2.2 Discussion—
PET is an acronym for portable electronic thermometers, a subset of digital contact thermometers (DCT).
4. Summary of Test Method
4.1 The temperature of a series of test specimens of fuel is lowered at a prescribed cooling rate. Commencing at a desired test
temperature and at each 1 °C interval thereafter, a separate specimen from the series is filtered through a 17 μm screen until a
minimum LTFT pass temperature is obtained. The minimum LTFT pass temperature is the lowest temperature, expressed as a
multiple of 1 °C, at which a test specimen can be filtered in 60 s or less.
4.2 Alternatively, a single specimen may be cooled as described under 4.1 and tested at a specified temperature to determine
whether it passes or fails at that temperature.
5. Significance and Use
5.1 The Low Temperature Flow Test results are indicative of the low temperature flow performance of the test fuel in some diesel
vehicles (according to CRC Report No. 528). The test method is especially useful for the evaluation of fuels containing flow
improver additives.
5.2 The test method can be used to supplement other measurements of diesel fuel low temperature behavior (in accordance with
Test Methods D97, D2500, and D3117).
6. Apparatus
6.1 Glass Specimen Vessels, (Borosilicate heat-resistant glass or equivalent) several 300 mL, clear, heat resistant, wide-mouthed
glass bottles having markings indicating 200 mL 6 10 mL and 50 mm to 60 mm ID or clear, heat resistant, tall form beakers with
no pour spouts and equivalent dimensions.
Available from Coordinating Research Council, Inc., 219 Perimeter Center Parkway, Atlanta, GA 30346.
Available from CGSB Sales Centre, Ottawa, Canada K1A 1G6.
D4539 − 22
FIG. 1 LTFT Sample Filtration Assembly
6.2 Glass Receiver Vessels, clear, heat resistant, glass containers graduated through 180 mL in 10 mL 6 2 mL increments.
6.3 Filtering Assembly (see Fig. 1),including a storage lid or some other form of cover, glass tubing, flexible fuel resistant tubing,
pinch clamp or valve, and rubber stopper, or other means to provide a vacuum seal.
6 7
6.4 Filter Assembly , as shown in detail in Fig. 2, for each sample container (300 mL beaker). 304SS sintered screen is a twill
Dutch weave mesh with a nominal filtration rating of 17 μm. The mesh is 65 wires/cm by 303/315 wires/cm. The wire 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 than 17 μm.
6.5 Programmable Cooling System, capable of cooling multiple specimens to the desired temperature at a mean rate of 1.0 °C per
hour between +10 °C and −30 °C. Absolute deviation of any single temperature point along the prescribed ramp function must not
exceed 0.5 °C in any specimen. The system’s size and shape are optional. Either liquid or air baths are acceptable.
6.6 Stop Watch or Electric Timer, capable of measuring tenths of a second.
6.7 Vacuum System, capable of maintaining a constant vacuum of 20.0 kPa 6 0.2 kPa below atmospheric pressure at the receiver
for the duration of each determination.
6.8 Temperature Measuring Device—Either a liquid-in-glass thermometer as described in 6.8.1 or a Digital Contact Thermometer
(DCT) meeting the requirements described in 6.8.2.
6.8.1 Liquid-in-glass Temperature Measuring Device—Conforming to specifications for ASTM Thermometer 114C for air baths.
For liquid baths use either ASTM Thermometer 5C in accordance with Specification E1, or ASTM Thermometer S5C in
accordance with Specification E2251, or an alternative liquid-in-glass thermometer with equal or better accuracy and equal
temperature response.
th
The sole source of supply of suitable filter cloth known to the committee at this time is Pall Aerospace Co., Pall Aeropower Corp., 6301 49 St. N, Pinellas Park, FL
33781. If you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at
a meeting of the responsible technical committee , which you may attend.
D4539 − 22
FIG. 2 LTFT Filter Assembly
6.8.2 Digital Contact Thermometer Requirements:
Parameter Requirement
DCT Guide E2877 Class F or better
A
Nominal Temperature Range –38 °C to +50 °C for liquid bath
–80 °C to 20 °C for air bath
Display Resolution 0.1 °C, minimum
B
Accuracy ±500 mK (±0.5 °C)
Sensor Type Platinum Resistance Thermometer (PRT)
C
Sensor Sheath 4.2 mm OD maximum
D
Sensor Length Less than 18 mm
E
Immersion Depth Less than 40 mm per Practice D7962
E
Measurement Drift Less than 500 mK (0.5 °C) per year
F
Response Time Less than or equal to 4 s per Footnote F
Calibration Error Less than 500 mK (0.5 °C) over the range of intended use.
Calibration Range Consistent with temperature range of use
D4539 − 22
Calibration Data Four data points evenly distributed over the calibration range that is consistent with the range of use. The calibration
data is to be included in calibration report.
Calibration Report From a calibration laboratory with demonstrated competency in temperature calibration which is traceable to a na-
tional calibration laboratory or metrology standards body.
A
The nominal temperature range may be different from the values shown provided the calibration and accuracy criteria are met.
B
Accuracy is the combined accuracy of the DCT unit which is the display and sensor.
C
Sensor sheath is the tube that holds the sensing element. The value is the outside diameter of the sheath segment containing the sensor element.
D
The physical length of the temperature sensing element.
E
As determined by Practice D7962 or an equivalent procedure.
F
Response Time—The 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 9 of
Test Method E644. The step change evaluation begins at 20 °C ± 5 °C air to 77 °C ± 5 °C with water circulating at 0.9 m ⁄s ± 0.09 m ⁄s past the sensor.
NOTE 2—A DCT display mounted on the end to the probe’s sheath is likely not suitable due to temperature exposure of the electronics. Consult
manufacturer for temperature limitations.
NOTE 3—When making measurements below –40 °C with a PRT, it may be necessary to use a 1000 ohm sensor in order to obtain accurate measurements.
6.8.3 The DCT calibration drift shall be checked at least annually by either measuring the ice point or against a reference
thermometer in a constant temperature bath at the prescribed immersion depth to ensure compliance with 6.8.2. See Practice
D7962.
NOTE 4—When a DCT’s calibration drifts in one direction over several calibration checks, it may be an indication of deterioration of the DCT.
7. Reagents
7.1 Jet A Aviation Turbine Fuel—As specified in Specification D1655, kerosine, as specified in Specification D3699, Grade No.
1 (or Grade Low Sulfur No. 1), as specified in Specification D975, or equivalent liquid that will not separate at temperatures down
to –30 °C.
7.2 Heptane—Reagent grade. (Warning—Flammable. See A1.2.)
7.3 Acetone—Reagent grade. (Warning—Flammable. See A1.1.)
8. Sampling
8.1 Obtain a sample in accordance with Practice D4057, or by Practice D4177.
8.2 Each specimen test requires a minimum of 200 mL. Ensure that sufficient sample is obtained to perform the subsequent series
of test specimens according to the procedure followed (see Section 4).
9. Procedure
9.1 Filter a fresh specimen of test fuel at 15 °C or higher, through dry, lintless filter paper, having a nominal filtration rating of
less than 17 μm. (Warning—Combustible liquid. See A1.3.)
NOTE 5—The purpose of this filtration step is to remove any contaminants that interfere with the effectiveness of low temperature flow improver additives.
However, this pre-filtration step may remove contaminants that affect the low temperature flow properties of the fuel in actual service. Users of this test
method may find it
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