ASTM D7501-09
(Test Method)Standard Test Method for Determination of Fuel Filter Blocking Potential of Biodiesel (B100) Blend Stock by Cold Soak Filtration Test (CSFT)
Standard Test Method for Determination of Fuel Filter Blocking Potential of Biodiesel (B100) Blend Stock by Cold Soak Filtration Test (CSFT)
SIGNIFICANCE AND USE
Some substances that are soluble or appear to be soluble in biodiesel (B100) at room temperature will, upon cooling to temperatures above the cloud point or standing at room temperature for extended periods, come out of solution. This phenomenon has been observed in both B100 and BXX blends. These substances can cause filter plugging. This method provides an accelerated means of assessing the presence of these substances in B100 and their propensity to plug filters.
B100 biodiesel fuels that give short filtration times are expected to give satisfactory operation of BXX blends at least down to the cloud point of the biodiesel blends.
The test method can be used in specifications as a means of controlling levels of minor filter plugging components in biodiesel and biodiesel blends.
SCOPE
1.1 This test method covers the determination by filtration time after cold soak of the suitability for a biodiesel (B100) blend stock that meets all other requirements of Specification D 6751 and has a cloud point below 68°F (20°C) to provide adequate low temperature operability performance to at least the cloud point of the finished blend.
1.2 The formal precision of this test method has not yet been determined. Interim precision for repeatability is included in 13.1.
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
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Designation:D7501–09
Standard Test Method for
Determination of Fuel Filter Blocking Potential of Biodiesel
(B100) Blend Stock by Cold Soak Filtration Test (CSFT)
This standard is issued under the fixed designation D7501; 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 3. Terminology
1.1 This test method covers the determination by filtration 3.1 Definitions:
time after cold soak of the suitability for a biodiesel (B100) 3.1.1 biodiesel, n—fuel comprised of mono-alkyl esters of
blend stock that meets all other requirements of Specification long chain fatty acids derived from vegetable oils or animal
D6751 and has a cloud point below 68°F (20°C) to provide fats, designated as B100.
adequate low temperature operability performance to at least 3.1.2 bond, v—to connect two parts of a system electrically
the cloud point of the finished blend. bymeansofaconductivewiretoeliminatevoltagedifferences.
1.2 Theformalprecisionofthistestmethodhasnotyetbeen 3.1.3 BXX blend, n—fuel blend consisting of up to 20
determined. Interim precision for repeatability is included in volume percent biodiesel designated as up to B20 conforming
13.1. to the requirements of Specification D6751 with the remainder
1.3 The values stated in inch-pound units are to be regarded being a light middle or middle distillate grade diesel fuel and
as standard. The values given in parentheses are mathematical meeting the requirements of this test method.
conversions to SI units that are provided for information only 3.1.3.1 Discussion—The abbreviation BXX represents a
and are not considered standard. specific blend concentration in the range B2 to B20, where XX
1.4 This standard does not purport to address all of the is the percent volume of biodiesel in the fuel blend.
safety concerns, if any, associated with its use. It is the 3.1.4 ground, v—to connect electrically with earth.
responsibility of the user of this standard to establish appro- 3.2 Definitions of Terms Specific to This Standard:
priate safety and health practices and determine the applica- 3.2.1 air chamber, n—unit to control temperature of sample
bility of regulatory limitations prior to use. for cooling with maximum 0.5°C variation from set point. The
unit shall use a microprocessor temperature controller with
2. Referenced Documents
digitalsetpointandreadout.Afood-graderefrigeratordoesnot
2.1 ASTM Standards:
provide adequate temperature stability for this test method.
D4057 Practice for Manual Sampling of Petroleum and 3.2.2 minor component, n—material present in B100, typi-
Petroleum Products
cally at concentrations well below 1% by mass.
D5452 Test Method for Particulate Contamination in Avia- 3.2.3 thermal history, n—range of temperatures that a batch
tion Fuels by Laboratory Filtration
or sample of B100 has experienced which can result in
D6300 Practice for Determination of Precision and Bias separation or precipitation of minor components.
Data for Use in Test Methods for Petroleum Products and
3.2.3.1 Discussion—Coolingsomebiodieselfuelscanresult
Lubricants in precipitation or separation of minor components that have
D6751 Specification for Biodiesel Fuel Blend Stock (B100)
limited solubility in B100. Heating these biodiesel fuels above
for Middle Distillate Fuels 40°C is believed to redissolve most of these minor components
and thus erase the thermal history of the sample.
3.3 Abbreviations:
This test method is under the jurisdiction of ASTM Committee D02 on
3.3.1 CSFT—Cold Soak Filtration Test
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.14 on Stability and Cleanliness of Liquid Fuels.
4. Summary of Test Method
Current edition approved April 1, 2009. Published April 2009. DOI: 10.1520/
D7501-09.
4.1 Inthistestmethod,300 mLofbiodiesel(B100)isstored
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
at 40 6 1°F (4.5 6 0.5°C) for 16 h, allowed to warm to 77 6
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
2°F (25 6 1°C), and vacuum filtered through a single 0.7 µm
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. glassfiberfilteratcontrolledvacuumlevelsof21–25in.ofHg.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7501–09
FIG. 1 Schematic of Filtration System
4.2 The filtration time is reported in seconds. 6.1.3 Electrical Bonding Apparatus, as described in Test
Method D5452 or by using other suitable means of electrical
5. Significance and Use grounding that ensure safe operation of the filtration apparatus
and flask.
5.1 Some substances that are soluble or appear to be soluble
6.1.4 Receiving Flask, 1-L borosilicate glass vacuum filter
in biodiesel (B100) at room temperature will, upon cooling to
flask, into which the filtration apparatus fits, and equipped with
temperatures above the cloud point or standing at room
a sidearm to connect to the safety flask.
temperature for extended periods, come out of solution. This
phenomenonhasbeenobservedinbothB100andBXXblends. 6.1.5 Safety Flask, 1-Lborosilicate glass vacuum filter flask
These substances can cause filter plugging. This method equipped with a sidearm to connect the vacuum system.Afuel
provides an accelerated means of assessing the presence of and solvent resistant rubber hose, through which the grounding
these substances in B100 and their propensity to plug filters. wire is connected to the sidearm of the receiving flask to the
tube, passes through the rubber stopper in the top of the safety
5.1.1 B100 biodiesel fuels that give short filtration times are
flask.
expected to give satisfactory operation of BXX blends at least
down to the cloud point of the biodiesel blends.
6.1.6 Vacuum System, capable of producing a vacuum of 70
to 100 kPa below atmospheric pressure when measured at the
5.2 Thetestmethodcanbeusedinspecificationsasameans
of controlling levels of minor filter plugging components in safety flask.Amechanical vacuum pump may be used if it has
this capability.
biodiesel and biodiesel blends.
NOTE 2—Water aspirated vacuum will not provide relative vacuum
6. Apparatus
within the prescribed range.
6.1 Filtration System—Arrange the following components
6.1.7 Chilling Apparatus, either 6.1.7.1 or 6.1.7.2 may be
as shown in Fig. 1.
used.
6.1.1 Funnel and Funnel Base, with a stainless steel filter
6.1.7.1 Circulating Water Bath, capable of sustaining a
supportfora47-mmdiameterglassfiberfilter,andlockingring
temperature of 40 6 1°F (4.5 6 0.5°C).
or spring action clip, capable of receiving 300 mL.
6.1.7.2 Air Chamber, capable of sustaining a temperature of
NOTE 1—Sintered glass supports were found to give much higher
40 6 1°F (4.5 6 0.5°C). The unit shall use microprocessor
filtration times during initial studies and are not recommended to be used.
temperature control and have a digital temperature control/
display.
6.1.2 Ground/Bond Wire, 0.912-2.59-mm (No. 10 through
No. 19) bare stranded flexible, stainless steel or copper 6.1.8 Circulating Water Bath, capable of sustaining a tem-
installed in the flasks and grounded as shown in Fig. 1. perature of 77 6 1°F (25 6 0.5°C).
D7501–09
6.1.9 Glass Fiber Filters, plain, 47-mm diameter, nominal with Practice D4057, and refers to an “all-levels” sample.
pore size 0.7-µm. (Warning—Samples obtained from static storage can give
6.2 Other Apparatus: results which are not representative of the bulk contents of the
6.2.1 Forceps, approximately 12-cm long, flat-bladed, with tank because of particulate matter settling.)
non-serrated, non-pointed tips. 8.2 Precautions—to avoid sample contamination include:
6.2.2 Graduated Cylinders, to contain at least 0.5 L of fluid 8.2.1 Selection of an appropriate sampling point.
and marked at 10-mL intervals. Samples that filter slowly may 8.2.2 Use of clean sample containers. Visually inspect the
require 100-mL graduated cylinders. sample container before taking the samples to verify that there
6.2.3 Petri Dishes, approximately 12.5 cm in diameter, with are no visible particles present inside the container.
removable glass supports for glass fiber filters. 8.2.3 Keeping a clean protective cover over the top of the
6.2.3.1 Small Watch Glasses, approximately 5 to 7 cm in sample container until the cap is replaced after filling.
diameter, have been found suitable to support the glass fiber 8.2.4 If the primary sample container cannot be selected
filters.
such that it is suitable for this test procedure, the sample shall
pass through only a minimum number of intermediate contain-
NOTE 3—B100 will dissolve some plastics. This can cause the filters to
ers prior to placement in the final container.
adhere to the plastic.
8.2.5 After filling the sample container with 300 mL of
6.2.4 Protective Cover, polyethylene film or clean alumi-
sample, protect the fuel sample from prolonged exposure to
num foil.
light by wrapping the container in aluminum foil or storing it
6.2.5 Timer, capable of displaying elapsed times of at least
in the dark to reduce the possibility of particulate formation by
900 s to the nearest 0.1 s.
light-promoted reactions.
6.2.6 Thermometer or RTD Sensor, for measuring sample
8.3 If 300 mL of sample is not received in a 500-mL bottle
temperature, should be capable of measurement 61°F
or the sample has been received in a container not suitable for
(60.5°C).
this test, follow the sampling condition procedure in 8.4.
8.4 Sample Conditioning—for samples received that might
7. Reagents and Materials
have been cooled to temperatures below 68°F (20°C):
7.1 Purity of Reagents—Reagent grade chemicals shall be
8.4.1 Upon receipt of a biodiesel blend stock (B100)
used in all tests. Unless otherwise indicated, it is intended that
sample, the entire sample is to be heated to 104°F (40°C) for
all reagents shall conform to the specifications of the Commit-
at least 3 h under an inert atmosphere to erase any thermal
tee onAnalytical Reagents of theAmerican Chemical Society,
history and to dissolve any solids that might have precipitated
where such specifications are available. Other grades may be
during transit. After heating for the required time, allow the
used, provided it is first ascertained that the reagent is of
sample to sit for 24 h at a temperature no lower than 68°F
sufficient purity to permit its use without lessening the accu-
(20°C).
racy of the determination.
8.4.2 This sample conditioning step may be omitted if the
7.2 Flushing Fluids—Flushing fluids are not required for
sample was collected from a heated tank at a production
the test as the filter is not weighed. However, heptane or
facility. In this case, proceed directly to 8.5.
isooctane may be used to wash the apparatus after filtration to
8.4.3 If there is any doubt about the thermal history of the
remove any residue.
sample, the sample conditioning step shall be performed.
7.2.1 Heptane,(Warning—Flammable.)
8.5 Analyzefuelsamplesassoonaspossibleaftersampling.
7.2.2 2,2,4-trimethylpentane (isooctane),(Warning—
8.6 Shake the sample vigorously for 1 min. If the sample is
Flammable.)
not already in a 500-mL bottle suitable for this test procedure,
7.3 Liquid or Powder Detergent, water-soluble, for cleaning
transfer 300 mL to a clean, fresh 500 6 15-mL bottle. If a
glassware.
300-mL sample was received is already in such a bottle,
proceed with the test procedure in Section 11.
8. Sampling
8.1 A separate representative sample shall be collected for
9. Preparation of Apparatus and Sample Containers
this test method. Samples may preferentially be obtained
9.1 Clean all components of the filtration apparatus using
dynamicallyfromasamplingloopinadistributionlineorfrom
the reagents described in 7.2 and 7.3.
the flushing line of a field sampling kit. Ensure that the line to
9.1.1 Filtration apparatus shall be clean and dry prior to use.
be sampled is flushed with fuel before collecting the sample.
9.1.2 Remove any labels, tags, and so forth.
Alternatively, circulate or agitate the contents of the tank in
order to collect a representative sample that includes any
10. Preparation of Glass Fiber Filter
precipitatesthatmighthavesettledinthetank.Oneoptionisto
sample the tank immediately after filling, before the contents 10.1 Each filtration uses one filter.The glass fiber filter used
for each individual test may be identified by marking the petri
have time to settle.
8.1.1 Where it is necessary to obtain samples from static dish used to hold and transport the filter.
10.2 Clean all glassware used in preparation of glass fiber
storage using a sampling container or intermediate containers,
follow the procedures given in Practice D4057 or equivalent, filter as described in 9.1.
taking precautions for cleanliness of all equipment used. This 10.3 Using forceps, place the filter on clean glass support
is interpreted to mean a representative sample in accordance rods or watch glasses in petri dish.
D7501–09
TABLE 1 Interim Precision Range from 2008 CSFT Robustness Study Data
100 s 150 s 200 s 250 s 300 s 360 s
Repeatability 14 20 26 32 39 46
Reproducibility 45 66 87 108 129 155
10.4 Placethepetridish,withitslidslightlyajar,inadrying sample container shall be filtered through the glass fiber filter
oven at 194°F (90 6 2°C and leave it for 30 min. to ensure a correct measure of the contamination in the sample.
10.5 Remove the petri dish from the drying oven. Keep the 11.8 Ifthefiltrationisnotcompletewhen720s(12min)has
petri dish cover ajar, such that the filter is protected from elapsed, turn off the vacuum system and record the duration of
contamination from the atmosphere.Allow 30 min for the filter the filtration to the nearest second. Record the pressure in the
to come to equilibrium with room air temperature and humid- system and the volume filtered just before the termination of
ity. the filtration.
10.6 Using clean forceps, place the filter centrally on the
12. Report
filter support of the filtration apparatus (see Fig. 1). Install the
12.1 Report the time for the 300 mLB100 to be completely
funnel and secure with locking ring or spring clip.
filtered as B100 CSFT time byASTM D7501 in seconds to the
10.7 Protect the funnel opening of the assembled filtration
nearest second.
apparatus with a clean protective cover until ready for use.
12.2 If the filtration of the 300 mL failed to be completed
11. Procedure
after 720 s, report the result as “B100 CSFT time greater than
720 s by AS
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