An American National Standard

Designation: D 6751 – 09

Standard Specification for

Biodiesel Fuel Blend Stock (B100) for Middle Distillate
Fuels1
This standard is issued under the fixed designation D 6751; 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* D 445 Test Method for Kinematic Viscosity of Transparent

1.1 This specification covers biodiesel (B100) Grades S15 and Opaque Liquids (and Calculation of Dynamic Viscos-
and S500 for use as a blend component with middle distillate ity)
fuels. D 524 Test Method for Ramsbottom Carbon Residue of
1.2 This specification prescribes the required properties of Petroleum Products
diesel fuels at the time and place of delivery. The specification D 613 Test Method for Cetane Number of Diesel Fuel Oil
requirements may be applied at other points in the production D 664 Test Method for Acid Number of Petroleum Products
and distribution system when provided by agreement between by Potentiometric Titration
the purchaser and the supplier. D 874 Test Method for Sulfated Ash from Lubricating Oils
1.3 Nothing in this specification shall preclude observance and Additives
of federal, state, or local regulations which may be more D 974 Test Method for Acid and Base Number by Color-
restrictive. Indicator Titration
D 975 Specification for Diesel Fuel Oils
NOTE 1—The generation and dissipation of static electricity can create D 976 Test Method for Calculated Cetane Index of Distil-
problems in the handling of distillate fuel oils with which biodiesel may
late Fuels
be blended. For more information on the subject, see Guide D 4865.
D 1160 Test Method for Distillation of Petroleum Products
1.4 The values stated in SI units are to be regarded as at Reduced Pressure
standard. No other units of measurement are included in this D 1266 Test Method for Sulfur in Petroleum Products
standard. (Lamp Method)
1.4.1 Exception—In Annex A1, the values stated in SI units D 1796 Test Method for Water and Sediment in Fuel Oils by
are to be regarded as the standard. The values given in the Centrifuge Method (Laboratory Procedure)
parentheses are for information only. D 2274 Test Method for Oxidation Stability of Distillate
Fuel Oil (Accelerated Method)
2. Referenced Documents
D 2500 Test Method for Cloud Point of Petroleum Products
2.1 ASTM Standards:2 D 2622 Test Method for Sulfur in Petroleum Products by
D 93 Test Methods for Flash Point by Pensky-Martens Wavelength Dispersive X-ray Fluorescence Spectrometry
Closed Cup Tester D 2709 Test Method for Water and Sediment in Middle
D 130 Test Method for Corrosiveness to Copper from Distillate Fuels by Centrifuge
Petroleum Products by Copper Strip Test D 2880 Specification for Gas Turbine Fuel Oils
D 189 Test Method for Conradson Carbon Residue of D 3117 Test Method for Wax Appearance Point of Distillate
Petroleum Products Fuels
D 3120 Test Method for Trace Quantities of Sulfur in Light
Liquid Petroleum Hydrocarbons by Oxidative Microcou-
1
This specification is under the jurisdiction of ASTM Committee D02 on lometry
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D 3242 Test Method for Acidity in Aviation Turbine Fuel
D02.E0 on Burner, Diesel, Non-Aviation Gas Turbine, and Marine Fuels.
Current edition approved April 15, 2009. Published June 2009. Originally D 3828 Test Methods for Flash Point by Small Scale Closed
approved in 1999 as PS 121–99. Adopted as a standard in 2002 as D 6751–02. Last Cup Tester
previous edition approved in 2008 as D 6751–08.
2
D 4057 Practice for Manual Sampling of Petroleum and
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
Petroleum Products
Standards volume information, refer to the standard’s Document Summary page on D 4177 Practice for Automatic Sampling of Petroleum and
the ASTM website. Petroleum Products

*A Summary of Changes section appears at the end of this standard.

Copyright (C) ASTM International. 100 Barr Harbour Dr. P.O. box C-700 West Conshohocken, Pennsylvania 19428-2959, United States

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 D 6751 – 09
D 4294 Test Method for Sulfur in Petroleum and Petroleum EN 14538 Fat and oil derivatives—Fatty acid methyl esters
Products by Energy Dispersive X-ray Fluorescence Spec- (FAME)—Determination of Ca, K, Mg and Na content by
trometry optical emission spectral analysis with inductively
D 4530 Test Method for Determination of Carbon Residue coupled plasma (ICP OES)5
(Micro Method)
D 4737 Test Method for Calculated Cetane Index by Four 3. Terminology
Variable Equation 3.1 Definitions:
D 4865 Guide for Generation and Dissipation of Static 3.1.1 biodiesel, n—fuel comprised of mono-alkyl esters of
Electricity in Petroleum Fuel Systems long chain fatty acids derived from vegetable oils or animal
D 4951 Test Method for Determination of Additive Ele- fats, designated B100.
ments in Lubricating Oils by Inductively Coupled Plasma 3.1.1.1 Discussion—biodiesel, as defined above, is regis-
Atomic Emission Spectrometry tered with the U.S. EPA as a fuel and a fuel additive under
D 5452 Test Method for Particulate Contamination in Avia- Section 211(b) of the Clean Air Act. There is, however, other
tion Fuels by Laboratory Filtration usage of the term biodiesel in the marketplace. Due to its EPA
D 5453 Test Method for Determination of Total Sulfur in registration and the widespread commercial use of the term
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel biodiesel in the U.S. marketplace, the term biodiesel will be
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence maintained for this specification.
D 5773 Test Method for Cloud Point of Petroleum Products 3.1.1.2 Discussion—Biodiesel is typically produced by a
(Constant Cooling Rate Method) reaction of a vegetable oil or animal fat with an alcohol such as
D 6217 Test Method for Particulate Contamination in methanol or ethanol in the presence of a catalyst to yield
Middle Distillate Fuels by Laboratory Filtration mono-alkyl esters and glycerin, which is removed. The finished
D 6300 Practice for Determination of Precision and Bias biodiesel derives approximately 10 % of its mass from the
Data for Use in Test Methods for Petroleum Products and reacted alcohol. The alcohol used in the reaction may or may
Lubricants not come from renewable resources.
D 6450 Test Method for Flash Point by Continuously 3.1.2 biodiesel blend (BXX), n—blend of biodiesel fuel with
Closed Cup (CCCFP) Tester diesel fuel oils.
D 6469 Guide for Microbial Contamination in Fuels and 3.1.2.1 Discussion—In the abbreviation BXX, the XX rep-
Fuel Systems resents the volume percentage of biodiesel fuel in the blend.
D 6584 Test Method for Determination of Free and Total 3.1.3 biodiesel fuel, n—synonym for biodiesel.
Glycerin in B-100 Biodiesel Methyl Esters by Gas Chro- 3.1.4 diesel fuel, n—middle petroleum distillate fuel.
matography 3.1.5 free glycerin, n—a measure of the amount of glycerin
D 6890 Test Method for Determination of Ignition Delay remaining in the fuel.
and Derived Cetane Number (DCN) of Diesel Fuel Oils by 3.1.6 Grade S15 B100, n—a grade of biodiesel meeting
Combustion in a Constant Volume Chamber ASTM Specification D 6751 and having a sulfur specification
D 7039 Test Method for Sulfur in Gasoline and Diesel Fuel of 15 ppm maximum.
by Monochromatic Wavelength Dispersive X-ray Fluores- 3.1.7 Grade S500 B100, n—a grade of biodiesel meeting
cence Spectrometry ASTM Specification D 6751 and having a sulfur specification
D 7397 Test Method for Cloud Point of Petroleum Products of 500 ppm maximum.
(Miniaturized Optical Method) 3.1.8 middle distillate fuel, n—kerosines and gas oils boil-
2.2 Government Standard: ing between approximately 150°C and 400°C at normal atmo-
40 CFR Part 79 Registration of Fuels and Fuel Additives spheric pressure and having a closed-cup flash point above
Section 211(b) Clean Air Act3 38°C.
2.3 Other Documents:4 3.1.9 total glycerin, n—the sum of the free glycerin and the
UOP 389 Trace Metals in Oils by Wet Ashing and ICP-OES glycerin portion of any unreacted or partially reacted oil or fat.
UOP 391–91 Trace Metals in Petroleum Products or Organ-
ics by AAS 4. Requirements
EN 14112 Fat and oil derivatives—Fatty acid methyl esters 4.1 The biodiesel specified shall be mono-alkyl esters of
(FAME)—Determination of oxidation stability (Acceler- long chain fatty acids derived from vegetable oils and animal
ated oxidation test)5 fats.
EN 14110 Fat and oil derivatives—Fatty acid methyl esters 4.2 Unless otherwise specified, samples for analysis shall be
(FAME)—Determination of methanol content5 taken by the procedure described in Practices D 4057 or
D 4177.
4.3 The biodiesel specified shall conform to the detailed
3
Available from U.S. Government Printing Office Superintendent of Documents, requirements shown in Table 1.
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
4
Available from ASTM International, 100 Barr Harbor Drive, PO Box C700,
NOTE 2—A considerable amount of experience exists in the U.S. with
West Conshohocken, PA. Visit the ASTM website, www.astm.org, or contact ASTM a 20 % blend of biodiesel, primarily produced from soybean oil, with
Customer Service at service@astm.org. 80 % diesel fuel (B20). Experience with biodiesel produced from animal
5
Available from the National CEN Members listed on the CEN website fat and other oils is similar. Experience with B20 and lower blends in other
(www.cenorm.be) or from the CEN/TC19 secretariat (astm@nen.nl). applications is not as prevalent. Although biodiesel (B100) can be used,

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 D 6751 – 09
TABLE 1 Detailed Requirements for Biodiesel (B100) (All Sulfur Levels)
Grade S15 Grade S500
Property Test MethodA Units
Limits Limits
Calcium and Magnesium, combined EN 14538 5 max 5 max ppm (µg/g)
Flash point (closed cup) D 93 93 min 93 min °C
Alcohol control
One of the following must be met:
1. Methanol content EN 14110 0.2 max 0.2 max mass %
2. Flash point D 93 130 min 130 min °C
Water and sediment D 2709 0.050 max 0.050 max % volume
Kinematic viscosity, 40°C D 445 1.9-6.0B 1.9–6.0B mm2/s
Sulfated ash D 874 0.020 max 0.020 max % mass
SulfurC D 5453 0.0015 max (15) 0.05 max (500) % mass (ppm)
Copper strip corrosion D 130 No. 3 max No. 3 max
Cetane number D 613 47 min 47 min
Cloud point D 2500 ReportD ReportD °C
Carbon residueE D 4530 0.050 max 0.050 max % mass
Acid number D 664 0.50 max 0.50 max mg KOH/g
Cold soak filterability Annex A1 360 maxF 360 maxF seconds
Free glycerin D 6584 0.020 max 0.020 max % mass
Total glycerin D 6584 0.240 max 0.240 max % mass
Phosphorus content D 4951 0.001 max 0.001 max % mass
Distillation temperature, D 1160 360 max 360 max °C
Atmospheric equivalent temperature,
90 % recovered
Sodium and Potassium, combined EN 14538 5 max 5 max ppm (µg/g)
Oxidation stability EN 14112 3 minimum 3 minimum hours
A
The test methods indicated are the approved referee methods. Other acceptable methods are indicated in 5.1.
B
See X1.3.1. The 6.0 mm2/s upper viscosity limit is higher than petroleum based diesel fuel and should be taken into consideration when blending.
C
Other sulfur limits can apply in selected areas in the United States and in other countries.
D
The cloud point of biodiesel is generally higher than petroleum based diesel fuel and should be taken into consideration when blending.
E
Carbon residue shall be run on the 100 % sample (see 5.1.11).
F
B100 intended for blending into diesel fuel that is expected to give satisfactory vehicle performance at fuel temperatures at or below –12°C shall comply with a cold
soak filterability limit of 200 s maximum.

blends of over 20 % biodiesel with diesel fuel (B20) should be evaluated 5.1.8 Cetane Number—Test Method D 613. Test Method
on a case by case basis until further experience is available. D 6890 may also be used. Test Method D 613 shall be the
NOTE 3—The user should consult the equipment manufacturer or referee method.
owner’s manual regarding the suitability of using biodiesel or biodiesel
blends in a particular engine or application. 5.1.9 Cloud Point—Test Method D 2500. Test Method
D 5773 or D 7397 may also be used. Test Method D 3117 may
5. Test Methods also be used because it is closely related. Test Method D 2500
5.1 The requirements enumerated in this specification shall shall be the referee test method. The precision and bias of Test
be determined in accordance with the following methods. Method D 3117 for biodiesel is not known and is currently
5.1.1 Flash Point—Test Methods D 93, except where other under investigation.
methods are prescribed by law. Test Methods D 3828 or 5.1.10 Acid Number—Test Method D 664. Test Methods
D 6450 can also be used. The precision and bias of Test D 3242 or D 974 may also be used. Test Method D 664 shall be
Methods D 3828 and D 6450 with biodiesel is not known and the referee test method.
is currently under investigation. Test Methods D 93 shall be the 5.1.11 Carbon Residue—Test Method D 4530. A 100 %
referee method. sample shall replace the 10 % residual, with percent residue in
5.1.2 Water and Sediment—Test Method D 2709. Test the original sample reported using the 10 % residual calcula-
Method D 1796 may also be used. Test Method D 2709 shall be tion (see X1.9.1). Test Methods D 189 or D 524 may also be
the referee method. The precision and bias of these test used. Test Method D 4530 shall be the referee method.
methods with biodiesel is not known and is currently under 5.1.12 Total Glycerin—Test Method D 6584.
investigation. 5.1.13 Free Glycerin—Test Method D 6584.
5.1.3 Viscosity—Test Method D 445. 5.1.14 Phosphorus Content—Test Method D 4951.
5.1.4 Sulfated Ash—Test Method D 874. 5.1.15 Distillation Temperature, Reduced Pressure—Test
5.1.5 Oxidation Stability—Test Method EN 14112. Method D 1160.
5.1.6 Sulfur—Test Method D 5453. Test Method D 7039 5.1.16 Calcium and Magnesium, combined—Test Method
may also be used. Other test methods may also be suitable for EN 14538. Test Method UOP 389 may also be used. Test
determining up to 0.05 % (500 ppm) sulfur in biodiesel fuels Method EN 14538 shall be the referee test method.
such as Test Methods D 1266, D 2622, D 3120 and D 4294 but 5.1.17 Sodium and Potassium, combined—Test Method
may provide falsely high results (see X1.5) although their EN 14538. Test Method UOP 391 may also be used. Test
precision and bias with biodiesel is unknown. Test Method Method EN 14538 shall be the referee test method.
D 5453 shall be the referee test method. 5.1.18 Cold Soak Filterability—The test method in Annex
5.1.7 Corrosion—Test Method D 130, 3 h test at 50°C. A1 shall be used to determine the cold soak filterability. B100

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 D 6751 – 09
intended for blending into diesel fuels that is expected to give 6. Workmanship
satisfactory vehicle performance at fuel temperatures at or
6.1 The biodiesel fuel shall be visually free of undissolved
below –12°C shall comply with a cold soak filtration limit of
water, sediment, and suspended matter.
200 s maximum. A cold soak filterability standard test method
is under development.
7. Keywords
NOTE 4—Interim precision information is provided in Annex A1 for the
cold soak filterability test to give the user some indication of the 7.1 alternative fuel; biodiesel fuel; diesel fuel oil; fuel oil;
repeatability and reproducibility expected. renewable resource

ANNEX

(Mandatory Information)

A1. DETERMINATION OF FUEL FILTER BLOCKING POTENTIAL OF BIODIESEL (B100) BLEND STOCK BY COLD SOAK
LABORATORY FILTRATION

A1.1 Scope A1.3.3 Abbreviations:

A1.1.1 This test method covers the determination by filtra- A1.3.3.1 CSFT—cold soak filtration test.
tion time after cold soak of the suitability for a Biodiesel
(B100) Blend Stock for blending with middle distillates to A1.4 Summary of Test Method
provide adequate low temperature operability performance to A1.4.1 In this test method, 300 mL of biodiesel (B100) is
at least the cloud point of the finished blend. stored at 4.4°C (40°F) for 16 h, allowed to warm to 20 to 22°C
A1.1.2 The interim precision of this test method has been (68 to 72°F), and vacuum filtered through a single 0.7 µm glass
determined. fiber filter.
A1.1.3 The values stated in SI units are to be regarded as the A1.4.2 In this test method, the filtration time is reported in
standard. The values given in parentheses are for information seconds.
only.
A1.1.4 This standard does not purport to address all of the A1.5 Significance and Use
safety concerns, if any, associated with its use. It is the A1.5.1 Some substances that are soluble or appear to be
responsibility of the user of this standard to establish appro- soluble in biodiesel at room temperature will, upon cooling or
priate safety and health practices and determine the applica- standing at room temperature for extended periods, come out
bility of regulatory limitations prior to use. of solution. These substances can cause filter plugging. This
test method provides an accelerated means of assessing the
A1.2 Referenced Documents propensity for these substances to plug filters.
A1.2.1 ASTM Standards:2 A1.5.1.1 Fuels that give short filtration times are expected
D 4057 Practice for Manual Sampling of Petroleum and to give satisfactory operation down to the cloud point of
Petroleum Products biodiesel blends.
D 4865 Guide for Generation and Dissipation of Static A1.5.2 The test method can be used in specifications as a
Electricity in Petroleum Fuel Systems means of controlling levels of minor filter plugging compo-
D 5452 Test Method for Particulate Contamination in nents in biodiesel and biodiesel blends.
Aviation Fuels by Laboratory Filtration
A1.6 Apparatus
A1.3 Terminology
A1.6.1 Filtration System—Arrange the following compo-
A1.3.1 Definitions: nents as shown in Fig. A1.1.
A1.3.1.1 biodiesel, n—fuel comprised of mono-alkyl esters A1.6.1.1 Funnel and Funnel Base, with a stainless steel
of long chain fatty acids derived from vegetable oils or animal filter support for a 47–mm diameter glass fiber filter and a
fats, designated B100. locking ring or spring action clip capable of receiving 300 mL.
A1.3.1.2 bond, v—to connect two parts of a system electri-
cally by means of a conductive wire to eliminate voltage NOTE A1.1—Sintered glass supports were found to give much higher
differences. filtration times during initial studies and should not be used.
A1.3.1.3 ground, v—to connect electrically with earth. A1.6.1.2 Ground/Bond Wire, 0.912 to 2.59 mm (No. 10
A1.3.2 Definitions of Terms Specific to this Standard: through No. 19) bare-stranded flexible stainless steel or copper
A1.3.2.1 filtered flushing fluids, n—either of two solvents, installed in the flasks and grounded as shown in Fig. A1.1.
heptane or 2,2, 4–trimethylpentane, filtered through a nominal NOTE A1.2—The electrical bonding apparatus described in Test
0.45 µm glass fiber filter. Method D 5452 or other suitable means of electrical grounding which
A1.3.2.2 glass fiber filter, n—the 0.7 µm glass fiber filters ensure safe operation of the filtration apparatus and flask can be used. If
used in this test method. the filtrate is to be subsequently tested for stability it is advisable not to use

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 D 6751 – 09

FIG. A1.1 Schematic of Filtration System

copper as copper ions catalyze gum formation during the stability test. A1.6.2.5 Protective Cover, polyethylene film or clean alu-
A1.6.1.3 Receiving Flask, 1-L borosilicate glass vacuum minum foil.
filter flask, into which the filtration apparatus fits, equipped A1.6.2.6 Liquid or Air Bath or Chamber, capable of sus-
with a sidearm to connect to the safety flask. taining a temperature of 4.4 6 1.1°C (40 6 2°F) for 16 h.
A1.6.1.4 Safety Flask, 1-L borosilicate glass vacuum filter A1.6.2.7 Timer, capable of displaying elapsed times of at
flask equipped with a sidearm to connect the vacuum system. least 900 s to the nearest 0.1 s.
A fuel and solvent resistant rubber hose, through which the
grounding wire passes, shall connect the sidearm of the A1.7 Reagents and Materials
receiving flask to the tube passing through the rubber stopper A1.7.1 Purity of Reagents—Reagent grade chemicals shall
in the top of the safety flask. be used in all tests. Unless otherwise indicated, it is intended
A1.6.1.5 Vacuum System, a vacuum system capable of that all reagents shall conform to the specifications of the
producing a vacuum of 70 to 100 kPa below atmospheric Committee on Analytical Reagents of the American Chemical
pressure when measured at the receiving flask. A mechanical Society, where such specifications are available.6 Other grades
vacuum pump may be used if it has this capability. may be used, provided it is first ascertained that the reagent is
of sufficient purity to permit its use without lessening the
NOTE A1.3—Water aspirated vacuum will not provide relative vacuum
within the prescribed range.
accuracy of the determination.
A1.7.2 Flushing Fluids—Flushing fluids are not required
A1.6.2 Other Apparatus: for the test as the filter is not weighed. However, heptane or
A1.6.2.1 Forceps, approximately 12-cm long, flat-bladed, isooctane may be used to wash the apparatus after filtration to
with non-serrated, non-pointed tips. remove any residue. Alternatively soap and water may be used
A1.6.2.2 Graduated Cylinders, to contain at least 0.5 L of in accordance with A1.7.3.
fluid and marked at 10-mL intervals. Graduated cylinders, A1.7.2.1 Heptane, (Warning—Flammable).
100-mL, may be required for samples which filter slowly. A1.7.2.2 2,2,4-trimethylpentane (isooctane), (Warning—
A1.6.2.3 Petri Dishes, approximately 12.5 cm in diameter, Flammable).
with removable glass supports for glass fiber filters.
NOTE A1.4—Small watch glasses, approximately 5 to 7 cm in diameter,
have also been found suitable to support the glass fiber filters. 6
Reagent Chemicals, American Chemical Society Specifications, American
NOTE A1.5—B100 will dissolve some plastics. This can cause the Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
filters to adhere to the plastic. listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
A1.6.2.4 Glass Fiber Filters, plain, 47-mm diameter, nomi- and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
nal pore size 0.7-µm. MD.

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 D 6751 – 09
A1.7.3 Liquid or Powder Detergent, water-soluble, for A1.9.4.1 Upon receipt of a Biodiesel Blend Stock (B100)
cleaning glassware. sample, the entire sample shall be heated to 40°C for at least
3 h under an inert atmosphere to erase any thermal history and
A1.8 Preparation of Apparatus and Sample Containers to dissolve any solids that might have precipitated during
A1.8.1 Clean all components of the filtration apparatus transit unless it is known that the sample has never been cooled
using the reagents described in A1.7.2 and A1.7.3. below 20°C. If the sample has never been exposed to tempera-
A1.8.1.1 Remove any labels, tags, and so forth. tures below 20°C then proceed to A1.9.5.
A1.9.4.2 After heating for the required time, allow the
A1.9 Sampling sample to sit for 24 h at a temperature no lower than 20°C.
A1.9.5 Shake the sample vigorously for 1 min, and transfer
A1.9.1 The sample container should be 500 6 15 mL in 300 mL to a clean fresh 500 6 15 mL bottle.
volume and have a screw-on cap with an inert liner. Glass
containers are preferred to facilitate a visual inspection of the A1.10 Preparation of Glass Fiber Filter
contents and the container before and after filling. Glass A1.10.1 Each filtration uses one filter. The glass fiber filter
containers also allow for visual inspection of the container, used for each individual test shall be identified by marking the
after the sample is emptied, to confirm complete emptying of petri dishes used to hold and transport the filters.
the container. Epoxy-lined sample cans, polytetrafluoroethyl- A1.10.2 Clean all glassware used in preparation of glass
ene (PTFE) bottles, and high density linear polyethylene fiber filter as described in A1.8.1.
bottles have also been found suitable as sample containers but A1.10.3 Using forceps, place the filters on clean glass
are less desirable since visual inspection of the interior of the support rods or watch glasses in petri dish.
container is more difficult. A1.10.4 Place the petri dish with its lid slightly ajar in a
A1.9.2 Precautions to avoid sample contamination shall drying oven at 90 6 5°C, and leave it for 30 min.
include selection of an appropriate sampling point. It is A1.10.5 Remove the petri dish from the drying oven. Keep
preferred to obtain samples dynamically from a sampling loop the petri dish cover ajar, such that the filter is protected from
in a distribution line, or from the flushing line of a field contamination from the atmosphere. Allow 30 min for the filter
sampling kit. Ensure that the line to be sampled is flushed with to come to equilibrium with room air temperature and humid-
fuel before collecting the sample. ity.
A1.9.2.1 Use clean sample containers. A1.10.6 Using clean forceps, place the filter centrally on the
A1.9.2.2 Keep a clean protective cover over the top of the filter support of the filtration apparatus (see Fig. A1.1). Install
sample container until the cap is installed. Similarly protect the the funnel and secure with locking ring or spring clip. Do not
funnel opening of the assembled filtration apparatus with a remove the plastic film from the funnel opening until ready to
clean protective cover until ready for use. start filtration.
A1.9.2.3 Where it is desirable or only possible to obtain
samples from static storage, follow the procedures given in A1.11 Procedure
Practice D 4057 or equivalent, taking precautions for cleanli- A1.11.1 Place 300 mL of sample in a glass 500–mL bottle,
ness of all equipment used. The sample should pass through a and set in a liquid or air bath or chamber at 4.4 6 1.1°C (40 6
minimum number of intermediate containers prior to place- 2°F) for 16 6 0.5 h.
ment in the prepared container. A1.11.2 After the 16-h cold soak is completed, allow the
A1.9.2.4 Samples obtained from static storage can give sample to come back to room temperature at 20 to 22°C (68 to
results that are not representative of the bulk contents of the 72°F) on its own without external heating. The sample shall be
tank because of particulate matter settling. Where possible, the completely liquid before filtration. The sample shall be filtered
contents of the tank should be circulated or agitated before within 1 h after reaching 20 to 22°C (68 to 72°F).
sampling, or the sampling should be performed shortly after a A1.11.3 Complete assembly of the receiving flask, 0.7 µm
tank has been filled. glass fiber filter and funnel as a unit (see Fig. A1.1) before
A1.9.3 Visually inspect the sample container before taking swirling the sample. To minimize operator exposure to fumes,
the samples to verify that there are no visible particles present the filtering procedure should be performed in a fume hood.
inside the container. Fill the sample container to contain A1.11.4 Start the vacuum system. Record the pressure in the
300 mL. Protect the fuel sample from prolonged exposure to system after 1 min of filtration. The vacuum shall be between
light by wrapping the container in aluminum foil or storing it 71.1 and 84.7 kPa (21 and 25 in. Hg) below atmospheric
in the dark to reduce the possibility of particulate formation by pressure. If the vacuum is not within the specified range, make
light-promoted reactions. Do not transfer the fuel sample from adjustments to the vacuum system.
its original sample container into an intermediate storage A1.11.5 Thoroughly clean the outside of the sample con-
container. If the original sample container is damaged or tainer in the region of the cap by wiping it with a damp,
leaking, then a new sample shall be obtained. lint-free cloth. Swirl the container vigorously for about 2 to 3 s
A1.9.3.1 If a 500-mL bottle is not available, or the sample to dislodge any particles that may have adhered to the walls of
has already been received in a container not suitable for this the container.
test, follow A1.9.5. A1.11.6 Immediately after swirling, pour the entire contents
A1.9.4 Analyze fuel samples as soon as possible after of the sample container into the filtration funnel and simulta-
sampling. neously start the timer. The entire contents of the sample

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 D 6751 – 09
container shall be filtered through the glass fiber filter to ensure 1649.7 The report is an attempt to supply such an analysis
a correct measure of the contamination in the sample. based on well-established methodologies. Subsequent to test
NOTE A1.6—Take care not to shake the sample vigorously, as this could
method publication a more thorough round robin is planned.
cause some of the solids to go back into solution. 200 s 360 s
Repeatability 34.0 61.0
A1.11.7 If the filtration is not complete when 720 s (12 min) Reproducibility 115.9 208.1
has elapsed, turn off the vacuum system and record the
duration of the filtration to the nearest second. Record the NOTE A1.7—The degree of freedom associated with the repeatability
estimate from this round robin study is 25 for repeatability which is below
pressure in the system and the volume filtered just before the 30 but acceptable. The degree of freedom associated with the reproduc-
termination of the filtration. ibility estimate from this round robin study is 10 and below acceptable
limits. For that reason only the repeatability is included in A1.13.1.4.
A1.12 Reporting Since the minimum requirement of 30 (in accordance with Practice
A1.12.1 Report the time for the 300–mL B100 to be D 6300) is not met, users are cautioned that the actual repeatability/
completely filtered as B100 filtration time in seconds. reproducibility may be significantly different than these estimates. An
A1.12.2 If the filtration of the 300 mL failed to be com- ASTM ILS will be conducted in the future.
pleted after 720 s, report the volume that was filtered after A1.13.1.4 The difference between successive test results,
720 s. obtained by the same operator using the same apparatus under
constant operating conditions on identical test material for
A1.13 Precision and Bias B100 filtration would in the long run, in the normal and correct
A1.13.1 Precision—The precision of this test method for operation of this test method, exceed 0.1689(X + 1.2018)
B100 filtration has not yet been determined. time(s) only in one case in twenty.
A1.13.1.1 Repeatability—The difference between succes- A1.13.2 Bias—The procedure given for the determination
sive test results, obtained by the same operator using the same of B100 filtration time has no bias because the value of the
apparatus under constant operating conditions on identical test filtration time is defined in terms of this test method.
material for B100 filtration has not yet been determined.
A1.13.1.2 Reproducibility—The difference between the two A1.14 Keywords
single and independent results obtained by different operators A1.14.1 biodiesel; diesel fuel; glass fiber filter; biodiesel;
working in different laboratories on identical test material for filter blocking potential, cold soak filtration test, CSFT, biodie-
B100 filtration has not yet been determined. sel blend; laboratory filtration; glass fiber filter; low tempera-
A1.13.1.3 Interim Precision—Repeatability and reproduc- ture operability, middle distillate fuel.
ibility determinations were made using data from the ASTM
Biodiesel Low Temperature Operability Task Force. The analy- 7
Supporting data have been filed at ASTM International Headquarters and may
sis of the data is the subject of a research report, RR:D02- be obtained by requesting Research Report RR: D02-1649.

APPENDIXES

(Nonmandatory Information)

X1. SIGNIFICANCE OF PROPERTIES SPECIFIED FOR BIODIESEL FUEL

X1.1 Introduction X1.2 Flash Point

X1.1.1 The properties of commercial biodiesel fuel depends X1.2.1 The flash point, as specified, is not directly related to
upon the refining practices employed and the nature of the engine performance. It is, however, of importance in connec-
renewable lipids from which it is produced. Biodiesel, for tion with legal requirements and safety precautions involved in
example, can be produced from a variety of vegetable oils or fuel handling and storage that are normally specified to meet
animal fats which produce similar volatility characteristics and insurance and fire regulations.
combustion emissions with varying cold flow properties. X1.2.2 The flash point for biodiesel has been set at 93°C
X1.1.2 The significance of the properties in this appendix (200°F) minimum, so biodiesel falls under the non-hazardous
are based primarily on the commercial use of biodiesel in category under National Fire Protection Association codes.
on-road and off-road diesel engine applications. Some of the
properties may take on other significance if biodiesel is used as X1.3 Viscosity
a fuel or blending component in other applications. See the X1.3.1 For some engines it may be advantageous to specify
respective finished product specifications for additional infor- a minimum viscosity because of power loss due to injection
mation on significance of properties of those applications. pump and injector leakage. Maximum allowable viscosity, on

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 D 6751 – 09
the other hand, is limited by considerations involved in engine fuel under prescribed test conditions which generally relates to
design and size, and the characteristics of the injection system. the temperature at which crystals begin to precipitate from the
The upper limit for the viscosity of biodiesel (6.0 mm2/s at fuel in use. Biodiesel generally has a higher cloud point than
40°C) is higher than the maximum allowable viscosity in petroleum based diesel fuel. The cloud point of biodiesel and
Specification D 975 Grade 2-D and 2-D low sulfur (4.1 mm/s its impact on the cold flow properties of the resulting blend
at 40°C). Blending biodiesel with diesel fuel close to its upper should be monitored by the user to ensure trouble-free opera-
limit could result in a biodiesel blend with viscosity above the tion in cold climates. For further information, consult Appen-
upper limits contained in Specification D 975. dix X4 of Specification D 975.

X1.4 Sulfated Ash X1.9 Carbon Residue

X1.4.1 Ash-forming materials may be present in biodiesel X1.9.1 Carbon residue gives a measure of the carbon
in three forms: (1) abrasive solids, (2) soluble metallic soaps, depositing tendencies of a fuel oil. While not directly correlat-
and (3) unremoved catalysts. Abrasive solids and unremoved ing with engine deposits, this property is considered an
catalysts can contribute to injector, fuel pump, piston and ring approximation. Although biodiesel is in the distillate boiling
wear, and also to engine deposits. Soluble metallic soaps have range, most biodiesels boil at approximately the same tempera-
little effect on wear but may contribute to filter plugging and ture and it is difficult to leave a 10 % residual upon distillation.
engine deposits. Thus, a 100 % sample is used to replace the 10 % residual
sample, with the calculation executed as if it were the 10 %
X1.5 Sulfur residual. Parameter E (final weight flask charge/original weight
X1.5.1 The effect of sulfur content on engine wear and flask charge) in 8.1.2 of Test Method D 4530-93 is a constant
deposits appears to vary considerably in importance and 20/200.
depends largely on operating conditions. Fuel sulfur can also
affect emissions control systems performance and various X1.10 Acid Number
limits on sulfur have been imposed for environmental reasons. X1.10.1 The acid number is used to determine the level of
B100 is essentially sulfur-free. free fatty acids or processing acids that may be present in
NOTE X1.1—Test Method D 5453 should be used with biodiesel. Use of
biodiesel. Biodiesel with a high acid number has been shown to
other test methods may provide falsely high results when analyzing B100 increase fueling system deposits and may increase the likeli-
with extremely low sulfur levels (less than 5 ppm). Biodiesel sulfur hood for corrosion.
analysis from RR: D02-14808, Biodiesel Fuel Cetane Number Testing
NOTE X1.2—Acid number measures a different phenomenon for
Program, January-April, 1999, using Test Method D 2622 yielded falsely
biodiesel than petroleum based diesel fuel. The acid number for biodiesel
high results due to the presence of the oxygen in the biodiesel. Sulfur
measures free fatty acids or degradation by-products not found in
results using Test Method D 2622 were more accurate with B20 than with
petroleum based diesel fuel. Increased recycle temperatures in new fuel
B100 due to the lower oxygen content of B20. Potential improvements to
system designs may accelerate fuel degradation which could result in high
Test Method D 2622 may provide more accurate values in the future.
acid values and increased filter plugging potential.
X1.6 Copper Strip Corrosion
X1.11 Free Glycerin
X1.6.1 This test serves as a measure of possible difficulties
X1.11.1 The free glycerin method is used to determine the
with copper and brass or bronze parts of the fuel system. The
level of glycerin in the fuel. High levels of free glycerin can
presence of acids or sulfur-containing compounds can tarnish
cause injector deposits, as well as clogged fueling systems, and
the copper strip, thus indicating the possibility for corrosion.
result in a buildup of free glycerin in the bottom of storage and
X1.7 Cetane Number fueling systems.
X1.7.1 Cetane number is a measure of the ignition quality of X1.12 Total Glycerin
the fuel and influences white smoke and combustion rough-
X1.12.1 The total glycerin method is used to determine the
ness. The cetane number requirements depend on engine
level of glycerin in the fuel and includes the free glycerin and
design, size, nature of speed and load variations, and on
the glycerine portion of any unreacted or partially reacted oil or
starting and atmospheric conditions.
fat. Low levels of total glycerin ensure that high conversion of
X1.7.2 The calculated cetane index, Test Methods D 976 or
the oil or fat into its mono-alkyl esters has taken place. High
D 4737, may not be used to approximate the cetane number
levels of mono-, di-, and triglycerides can cause injector
with biodiesel or its blends. There is no substantiating data to
deposits and may adversely affect cold weather operation and
support the calculation of cetane index with biodiesel or
filter plugging.
biodiesel blends.
X1.13 Phosphorus Content
X1.8 Cloud Point
X1.13.1 Phosphorus can damage catalytic converters used
X1.8.1 Cloud point is of importance in that it defines the
in emissions control systems and its level must be kept low.
temperature at which a cloud or haze of crystals appears in the
Catalytic converters are becoming more common on diesel-
powered equipment as emissions standards are tightened, so
8
Supporting data have been filed at ASTM International Headquarters and may low phosphorus levels will be of increasing importance.
be obtained by requesting Research Report RR: D02–1480. Biodiesel produced from U.S. sources has been shown to have

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 D 6751 – 09
low phosphorus content (below 1 ppm) and the specification the flash point approaches 100°C, the flash point specification
value of 10 ppm maximum is not problematic. Biodiesel from has been set at 130°C minimum to ensure an actual value of
other sources may or may not contain higher levels of 100°C minimum. Improvements and alternatives to Test
phosphorus and this specification was added to ensure that all Method D 93 are being investigated. Once complete, the
biodiesel, regardless of the source, has low phosphorus con- specification of 100°C minimum may be reevaluated for
tent. alcohol control.
X1.14 Reduced Pressure Distillation X1.16 Calcium and Magnesium
X1.14.1 Biodiesel exhibits a boiling point rather than a X1.16.1 Calcium and magnesium may be present in biodie-
distillation curve. The fatty acids chains in the raw oils and fats sel as abrasive solids or soluble metallic soaps. Abrasive solids
from which biodiesel is produced are mainly comprised of can contribute to injector, fuel pump, piston, and ring wear, as
straight chain hydrocarbons with 16 to 18 carbons that have well as to engine deposits. Soluble metallic soaps have little
similar boiling temperatures. The atmospheric boiling point of effect on wear, but they may contribute to filter plugging and
biodiesel generally ranges from 330 to 357°C, thus the speci- engine deposits. High levels of calcium and magnesium
fication value of 360°C is not problematic. This specification compounds may also be collected in exhaust particulate
was incorporated as an added precaution to ensure the fuel has removal devices, are not typically removed during passive or
not been adulterated with high boiling contaminants. active regeneration, and can create increased back pressure and
NOTE X1.3—The density of biodiesel meeting the specifications in
reduced time to service maintenance.
Table 1 falls between 0.86 and 0.90, with typical values falling between X1.17 Sodium and Potassium
0.88 and 0.89. Since biodiesel density falls between 0.86 and 0.90, a
separate specification is not needed. The density of raw oils and fats is X1.17.1 Sodium and potassium may be present in biodiesel
similar to biodiesel, therefore use of density as an expedient check of fuel as abrasive solids or soluble metallic soaps. Abrasive solids can
quality may not be as useful for biodiesel as it is for petroleum based contribute to injector, fuel pump, piston and ring wear, and also
diesel fuel. This section has been added to provide users and engine to engine deposits. Soluble metallic soaps have little effect on
interests with this information. wear, but they may contribute to filter plugging and engine
NOTE X1.4—In certain items of fuel injection equipment in compres-
sion ignition engines, such as rotary/distributor fuel pumps and injectors,
deposits. High levels of sodium or potassium compounds may
the fuel functions as a lubricant as well as a source for combustion. also be collected in exhaust particulate removal devices, are
Blending biodiesel fuel with petroleum based compression-ignition fuel not typically removed during passive or active regeneration,
typically improves fuel lubricity. and they can create increased back pressure and reduced period
to service maintenance.
X1.15 Alcohol Control
X1.15.1 Alcohol control is to limit the level of unreacted X1.18 Oxidation Stability
alcohol remaining in the finished fuel. This can be measured X1.18.1 Products of oxidation in biodiesel can take the form
directly by the volume percent alcohol or indirectly through a of various acids or polymers, which, if in high enough
high flash point value. concentration, can cause fuel system deposits and lead to filter
X1.15.2 The flash point specification, when used for alcohol clogging and fuel system malfunctions. Additives designed to
control for biodiesel, is intended to be 100°C minimum, which retard the formation of acids and polymers can significantly
has been correlated to 0.2 vol % alcohol. Typical values are improve the oxidation stability performance of biodiesel. See
over 160°C. Due to high variability with Test Method D 93 as Appendix X2 for additional information on long-term storage.

X2. LONG-TERM STORAGE OF BIODIESEL

X2.1 Scope prolonged periods should be selected to avoid formation of

X2.1.1 This appendix provides guidance for consumers of sediments, high acid numbers, and high viscosities that can
biodiesel (B100) who may wish to store quantities of fuels for clog filters, affect fuel pump operation or plug combustor
extended periods. Consistently successful long-term fuel stor- nozzles or injectors. The selection of biodiesel should result
age requires attention to fuel selection, storage conditions, and from supplier-user discussions.
monitoring of properties prior to and during storage. This X2.1.3 These suggested practices are general in nature and
appendix is directed toward biodiesel (B100) and may be more should not be considered substitutes for any requirement
or less applicable to blends of biodiesel with petroleum based imposed by the warranty of the distillate fuel equipment
diesel fuel. manufacturers or by federal, state, or local government regu-
X2.1.2 Normally produced biodiesel has adequate stability lations. Although they cannot replace knowledge of local
properties to withstand normal storage without the formation of conditions or good engineering and scientific judgment, these
troublesome amounts of insoluble degradation products, al- suggested practices do provide guidance in developing an
though data suggests some biodiesel may degrade faster than individual fuel management system for the biodiesel fuel user.
petroleum based diesel fuel. Biodiesel that is to be stored for They include suggestions in the operation and maintenance of

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 D 6751 – 09
existing fuel storage and handling facilities and for identifying lation of this test with actual storage stability is unknown, and
where, when, and how fuel quality should be monitored. may depend upon field conditions and fuel composition.
X2.5.2 Performance criteria for accelerated stability tests
X2.2 Terminology that ensure satisfactory long-term storage of biodiesel (B100)
X2.2.1 bulk fuel—fuel in the storage facility in quantities have not been established.
over 50 gallons.
X2.2.2 combustor fuel—fuel entering the combustion zone X2.6 Fuel Monitoring
of the burner or engine after filtration or other treatment of bulk X2.6.1 A plan for monitoring the quality of bulk fuel during
fuel. prolonged storage is an integral part of a successful monitoring
X2.2.3 fuel contaminants—foreign materials that make fuel program. A plan to replace aged fuel with fresh product at
less suitable or unsuitable for the intended use. Fuel contami- established intervals is also desirable.
nants include materials introduced subsequent to the manufac- X2.6.2 Stored fuel should be periodically sampled and its
ture of fuel and fuel degradation products. quality assessed. Practice D 4057 provides guidance for sam-
X2.2.4 fuel-degradation products—those materials formed pling. Fuel contaminants and degradation products may settle
in fuel after it is produced. Insoluble degradation products may to the bottom of a quiescent tank although detrimental changes
combine with other fuel contaminants to reinforce deleterious to biodiesel can occur (rising acid value) without causing
effects. Soluble degradation products (acids and gums) may be sediment formation. A Bottom or Clearance sample, as defined
more or less volatile than the fuel and may cause an increase in in Practice D 4057, should be included in the evaluation along
injector and nozzle deposits. The formation of degradation with an All Level sample.
products may be catalyzed by contact with metals, especially X2.6.3 The quantity of insoluble fuel contaminants present
those containing copper and, to a lesser extent, iron. in biodiesel can be determined using Test Method D 6217 with
X2.2.5 long-term storage—storage of fuel for longer than 6 glass fiber filters and abundant washing although no precision
months after it is received by the user. or bias testing has been performed with biodiesel using Test
Method D 6217.
X2.3 Fuel Selection X2.6.4 The acid value of biodiesel appears to exceed its
X2.3.1 The stability properties of biodiesel are not fully specified maximum before other deleterious fuel property
understood and appear to depend on the vegetable oil and changes occur. A conscientious program of measuring the acid
animal fat sources, severity of processing, and whether addi- value of biodiesel may be sufficient for monitoring biodiesel
tional production plant treatment has been carried out or stability.
stability additives are present.
X2.3.2 The composition and stability properties of biodiesel X2.7 Fuel Storage Conditions
produced at specific production plants may be different. Any X2.7.1 Contamination levels in fuel can be reduced by
special requirements of the user, such as long-term storage, storage in tanks kept free of water, and tankage should have
should be discussed with the supplier. provisions for water draining on a scheduled basis. Water
promotes corrosion, and microbiological growth may occur at
X2.4 Fuel Additives a fuel-water interface. Refer to Guide D 6469 for a more
X2.4.1 Available fuel additives appear to improve the long complete discussion. Underground or isothermal storage is
term storage of biodiesel. Most additives should be added as preferred to avoid temperature extremes; above-ground storage
close to the production site as possible to obtain maximum tanks should be sheltered or painted with reflective paint. High
benefits. storage temperatures accelerate fuel degradation. Fixed roof
X2.4.2 Biocides or biostats destroy or inhibit the growth of tanks should be kept full to limit oxygen supply and tank
fungi and bacteria which can grow at fuel-water interfaces to breathing. The use of airtight sealed containers, such as drums
give high particulate concentrations in the fuel. Available or totes, can enhance the storage life of biodiesel.
biocides are soluble in the fuel phase or the water phase, or X2.7.2 Copper and copper-containing alloys should be
both. Refer to Guide D 6469 for a more complete discussion. avoided with biodiesel due to increased sediment and deposit
formation. Contact with lead, tin, and zinc can also cause
X2.5 Tests for Fuel Quality increased sediment levels that can rapidly plug filters and
X2.5.1 Test methods for estimating the storage stability of should be avoided.
biodiesel (B100) are being developed. Modifications of Test X2.7.3 Appendix X3 of Specification D 2880 discusses fuel
Method D 2274 to use glass fiber filters, varying times and contaminants as a general topic. The discussion in Specifica-
temperatures, and the measurement of pre-test and post-test tion D 2880 pertains to gas turbine combustion which may or
acid number and viscosity appear promising. However, corre- may not be applicable to diesel engine combustion.

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SUMMARY OF CHANGES

Subcommittee D02.E0 has identified the location of selected changes to this standard since the last issue
(D 6751–08) that may impact the use of this standard. (Approved April 15, 2009.)

(1) Added Test Method D 7397 cloud point as an option to

Test Method D 2500 in 5.1.9 and to the Referenced
Documents.

Subcommittee D02.E0 has identified the location of selected changes to this standard since the last issue
(D 6751–07b´1) that may impact the use of this standard. (Approved Oct. 1, 2008.)

(1) Added Annex A1. (3) Added 5.1.18.

(2) Revised Table 1. (4) Added Note 4.

Subcommittee D02.E0 has identified the location of selected changes to this standard since the last issue
(D 6751–07a) that may impact the use of this standard. (Approved Sept. 15, 2007.)

(1) Added Test Method D 6890 to Referenced Documents and (3) Revised 1.2.
5.1.8.
(2) Added Test Method D 7039 to Referenced Documents and
5.1.6.

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