ASTM D7321-08
(Test Method)Standard Test Method for Test Method for Particulate Contamination of Biodiesel B100 Blend Stock Biodiesel Esters and Biodiesel Blends by Laboratory Filtration
Standard Test Method for Test Method for Particulate Contamination of Biodiesel B100 Blend Stock Biodiesel Esters and Biodiesel Blends by Laboratory Filtration
SIGNIFICANCE AND USE
The mass of particulates present in a fuel is a significant factor, along with the size and nature of the individual particles, in the rapidity with which fuel system filters and other small orifices in fuel systems can become plugged. This test method provides a means of assessing the mass of particulates present in a fuel sample.
The test method can be used in specifications and purchase documents as a means of controlling particulate contamination levels in the fuels purchased.
SCOPE
1.1 This test method covers the determination of the mass of particulate contamination in B100 biodiesel in accordance with Specification D 6751 and BXX blends that are prepared against all No. 1 and No. 2 grade fuels allowed within Specifications D 396, D 975, D 2880, and D 3699.
Note 1—Middle distillate fuels with flash points less than 38°C have been ignited by discharges of static electricity when the fuels have been filtered through inadequately bonded or grounded glass fiber filter systems. See Guide D 4865 for a more detailed discussion of static electricity formation and discharge.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D7321–08
Standard Test Method for
Test Method for Particulate Contamination of Biodiesel B100
Blend Stock Biodiesel Esters and Biodiesel Blends by
Laboratory Filtration
This standard is issued under the fixed designation D7321; 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 D6751 Specification for Biodiesel Fuel Blend Stock (B100)
for Middle Distillate Fuels
1.1 Thistestmethodcoversthedeterminationofthemassof
particulatecontaminationinB100biodieselinaccordancewith
3. Terminology
Specification D6751 and BXX blends that are prepared against
3.1 Definitions:
all No. 1 and No. 2 grade fuels allowed within Specifications
3.1.1 biodiesel, n—fuel comprised of mono-alkyl esters of
D396, D975, D2880, and D3699.
long chain fatty acids derived from vegetable oils or animal
NOTE 1—Middle distillate fuels with flash points less than 38°C have
fats, designated B100.
been ignited by discharges of static electricity when the fuels have been
3.1.2 biodiesel blend, BXX, n—blend of biodiesel fuel with
filtered through inadequately bonded or grounded glass fiber filter
petroleum based biodiesel fuel.
systems. See Guide D4865 for a more detailed discussion of static
3.1.3 bond, v—to connect two parts of a system electrically
electricity formation and discharge.
bymeansofaconductivewiretoeliminatevoltagedifferences.
1.2 The values stated in SI units are to be regarded as the
3.1.4 ground, v—to connect electrically with earth.
standard. The values given in parentheses are for information
3.2 Definitions of Terms Specific to This Standard:
only.
3.2.1 control glass fiber filter, n—lower of the two stacked
1.3 This standard does not purport to address all of the
glass fiber filters used in this test method.
safety concerns, if any, associated with its use. It is the
3.2.2 filtered flushing fluids, n—either of two solvents,
responsibility of the user of this standard to establish appro-
heptane or 2,2,4-trimethylpentane, filtered through a nominal
priate safety and health practices and determine the applica-
0.45 µm filter.
bility of regulatory limitations prior to use.
3.2.3 testglassfiberfilter,n—upperofthetwostackedglass
fiber filters used in this test method.
2. Referenced Documents
2.1 ASTM Standards:
4. Summary of Test Method
D396 Specification for Fuel Oils
4.1 B100 Biodiesel Blend Stock Filtration:
D975 Specification for Diesel Fuel Oils
4.1.1 Ameasuredvolumeofabout400mLofbiodieselester
D1193 Specification for Reagent Water
(B100) is vacuum filtered through two 0.7 µm glass fiber filters
D2880 Specification for Gas Turbine Fuel Oils
(a test filter and a control filter). When the contamination is
D3699 Specification for Kerosine
high or of a nature that induces slow filtration rates, two or
D4057 Practice for Manual Sampling of Petroleum and
more filtrations using a fresh filter set consisting of test and
Petroleum Products
control filters each time may be required to complete filtration
D4865 Guide for Generation and Dissipation of Static
in a reasonable time.
Electricity in Petroleum Fuel Systems
4.1.2 After the filtration has been completed, the test filter
D5452 Test Method for Particulate Contamination in Avia-
andcontrolfiltersarewashedwithsolvent,dried,andweighed.
tion Fuels by Laboratory Filtration
The particulate contamination level is determined by subtract-
ing the mass gain from the control filter from the mass gained
This test method is under the jurisdiction of ASTM Committee D02 on by the test filter, and is reported in units of g/m or its
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
equivalent in mg/L.
D02.14 on Stability and Cleanliness of Liquid Fuels.
4.2 BXX Biodiesel Blend Filtration:
Current edition approved March 15, 2008. PublishedApril 2008. DOI: 10.1520/
4.2.1 A measured volume of about 800 mL of biodiesel
D7321-08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
blend (BXX) is vacuum filtered through two 0.7 µm glass fiber
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
filters(atestfilterandacontrolfilter).Whenthecontamination
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7321–08
is high or of a nature that induces slow filtration rates, two or which the grounding wire passes shall connect the sidearm of
more filtrations using a fresh filter set consisting of test and the receiving flask to the tube passing through the rubber
control filters each time may be required to complete filtration stopper in the top of the safety flask.
in a reasonable time. 6.1.5 Vacuum System, either a water aspirated or a mechani-
4.2.2 After the filtration has been completed, the test filter cal vacuum pump may be used if capable of producing a
andcontrolfiltersarewashedwithsolvent,dried,andweighed. vacuum of 1 to 100 kPa below atmospheric pressure when
The particulate contamination level is determined by subtract- measured at the receiving flask.
ing the mass gain from the control filter from the mass gained 6.2 Other Apparatus:
by the test filter, and is reported in units of g/m or its 6.2.1 Air Ionizer, if used for the balance case.Air ionizers if
equivalent in mg/L. used should be replaced annually.
NOTE 3—When using a solid-pan balance, the air ionizer may be
5. Significance and Use
omittedprovidedthat,whenweighingaglassfiberfilter,itisplacedonthe
5.1 The mass of particulates present in a fuel is a significant
pan so that no part protrudes over the edge of the pan.
factor, along with the size and nature of the individual
6.2.2 Analytical Balance, single- or double-pan, with the
particles, in the rapidity with which fuel system filters and
precision standard deviation of 0.07 mg or less.
other small orifices in fuel systems can become plugged. This
6.2.3 Crucible Tongs, for handling clean sample container
test method provides a means of assessing the mass of
lids.
particulates present in a fuel sample.
6.2.4 Drying Oven, naturally convected (without fan-
5.2 The test method can be used in specifications and
assisted air circulation), controlling to 90 6 5°C.
purchase documents as a means of controlling particulate
6.2.5 Flushing Fluid Dispenser, an apparatus for dispensing
contamination levels in the fuels purchased.
flushing fluid through a nominal 0.45 µm filter.
6.2.6 Forceps, approximately 12-cm long, flat-bladed, with
6. Apparatus
non-serrated, non-pointed tips.
6.1 Filtration System—Arrange the following components
6.2.7 Graduated Cylinders, to contain at least 1 L of fluid
as shown in Fig. 1.
and marked at 10-mL intervals. For samples that filter slowly,
6.1.1 Funnel and Funnel Base, with filter support for a
100-mL graduated cylinders may be required.
47-mm diameter glass fiber, and locking ring or spring action
6.2.8 Petri Dishes, approximately 12.5 cm in diameter, with
clip.
removable glass supports for glass fiber filters.
6.1.2 Ground/Bond Wire, 0.912-2.59 mm (No. 10 through
NOTE 4—Small watch glasses, approximately 5 to 7 cm in diameter,
No. 19) bare stranded flexible, stainless steel, or copper
have also been found suitable to support the glass fiber filters.
installed in the flasks and grounded as shown in Fig. 1.
7. Reagents and Materials
NOTE 2—The electrical bonding apparatus described in Test Method
D5452 or other suitable means of electrical grounding that ensure safe
7.1 Purity of Reagents—Reagent grade chemicals shall be
operation of the filtration apparatus and flask can be used. If the filtrate is
used in all tests. Unless otherwise indicated, it is intended that
to be subsequently tested for stability, it is advisable not to use copper
all reagents shall conform to the specifications of the Commit-
since copper ions catalyze gum formation during the stability test.
tee onAnalytical Reagents of theAmerican Chemical Society,
6.1.3 Receiving Flask, 1.5 L or larger borosilicate glass 3
where such specifications are available. Other grades may be
vacuum filter flask, into which the filtration apparatus fits,
used, provided it is first ascertained that the reagent is of
equipped with a sidearm to connect to the safety flask.
sufficient purity to permit its use without lessening the accu-
6.1.4 Safety Flask, 1.5 Lor larger borosilicate glass vacuum
racy of the determination.
filter flask equipped with a sidearm to connect the vacuum
7.2 Purity of Water—Unless otherwise indicated, references
system. A fuel and solvent resistance rubber hose through
to water mean reagent water as defined byTypes I, II and III of
Specification D1193.
7.3 Flushing Fluids:
7.3.1 Heptane,(Warning—Flammable).
7.3.2 2,2,4-trimethylpentane (isooctane),(Warning—
Flammable).
7.4 propan-2-ol (2-propanol; isopropyl alcohol),
(Warning—Flammable).
7.5 Liquid or Powder Detergent, water-soluble, for cleaning
glassware.
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
FIG. 1 Schematic of Filtration System MD.
D7321–08
7.6 Test Glass Fiber Filters, plain, 47-mm diameter, nomi- of particulate formation by light-promoted reactions. Do not
nal pore size 0.7-µm. transfer the fuel sample from its original sample container into
7.7 Control Glass Fiber Filters, (see Note 7), 47-mm an intermediate storage container. If the original sample
diameter, nominal pore size 0.7-µm. container is damaged or leaking, then a new sample must be
7.7.1 Glassfiberfilterswithagridimprintedontheirsurface obtained.
may be used as control glass fiber filters for identification. 8.1.5 Analyze fuel samples as soon as possible after sam-
7.8 Protective Cover, polyethylene film or clean aluminum pling.Whenafuelcannotbeanalyzedwithinoneday,itshould
foil. be blanketed with an inert gas such as oxygen-free nitrogen,
argon, or helium. Store at a temperature no higher than 10°C
8. Sampling (50°F);sampleswithcloudpointsabove10°Cmaybestoredat
room temperature.
8.1 Sampling for Procedure for Biodiesel Blend Stock
8.2 Sampling for Procedure for Biodiesel Blends (BXX):
(B100):
8.2.1 The sample container for BXX shall be 1 L(60.15 L)
8.1.1 The sample container should be 500 mL (60.15 L) in
in volume and have a screw-on cap with an inert liner. Glass
volume and have a screw-on cap with an inert liner. Glass
containers are preferred to facilitate a visual inspection of the
containers are preferred to facilitate a visual inspection of the
contents and the container before and after filling. Glass
contents and the container before and after filling. Glass
containers also allow for visual inspection of the container,
containers also allow for visual inspection of the container,
after the sample is emptied, to confirm complete rinsing of the
after the sample is emptied, to confirm complete rinsing of the
container. Epoxy-lined sample cans, polytetrafluoroethylene
container. Epoxy-lined sample cans, polytetrafluoroethylene
(PTFE) bottles, and high density linear polyethylene bottles
(PTFE) bottles, and high density linear polyethylene bottles
have also been found suitable as sample containers, but these
have also been found suitable as sample containers, but they
are less desirable since visual inspection of the interior of the
are less desirable since visual inspection of the interior of the
container is more difficult.
container is more difficult.
8.2.1.1 It is important to note that the entire contents of the
8.1.1.1 It is imperative that the entire contents of the sample
sample container are filtered during the BXX filtration. This
container are filtered during the B100 filtration. This includes
includes not only all of the fuel but also all rinsings of the
not only all of the fuel but also all rinsings of the interior of the
interior of the container with flushing fluid. Because of this,
container with flushing fluid. Because of this, take care to
take care to protect the sample from any external contamina-
protect the sample from any external contamination.
tion.The expectation is, allowing for ullage, that the volume in
8.1.2 Ifitisnotpossibletosampleina500mLbottle,orthe
the 1-L sample bottle will be 800 mL (60.15 L).
sample has already been received ina1L bottle, follow
8.2.2 Follow 8.1.3-8.1.5.
8.1.2.1.
8.1.2.1 Vigorously shake the sample for 1 min, and transfer
9. Preparation of Apparatus and Sample Containers
400 mL to a clean fresh 500 mL (60.15 L) bottle. If a clean
fresh 500 mL (60.15 L) bottle is not available, use a clean 9.1 Clean all components of the filtration apparatus as
fresh 1 L (60.15 L) bottle. described in 9.1.1-9.1.4.
8.1.3 Precautions to avoid sample contamination shall in- 9.1.1 Remove any labels, tags, and so forth.
clude selection of an appropriate sampling point. Samples 9.1.2 Rinse apparatus thoroughly with propan-2-ol that has
should preferentially be obtained dynamically from a sampling been filtered through a 0.45 µm glass fiber filter.
loop in a distribution line, or from the flushing line of a field
9.1.3 Rinse thoroughly with filtered flushing fluid and dry.
sampling kit. Ensure that the line to be sampled is flushed with 9.1.4 Keepacleanprotectivecover(thecovermayberinsed
fuel before taking the sample.
withfilteredflushingfluid)overthetopofthesamplecontainer
8.1.3.1 Where it is desirable or only possible to obtain until the cap is installed. Similarly protect the funnel opening
samples from static storage, follow the procedures given in
of the assembled filtration apparatus with a clean protective
Practice D4057 or equivalent, taking precautions for cleanli- cover until ready for use.
ness of all equipment used. Ensure that the sample has not
9.1.5 Use clean sample containers.
passed through intermediate containers prior to placement in
the prepared container.
10. Preparation of Glass fiber Filters
10.1 Each set of test filters consists of one test glass fiber
NOTE 5—Samplesobtainedfromstaticstoragemaygiveresultsthatare
not representative of the bulk contents of the tank because of particulate
filterandonecontrolglassfiberfilter.Forfuelscontaininglittle
matter settling. Where possible, the contents of the tank should be
particulate materials, only one set of filters is required. If the
circulated or agitated before sampling, or the sampl
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