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Designation: D 7467 – 09

Standard Specification for


Diesel Fuel Oil, Biodiesel Blend (B6 to B20)1
This standard is issued under the fixed designation D 7467; 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* 2. Referenced Documents


1.1 This specification covers fuel blend grades of 6 to 20 2.1 ASTM Standards:2
volume percent (%) biodiesel with the remainder being a light D 56 Test Method for Flash Point by Tag Closed Cup Tester
middle or middle distillate diesel fuel, collectively designated D 86 Test Method for Distillation of Petroleum Products at
as B6 to B20. These grades are suitable for various types of Atmospheric Pressure
diesel engines. D 93 Test Methods for Flash Point by Pensky-Martens
1.1.1 The biodiesel component of the blend shall conform to Closed Cup Tester
the requirements of Specification D 6751. The remainder of the D 129 Test Method for Sulfur in Petroleum Products (Gen-
fuel shall be a light middle or middle distillate grade diesel fuel eral Bomb Method)
conforming to Specification D 975 grades No. 1-D and No. D 130 Test Method for Corrosiveness to Copper from
2-D of any sulfur level specified with the following exceptions. Petroleum Products by Copper Strip Test
The light middle or middle distillate grade diesel fuel whose D 445 Test Method for Kinematic Viscosity of Transparent
sulfur level, aromatic level, cetane, or lubricity falls outside of and Opaque Liquids (and Calculation of Dynamic Viscos-
Specification D 975 may be blended with biodiesel meeting ity)
Specification D 6751, provided the finished mixtures meets this D 482 Test Method for Ash from Petroleum Products
specification. D 524 Test Method for Ramsbottom Carbon Residue of
1.1.2 The fuel sulfur grades are described as follows: Petroleum Products
1.1.2.1 Grade B6 to B20 S15—A fuel with a maximum of D 613 Test Method for Cetane Number of Diesel Fuel Oil
15 ppm sulfur. D 664 Test Method for Acid Number of Petroleum Products
1.1.2.2 Grade B6 to B20 S500—A fuel with a maximum of by Potentiometric Titration
500 ppm sulfur. D 975 Specification for Diesel Fuel Oils
1.1.2.3 Grade B6 to B20 S5000—A fuel with a maximum of D 976 Test Method for Calculated Cetane Index of Distil-
5000 ppm sulfur. late Fuels
1.2 This specification prescribes the required properties of D 1266 Test Method for Sulfur in Petroleum Products
B6 to B20 biodiesel blends at the time and place of delivery. (Lamp Method)
The specification requirements may be applied at other points D 1319 Test Method for Hydrocarbon Types in Liquid
in the production and distribution system when provided by Petroleum Products by Fluorescent Indicator Adsorption
agreement between the purchaser and the supplier. D 1552 Test Method for Sulfur in Petroleum Products
1.2.1 Nothing in this specification shall preclude observance (High-Temperature Method)
of federal, state, or local regulations that may be more D 2500 Test Method for Cloud Point of Petroleum Products
restrictive. D 2622 Test Method for Sulfur in Petroleum Products by
NOTE 1—The generation and dissipation of static electricity can create
Wavelength Dispersive X-ray Fluorescence Spectrometry
problems in the handling of distillate diesel fuel oils. For more informa- D 2709 Test Method for Water and Sediment in Middle
tion on this subject, see Guide D 4865. Distillate Fuels by Centrifuge
D 2880 Specification for Gas Turbine Fuel Oils
1.3 The values stated in SI units are to be regarded as
D 3117 Test Method for Wax Appearance Point of Distillate
standard. No other units of measurement are included in this
Fuels
standard.
D 3120 Test Method for Trace Quantities of Sulfur in Light
1
This specification is under the jurisdiction of ASTM Committee D02 on
2
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D02.E0 on Burner, Diesel, Non-Aviation Gas Turbine, and Marine Fuels. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved March 1, 2009. Published March 2009. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 2008. Last previous edition approved in 2008 as D 7467–08. the ASTM website.

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


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D 7467 – 09
Liquid Petroleum Hydrocarbons by Oxidative Microcou- 3. Terminology
lometry 3.1 Definitions:
D 3828 Test Methods for Flash Point by Small Scale Closed
3.2 biodiesel, n—fuel comprised of mono-alkyl esters of
Cup Tester
long chain fatty acids derived from vegetable oils or animal
D 4057 Practice for Manual Sampling of Petroleum and
fats, designated B100.
Petroleum Products
D 4294 Test Method for Sulfur in Petroleum and Petroleum 3.3 B6 to B20, n—fuel blend consisting of 6 to 20 volume
Products by Energy Dispersive X-ray Fluorescence Spec- percent biodiesel conforming to the requirements of Specifi-
trometry cation D 6751 with the remainder being a light middle or
D 4539 Test Method for Filterability of Diesel Fuels by middle distillate grade diesel fuel and meeting the requirements
Low-Temperature Flow Test (LTFT) of this specification.
D 4737 Test Method for Calculated Cetane Index by Four 3.3.1 Discussion—The abbreviation BXX represents a spe-
Variable Equation cific blend concentration in the range B6 to B20, where XX is
D 4865 Guide for Generation and Dissipation of Static the percent volume of biodiesel in the fuel blend.
Electricity in Petroleum Fuel Systems 3.4 S(numerical specification maximum)—indicates the
D 5453 Test Method for Determination of Total Sulfur in maximum sulfur content, in weight ppm (µg/g), allowed by this
Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel specification.
Engine Fuel, and Engine Oil by Ultraviolet Fluorescence
D 5771 Test Method for Cloud Point of Petroleum Products 4. Test Methods
(Optical Detection Stepped Cooling Method) 4.1 The requirements enumerated in this specification shall
D 5772 Test Method for Cloud Point of Petroleum Products be determined in accordance with the following methods:
(Linear Cooling Rate Method) 4.1.1 Acid Number—Test Method D 664.
D 5773 Test Method for Cloud Point of Petroleum Products
4.1.2 Flash Point—Test Method D 93, except where other
(Constant Cooling Rate Method)
methods are prescribed by law. Test Method D 3828 may be
D 6079 Test Method for Evaluating Lubricity of Diesel
used as an alternate with the same limits. Test Method D 56
Fuels by the High-Frequency Reciprocating Rig (HFRR)
may be used as an alternate with the same limits, provided the
D 6217 Test Method for Particulate Contamination in
flash point is below 93°C. This test method will give slightly
Middle Distillate Fuels by Laboratory Filtration
lower values. In cases of dispute, Test Method D 93 shall be
D 6371 Test Method for Cold Filter Plugging Point of
used as the referee method.
Diesel and Heating Fuels
D 6468 Test Method for High Temperature Stability of 4.1.3 Cloud Point—Test Method D 2500. For all B6 to B20
Middle Distillate Fuels grades in Table 1 the automatic Test Methods D 5771, D 5772,
D 6469 Guide for Microbial Contamination in Fuels and or D 5773 can be used as alternates with the same limits. Test
Fuel Systems Method D 3117 can also be used since it is closely related to
D 6751 Specification for Biodiesel Fuel Blend Stock Test Method D 2500. In case of dispute, Test Method D 2500
(B100) for Middle Distillate Fuels shall be the referee test method.
D 6890 Test Method for Determination of Ignition Delay 4.1.4 Cold Filter Plugging Point (CFPP)—Test Method
and Derived Cetane Number (DCN) of Diesel Fuel Oils by D 6371.
Combustion in a Constant Volume Chamber 4.1.5 Low Temperature Flow Test (LTFT)—Test Method
D 7371 Test Method for Determination of Biodiesel (Fatty D 4539.
Acid Methyl Esters) Content in Diesel Fuel Oil Using Mid 4.1.6 Water and Sediment—Test Method D 2709.
Infrared Spectroscopy (FTIR-ATR-PLS Method) 4.1.7 Carbon Residue—Test Method D 524.
E 29 Practice for Using Significant Digits in Test Data to 4.1.8 Ash—Test Method D 482.
Determine Conformance with Specifications 4.1.9 Distillation—Test Method D 86.
2.2 Other Standards:
4.1.10 Viscosity—Test Method D 445.
26 CFR Part 48 Manufacturers and Retailers Excise Taxes3
40 CFR Part 80 Regulation of Fuels and Fuel Additives3 4.1.11 Sulfur—Table 2 shows the referee test methods and
EN 14078 Liquid petroleum products - Determination of alternate test methods for sulfur, the range over which each test
fatty acid methyl ester (FAME) content in middle distil- method applies and the corresponding fuel grades.
lates - Infrared spectrometry method4 4.1.12 Aromaticity—Test Method D 1319. This test method
EN 14112 Fat and oil derivatives - Fatty acid methyl esters provides an indication of the aromatic content of fuels. For
(FAME) - Determination of oxidation stability (Acceler- fuels with a maximum final boiling point of 315°C, this test
ated oxidation test)4 method is a measurement of the aromatic content of the fuel.
Grade S5000 does not have an aromatics content.
4.1.13 Cetane Index—Test Method D 976.
3
Available from U.S. Government Printing Office Superintendent of Documents, 4.1.14 Lubricity—Test Method D 6079.
732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401.
4
Available from the National CEN members listed on the CEN website 4.1.15 Copper Corrosion—Test Method D 130, 3 h test at
(www.cenorm.be.) or from the CEN/TC 19 Secretariat (astm@nen.nl). 50°C minimum.

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D 7467 – 09
TABLE 1 Detailed Requirements for B6 to B20 Biodiesel Blends
Grade
Property Test Method
B6 to B20 S15 B6 to B20 S500A B6 to B20 S5000B
Acid Number, mg KOH/g, max D 664 0.3 0.3 0.3
Viscosity, mm2/s at 40°C D 445 1.9-4.1C 1.9-4.1C 1.9- 4.1C
Flash Point, °C, min D 93 52D 52D 52D
E E E
Cloud Point, °C, max or LTFT/CFPP, °C, max D 2500, D 4539, D 6371
Sulfur Content, (µg/g) D 5453 15 ... ...
mass %, max D 2622 ... 0.05 ...
mass %, max D 129 ... ... 0.50
Distillation Temperature, °C, 90% vol recovered, max D 86 343 343 343
Ramsbottom Carbon Residue on 10% bottoms, mass %, max D 524 0.35 0.35 0.35
Cetane Number, min D 613F 40G 40G 40G
One of the following must be met: D 976-80H 40 40 40
(1) Cetane index, min.
(2) Aromaticity, %vol, max D 1319-03H 35 35 ...
Ash Content, mass%, max D 482 0.01 0.01 0.01
Water and Sediment, volume%, max D 2709 0.05 0.05 0.05
Copper Corrosion, 3 h at 50°C, max D 130 No. 3 No. 3 No. 3
Biodiesel Content, % (V/V) D 7371 6. - 20. 6. - 20. 6. - 20.
Oxidation Stability, hours, min EN 14112 6 6 6
Lubricity, HFRR at 60°C, micron (µm), max D 6079 520I 520I 520I
A
Under United States of America regulations, if Grades B6-20 S500 are sold for tax exempt purposes then, at, or beyond terminal storage tanks, they are required by
26 CFR Part 48 to contain the dye Solvent Red 164 at a concentration spectrally equivalent to 3.9 lb per thousand barrels of the solid dye standard Solvent Red 164, or
the tax must be collected.
B
Under United States of America regulations, Grades B6-20 S5000 are required by 40 CFR part 80 to contain a sufficient amount of the dye Solvent Red 164 so its
presence is visually apparent. At or beyond terminal storage tanks, they are required by 26 CFR Part 48 to contain the dye Solvent Red 164 at a concentration spectrally
equivalent to 3.9 lb per thousand barrels of the solid dye standard Solvent Red 26.
C
If Grade No. 1-D or blends of Grade No. 1-D and Grade No. 2-D diesel fuel are used, the minimum viscosity shall be 1.3 mm2/s.
D
If Grade No. 1-D or blends of Grade No. 1-D and Grade No. 2-D diesel fuel are used, or a cloud point of less than -12°C is specified, the minimum flash point shall
be 38°C.
E
It is unrealistic to specify low temperature properties that will ensure satisfactory operation at all ambient conditions. In general, cloud point (or wax appearance point)
Low Temperature Flow Test, and Cold Filter Plugging Point Test may be useful to estimate vehicle low temperature operability limits but their use with B6 to B20 has not
been validated. However, satisfactory operation below the cloud point (or wax appearance point) may be achieved depending on equipment design, operating conditions,
and the use of flow-improver additives as described in X3.1.2. Appropriate low temperature operability properties should be agreed upon between the fuel supplier and
purchaser for the intended use and expected ambient temperatures. Test Methods D 4539 and D 6371 may be especially useful to estimate vehicle low temperature
operability limits when flow improvers are used but their use with B6 to B20 from a full range of biodiesel feedstock sources has not been validated. Due to fuel delivery
system, engine design, and test method differences, low temperature operability tests may not provide the same degree of protection in various vehicle operating classes.
Tenth percentile minimum air temperatures for U.S. locations are provided in Appendix X3 as a means of estimating expected regional temperatures. The tenth percentile
minimum air temperatures may be used to estimate expected regional target temperatures for use with Test Methods D 2500, D 4539, and D 6371. Refer to X3.1.3 for
further general guidance on test application.
F
Calculated cetane index approximation, Test Method D 4737, is not applicable to biodiesel blends.
G
Low ambient temperatures, as well as engine operation at high altitudes, may require the use of fuels with higher cetane ratings. If the diesel fuel is qualified under
Table 1 of Specification D 975 for cetane, it is not necessary to measure the cetane number of the blend. This is because the cetane number of the individual blend
components will be at least 40, so the resulting blend will also be at least 40 cetane number.
H
These test methods are specified in 40 CFR Part 80.
I
If the diesel fuel is qualified under Table 1 of Specification D 975 for lubricity, it is not necessary to measure the lubricity of the blend. This is because the lubricity of
the individual blend components will be less than 520 micron (µm) so the resulting blend will also be less than 520 (µm).

TABLE 2 Sulfur Test Methods


Sulfur Test Method Range Grades Units Used to Report ResultsA
D 129 >0.1 mass % S5000 mass %
(referee)
D 1266 0.0005 to 0.4 mass % S500 mass %
5 to 4000 mg/kg (wt ppm)
D 1552 >0.06 mass % S5000 mass %
D 2622 0.0003 to 5.3 mass % all grades mass %
(referee for S500 grades) 3 to 53 000 mg/kg (wt ppm)
D 3120 3.0 to 100 mg/kg (wt ppm) S15, S500 ppm (µg/g)
(S500 grades must be diluted before testing)
D 4294 0.0150 to 5.00 mass % S5000 mass %
150 to 50 000 mg/kg (wt ppm)
D 5453 0.0001 to 0.8 mass % all grades ppm (µg/g)
(referee for S15 grades) 1.0 to 8000 mg/kg (wt ppm)
A
Results reported in mg/kg and in ppm (µg/g) are numerically the same. The units used in Table 1 for the sulfur requirements are the units in which results for the referee
test are reported.

4.1.17 Oxidation Stability—Test Method EN 14112. The


4.1.16 Cetane Number—Test Method D 613. Test Method subcommittee is aware of potential issues in the current version
D 6890 may also be used. In cases of dispute, Test Method when used for biodiesel blends. This standard is being revised
D 613 shall be the referee test method. to resolve these issues. See X1.16.2 for further information.

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D 7467 – 09
4.1.18 Biodiesel Content—Test Method D 7371. Test 6. Requirements
Method EN 14078 may also be used. In cases of dispute, Test
6.1 The biodiesel blend (B6 to B20) specified shall conform
Method D 7371 shall be the referee test method. See Practice
to the detailed requirements shown in Table 1.
E 29 for guidance on significant digits.
5. Workmanship 7. Keywords
5.1 The biodiesel blend (B6 to B20) shall be visually free of 7.1 biodiesel; biodiesel blend; diesel; fuel oil; petroleum
undissolved water, sediment, and suspended matter. and petroleum products
5.2 The biodiesel blend (B6 to B20) shall also be free of any
adulterant or contaminant that may render the fuel unaccept-
able for its commonly used applications.

APPENDIXES

(Nonmandatory Information)

X1. SIGNIFICANCE OF ASTM SPECIFICATION FOR B6 to B20 BIODIESEL BLENDS

X1.1 Introduction hand, is limited by considerations involved in engine design


X1.1.1 The properties of commercial B6 to B20 blends and size, and the characteristics of the injection system.
depend on the refining practices employed and the nature of the X1.5 Carbon Residue
distillate fuel oils and biodiesel from which they are produced.
Distillate fuel oils, for example, may be produced within the X1.5.1 Carbon residue gives a measure of the carbon
boiling range of 150 and 400°C having many possible combi- depositing tendencies of a fuel oil when heated in a bulb under
nations of various properties, such as volatility, ignition qual- prescribed conditions. While not directly correlating with
ity, viscosity, and other characteristics. Biodiesel, for example, engine deposits, this property is considered an approximation.
can be produced from a variety of animal fats or vegetable oils X1.6 Sulfur
that produce similar volatility characteristics and combustion
X1.6.1 The effect of sulfur content on engine wear and
emissions with varying cold flow properties.
deposits appears to vary considerably in importance and
depends largely on operating conditions. Fuel sulfur can affect
X1.2 Cetane Number
emission control systems performance. To ensure maximum
X1.2.1 Cetane number is a measure of the ignition quality of availability of fuels, the permissible sulfur content should be
the fuel and influences combustion roughness. The cetane specified as high as is practicable, consistent with maintenance
number requirements depend on engine design, size, nature of considerations and legal limits.
speed and load variations, and on starting and atmospheric
conditions. Increase in cetane number over values actually X1.7 Flash Point
required does not materially improve engine performance. X1.7.1 The flash point as specified is not directly related to
Accordingly, the cetane number specified should be as low as engine performance. It is, however, of importance in connec-
possible to ensure maximum fuel availability. tion with legal requirements and safety precautions involved in
fuel handling and storage, and it is normally specified to meet
X1.3 Distillation insurance and fire regulations.
X1.3.1 The fuel volatility requirements depend on engine X1.8 Cloud Point
design, size, nature of speed and load variations, and starting
X1.8.1 Cloud point is of importance in that it defines the
and atmospheric conditions. For engines in services involving
temperature at which a cloud or haze of wax crystals appears
rapidly fluctuating loads and speeds, as in bus and truck
in the oil under prescribed test conditions that generally relates
operation, the more volatile fuels may provide best perfor-
to the temperature at which wax crystals begin to precipitate
mance, particularly with respect to smoke and odor. The
from the oil in use.
biodiesel portion of the B6 to B20 may also provide smoke and
odor improvements. However, best fuel economy is generally X1.9 Ash
obtained from the heavier types of fuels because of their higher X1.9.1 Ash-forming materials may be present in fuel oil in
heat content. three forms: (1) abrasive solids, (2) soluble metallic soaps, and
(3) unremoved biodiesel catalysts. Abrasive solids and unre-
X1.4 Viscosity moved biodiesel catalysts contribute to injector, fuel pump,
X1.4.1 For some engines it is advantageous to specify a piston and ring wear, and also to engine deposits. Soluble
minimum viscosity because of power loss due to injection metallic soaps have little effect on wear but may contribute to
pump and injector leakage. Maximum viscosity, on the other engine deposits and filter clogging.

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D 7467 – 09
X1.10 Copper Strip Corrosion materials from petroleum based diesel fuel. Based on this, a
X1.10.1 This test serves as a measure of possible difficulties specification for finished blends for these compounds has not
with copper and brass or bronze parts of the fuel system. been established. If measured, the level of these materials
should not exceed the maximum contribution derived from
X1.11 Aromaticity biodiesel based on the blend content and the maximum level
X1.11.1 This test is used as an indication of the aromatics allowed in Specification D 6751 and the contribution of the
content of diesel fuel. Aromatics content is specified to prevent petroleum based diesel fuel.
an increase in the average aromatics content in diesel fuels. X1.15 Other
Increases in aromatics content of fuels over current levels may
have a negative impact on emissions. Use of Test Method X1.15.1 Microbial Contamination:
D 1319-03 or cetane index, Test Method D 976-80, is required X1.15.1.1 Uncontrolled microbial contamination in fuel
in the United States of America by 40 CFR Part 80. The systems can cause or contribute to a variety of problems,
precision and bias of Test Method D 1319-03 with biodiesel including increased corrosivity and decreased stability, filter-
blends is not known and is currently under investigation. ability, and caloric value. Microbial processes in fuel systems
can also cause or contribute to system damage.
X1.12 Cetane Index X1.15.1.2 Because the microbes contributing to the afore-
X1.12.1 Cetane index is specified as a limitation on the mentioned problems are not necessarily present in the fuel
amount of high aromatic components in S15 and S500 Grades. itself, no microbial quality criterion for fuels is recommended.
Use of Test Method D 1319-03 or cetane index, Test Method However, it is important that personnel responsible for fuel
D 976-80, is required in the United States of America by 40 quality understand how uncontrolled microbial contamination
CFR Part 80. The precision and bias of Test Method D 976-80 can affect fuel quality.
with biodiesel blends is not known. X1.15.1.3 Guide D 6469 provides personnel with limited
microbiological background an understanding of the symp-
X1.13 Total and Free Glycerin toms, occurrences, and consequences of microbial contamina-
tion. Guide D 6469 also suggests means for detecting and
X1.13.1 High levels of total or free glycerin can cause
controlling microbial contamination in fuels and fuel systems.
injector deposits and may adversely affect cold weather opera-
Good housekeeping, especially keeping fuel dry, is critical.
tion and filter plugging and result in a buildup of material in the
bottom of storage and fueling systems. The total and free X1.16 Oxidation Stability
glycerin levels are controlled by Specification D 6751 to 0.24% X1.16.1 If the biodiesel is qualified under Table 1 of Speci-
mass maximum and 0.02% mass maximum, respectively. fication D 6751 for oxidation stability, it may not be necessary
Diesel fuel contains no total or free glycerin, so the level of to measure the oxidation stability of the blend. Existing data5
total and free glycerin in a biodiesel blend is solely derived indicates the oxidation stability of B6 to B20 should be over 6
from the biodiesel contribution and is extremely low and in h if the oxidation stability of the biodiesel is 3 h or higher at the
direct proportion to the level of biodiesel added and its total time of blending.
and free glycerin values. In finished blends, the ability to X1.16.2 Special precautions may be necessary to eliminate
measure total and free glycerin is compromised by interference falsely low readings using EN 14112 with biodiesel blends.
with naturally occurring petroleum diesel fuel components and The petroleum portion of the blend may affect tubing between
the extremely low values. No ASTM test methods for measur- the reaction vessel and the measuring vessel and the plastic seal
ing total and free glycerin in blends currently exist, so no on the top of the reaction vessel or condense in various parts of
specification for the finished B6 to B20 blend is included. If the test setup. Some of these parts may need to be replaced
test methods become available, the level of total and free frequently, and all components should be thoroughly cleaned to
glycerin should not exceed the maximum contribution derived prevent falsely low readings. Improvements to these parts and
from biodiesel based on the blend content and the maximum potential changes in the test method are currently being
level allowed in Specification D 6751. evaluated.
X1.14 Calcium and Magnesium, Sodium and Potassium, X1.17 Acid Number
and Phosphorus Content
X1.17.1 The acid number is used to determine the level of
X1.14.1 Calcium and magnesium combined and sodium free fatty acids or processing acids that may be present in the
and potassium combined are controlled to 5 ppm maximum in biodiesel or diesel fuel oil when produced, or those which form
Specification D 6751. Phosphorus is controlled to 10 ppm upon aging. Biodiesel blends with a high acid number have
maximum in Specification D 6751. The presence of high levels been shown to increase fueling system deposits and may
of these elements could adversely affect exhaust catalysts and increase the likelihood for corrosion.
after-treatment systems. The concentration of these materials
due to biodiesel in a B6 to B20 blends should be less than 1 or 5
McCormick, R. L., and Westbrook, S. R., “Empirical Study of the Stability of
2 ppm, making accurate measurement difficult. There are also
Biodiesel and Biodiesel Blends, Milestone Report,” NREL/TP-540-41619, National
no controls for these materials in Specification D 975 at present Renewable Energy Laboratory, Golden, Colorado, May 2007. http://www.nrel.gov/
and no available database for the potential contribution of these docs/fy07osti/41619.pdf.

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D 7467 – 09

X2. STORAGE AND THERMAL STABILITY OF B6 TO B20 BLENDS

X2.1 Scope X2.2.5 severe use—use of the fuel in applications which


X2.1.1 This appendix provides guidance for consumers of may result in engines operating under high load conditions that
B6 to B20 who may wish to store quantities of fuels for may cause the fuel to be exposed to excessive heat.
extended periods or use the fuel in severe service or high
temperature applications. Fuels containing residual compo- X2.3 Fuel Selection
nents are excluded. Consistently successful long-term fuel X2.3.1 Certain distilled refinery and biodiesel products are
storage or use in severe applications requires attention to fuel generally more suitable for long-term storage and severe
selection, storage conditions, handling and monitoring of service than others. The stability properties of B6 to B20
properties during storage and prior to use. blends are highly dependent on the crude oil sources, severity
X2.1.2 Normally produced fuels have adequate stability of processing, use of additives and whether additional refinery
properties to withstand normal storage and use without the treatment has been carried out.
formation of troublesome amounts of insoluble degradation X2.3.2 The composition and stability properties of B6 to
products although data suggests some B6 to B20 blends may B20 produced at specific refineries or blending locations may
degrade faster than petrodiesel. Fuels that are to be stored for be different. Any special requirements of the user, such as
prolonged periods or used in severe applications should be long-term storage or severe service, should be discussed with
selected to avoid formation of sediments or gums, high acid the supplier.
numbers, or high viscosity which can overload filters or plug X2.3.3 Blends of fuels from various sources may interact to
injectors. Selection of these fuels should result from supplier- give stability properties worse than expected based on the
user discussions. characteristics of the individual fuels.
X2.1.3 These suggested practices are general in nature and
should not be considered substitutes for any requirements X2.4 Fuel Additives
imposed by the warranty of the distillate fuel equipment X2.4.1 Available fuel additives can improve the suitability
manufacturer or by federal, state, or local government regula- of marginal fuels for long-term storage and thermal stability,
tions. Although they cannot replace a knowledge of local but may be unsuccessful for fuels with markedly poor stability
conditions or good engineering and scientific judgment, these properties. Most additives should be added at the refinery or
suggested practices do provide guidance in developing an during the early weeks of storage to obtain maximum benefits.
individual fuel management system for the B6 to B20 fuel user. X2.4.2 Biocides or biostats destroy or inhibit the growth of
They include suggestions in the operation and maintenance of fungi and bacteria, which can grow at fuel-water interfaces to
existing fuel storage and handling facilities and for identifying give high particulate concentrations in the fuel. Available
where, when, and how fuel quality should be monitored or biocides are soluble in both the fuel and water or in the water
selected for storage or severe use. phase only.

X2.2 Definitions X2.5 Tests for Fuel Quality


X2.2.1 bulk fuel—fuel in the storage facility in quantities X2.5.1 At the time of manufacture, the storage stability of
over 50 gal. B6 to B20 may be assessed using Test Method EN 14112.
X2.2.2 fuel contaminants—foreign materials that make fuel Other tests methods are under development. However, these
less suitable or unsuitable for the intended use. accelerated stability tests may not correlate well with field
X2.2.2.1 Discussion storage stability due to varying field conditions and to fuel
Fuel contaminants include materials introduced subsequent composition.
to the manufacture of fuel and fuel degradation products. X2.5.2 Performance criteria for accelerated stability tests
X2.2.3 fuel-degradation products—those materials that are that ensure satisfactory long-term storage of fuels have not
formed in fuel during extended storage or exposure to high been established.
temperatures. X2.5.3 Test Method D 6468 provides an indication of ther-
X2.2.3.1 Discussion—Insoluble degradation products may mal oxidative stability of middle distillate fuels when heated to
combine with other fuel contaminants to reinforce deleterious temperatures near 150°C.
effects. Soluble degradation products (soluble gums) are less
volatile than fuel and may carbonize to form deposits due to X2.6 Fuel Monitoring
complex interactions and oxidation of small amounts of X2.6.1 A plan for monitoring the quality of bulk fuel during
olefinic or sulfur-, oxygen-, or nitrogen-contaminating com- prolonged storage is an integral part of a successful program. A
pounds present in fuels. The formation of degradation products plan to replace aged fuel with fresh product at established
may be catalyzed by dissolved metals, especially copper salts. intervals is also desirable.
When dissolved copper is present it can be deactivated with X2.6.2 Stored fuel should be periodically sampled and its
metal deactivator additives. quality assessed. Practice D 4057 provides guidance for sam-
X2.2.4 long-term storage—storage of fuel for longer than 6 pling. Fuel contaminants and degradation products will usually
months after it is received by the user. settle to the bottom of a quiescent tank. A “Bottom” or

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D 7467 – 09
“Clearance” sample, as defined in Practice D 4057, should be X2.8.2 Inadequate high temperature stability may result in
included in the evaluation along with an “All Level” sample. the formation of insoluble degradation products.
X2.6.3 The quantity of insoluble fuel contaminants present
in fuel can be determined using Test Method D 6217 although X2.9 Use of Degraded Fuels
no precision or bias testing has been performed with B6 to B20 X2.9.1 Fuels that have undergone mild-to-moderate degra-
blends. dation can sometimes be consumed in a normal way, depend-
X2.6.4 Test Method D 6468 can be used for investigation of ing on the fuel system requirements. Filters and other cleanup
operational problems that might be related to fuel thermal equipment can require special attention and increased mainte-
stability. Testing samples from the fuel tank or from bulk nance. Burner nozzle or injector fouling can occur more
storage may give an indication as to the cause of filter rapidly.
plugging. It is more difficult to monitor the quality of fuels in X2.9.2 Fuels containing very large quantities of fuel degra-
vehicle tanks since operation may be on fuels from multiple dation products and other contaminants or with runaway
sources. microbiological growth require special attention. Consultation
X2.6.5 Some additives exhibit effects on fuels tested in with experts in this area is desirable. It can be possible to drain
accordance with Test Method D 6468 that may or may not be the sediment or draw off most of the fuel above the sediment
observed in the field. Data have not been developed that layer and use it with the precautions described in X2.9.1.
correlate results from the test method for various engine types However, very high soluble gum levels or corrosion products
and levels of operating severity. from microbiological contamination can cause severe opera-
X2.6.6 Ongoing monitoring of the acid number is a useful tional problems.
means of monitoring oxidation or degradation of biodiesel
X2.10 Thermal Stability Guidelines
blends.
X2.10.1 Results from truck fleet experience suggests that
X2.7 Fuel Storage Conditions Test Method D 6468 can be used to qualitatively indicate
X2.7.1 Contamination levels in fuel can be reduced by whether diesel fuels have satisfactory thermal stability perfor-
storage in tanks kept free of water, and tankage should have mance properties.6,7
provisions for water draining on a scheduled basis. Water X2.10.2 Performance in engines has not been sufficiently
promotes corrosion, and microbiological growth may occur at correlated with results from Test Method D 6468 to provide
a fuel-water interface. Refer to Guide D 6469 for a more definitive specification requirements. However, the following
complete discussion. Underground storage is preferred to avoid guidelines are suggested.
temperature extremes; above-ground storage tanks should be X2.10.2.1 Fuels giving a Test Method D 6468 reflectance
sheltered or painted with reflective paint. High storage tem- value of 70 % or more in a 90 minute test at the time of
peratures accelerate fuel degradation. Fixed roof tanks should manufacture should give satisfactory performance in normal
be kept full to limit oxygen supply and tank breathing. use.
X2.7.2 Copper and copper-containing alloys should be X2.10.2.2 Fuels giving a Test Method D 6468 reflectance
avoided. Copper can promote fuel degradation and may pro- value of 80 % or more in a 180 minute test at the time of
duce mercaptide gels. Zinc coatings can react with water or manufacture should give satisfactory performance in severe
organic acids in the fuel to form gels that rapidly plug filters. use.
X2.7.3 Appendix X2 of Specification D 2880 discusses fuel X2.10.3 Thermal stability as determined by Test Method
contaminants as a general topic. D 6468 is known to degrade during storage.8 The guidance
under X2.10 is for fuels used within six months of
X2.8 Fuel Use Conditions manufacture.
X2.8.1 Many diesel engines are designed so that the diesel
6
fuel is used for heat transfer. In modern heavy-duty diesel Bacha, John D., and Lesnini, David G., “Diesel Fuel Thermal Stability at
300°F,” Proceedings of the 6th International Conference on Stability and Handling
engines, for example, only a portion of the fuel that is of Liquid Fuels, Vancouver, B.C., October 1997.
circulated to the fuel injectors is actually delivered to the 7
Schwab, Scott D., Henly, Timothy J., Moxley, Joel F., and Miller, Keith,
combustion chamber. The remainder of the fuel is circulated “Thermal Stability of Diesel Fuel,” Proceedings of the 7th International Conference
on Stability and Handling of Liquid Fuels, Graz, Austria, September 2000.
back to the fuel tank, carrying heat with it. Thus adequate high 8
Henry, C. P., “The du Pont F21 149°C (300°F) Accelerated Stability Test,”
temperature stability can be a necessary requirement in some Distillate Fuel Stability and Cleanliness, ASTM STP 751, Stavinoha, L. L., Henry,
severe applications or types of service. C. P., editors, ASTM International, W. Conshohocken, PA, 1981, pp. 22-33.

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D 7467 – 09

X3. TENTH PERCENTILE MINIMUM AMBIENT AIR TEMPERATURES FOR THE UNITED STATES
(EXCEPT HAWAII)

X3.1 Introduction low temperature operability limit of fuels without cold flow
X3.1.1 The tenth percentile minimum ambient air tem- additives in most vehicles with diesel fuel that contains no
peratures shown on the following maps (Figs. X3.1-X3.12) and biodiesel, and its relevance with B6 to B20 blends has not been
in Table X3.1 were derived from an analysis of historical validated.
hourly temperature readings recorded over a period of 15 to 21 X3.1.2.1 Long term weather patterns (Average winter low
years from 345 weather stations in the United States. This temperatures will be exceeded on occasion).
study was conducted by the U.S. Army Mobility Equipment X3.1.2.2 Short term local weather conditions (Unusual cold
Research and Development Center (USAMERDC), Coating periods do occur).
and Chemical Laboratory, Aberdeen Proving Ground, MD X3.1.2.3 Elevation (High locations are usually colder than
21005. The tenth percentile minimum ambient air temperature surrounding lower areas).
is defined as the lowest ambient air temperature which will not X3.1.2.4 Specific engine design.
go lower on average more than 10 % of the time. In other X3.1.2.5 Fuel system design (Recycle rate, filter location,
words, the daily minimum ambient air temperature would on filter capacity, filter porosity, and so forth.)
average not be expected to go below the monthly tenth X3.1.2.6 Fuel viscosity at low temperatures.
percentile minimum ambient air temperature more than 3 days X3.1.2.7 Equipment add-ons (Engine heaters, radiator cov-
for a 30-day month. See Table X3.1. ers, fuel line and fuel filter heaters and so forth.)
X3.1.2 These data may be used to estimate low temperature X3.1.2.8 Types of operation (Extensive idling, engine shut-
operability requirements. In establishing low temperature op- down, or unusual operation).
erability requirements, consideration should be given to the X3.1.2.9 Low temperature flow improver additives in fuel.
following. These factors, or any combination, may make low X3.1.2.10 Geographic area for fuel use and movement
temperature operability more or less severe than normal. As between geographical areas.
X3.1.2.1 through X3.1.2.12 indicate, field work suggests that X3.1.2.11 General housekeeping (Dirt or water, or both, in
cloud point (or wax appearance point) is a fair indication of the fuel or fuel supply system).

FIG. X3.1 October—10th Percentile Minimum Temperatures

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D 7467 – 09

FIG. X3.2 November—10th Percentile Minimum Ambient Air Temperatures

X3.1.2.12 Impact failure for engine to start or run (Critical 10°C below the cloud point should be viewed with caution
vs. non-critical application). because those results did not necessarily reflect the true vehicle
X3.1.3 Historical Background—Three test methods have low temperature operability limits.10 CFPP has been applied to
been widely used to estimate or correlate with low temperature many areas of the world where similar vehicle designs are
vehicle operability with diesel fuel that contains no biodiesel. used. The Low Temperature Flow Test (LTFT), Test Method
These test methods may be useful to estimate or correlate with D 4539, was designed to correlate with the most severe and one
lower temperature vehicle operability with B6 to B20, but their of the most common fuel delivery systems used in North
use with B6 to B20 has not been validated. Cloud point, Test American Heavy Duty trucks. Under prescribed slow cool
Method D 2500, is the oldest of the three and most conserva- conditions (1°C/h), similar to typical field conditions, several
tive of the tests. The cloud point test indicates the earliest 200 cc fuel specimens in glass containers fitted with 17 µm
appearance of wax precipitation that might result in plugging screen assemblies are cooled. At 1°C intervals one specimen is
of fuel filters or fuel lines under prescribed cooling conditions. drawn through the screen under a 20 kPa vacuum. Approxi-
Although not 100 % failsafe, it is the most appropriate test for mately 90 % of the fuel must come over in 60 s or less for the
applications that can not tolerate much risk. The Cold Filter result to be a pass. This process is continued at lower
Plugging Point (CFPP) test, Test Method D 6371, was intro- temperatures (1°C increments) until the fuel fails to come over
duced in Europe in 1965. The CFPP was designed to correlate in the allotted 60 s. The lowest passing temperature is defined
with the majority of European vehicles. Under rapid cooling as the LTFT for that fuel. In 1981, a CRC program was
conditions, 20 cc fuel is drawn through a 45 micron screen then conducted to evaluate the efficacy of cloud point, CFPP, pour
allowed to flow back through the screen for further cooling. point, and LTFT for protecting the diesel vehicle population in
This process is continued every 1°C until either the 20 cc fuel North America and to determine what benefit flow-improvers
fails to be drawn through the screen in 60 s or it fails to return could provide. The field test consisted of 3 non-flow improved
through the screen in 60 s. It was field tested many times in diesel fuels, 5 flow improved diesel fuels, 4 light-duty passen-
Europe9 before being widely accepted as a European specifi- ger cars, and 3 heavy-duty trucks. The field trial resulted in two
cation. Field tests have also shown CFPP results more than

9 10
“Low Temperature Operability of Diesels. A Report by CEC Investigation “SFPP—A New Laboratory Test for Assessment of Low Temperature Oper-
Group IGF-3,” CEC, P-171-82. ability of Modern Diesel Fuels,” CEC/93/EF 15, May 1993, pp. 5-7.

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D 7467 – 09

FIG. X3.3 December—10th Percentile Minimum Ambient Air Temperatures

documents11,12 that provide insight into correlating laboratory flow-improved fuels. On the other hand, cloud point came
tests to North American vehicle performance in the field. The closest to a fail-safe predictor of vehicle performance for all
general conclusions of the study were: vehicles.
(1) In overnight cool down, 30 % of the vehicles tested had Since the 1981 field test, non-independent studies13 using
a final fuel tank temperature within 2°C of the overnight newer vehicles verified the suitability of the LTFT for North
minimum ambient temperature. American heavy-duty trucks. Users are advised to review these
(2) The use of flow-improved diesel fuel permits some and any more recent publications when establishing low
vehicles to operate well below the fuel cloud point. temperature operability requirements and deciding upon test
(3) Significant differences exist in the severity of diesel methods.
vehicles in terms of low temperature operation. X3.1.3.1 Current Practices—It is recognized that fuel dis-
(4) No single laboratory test was found that adequately tributors, producers, and end users in the United States use
predicts the performance of all fuels in all vehicles. cloud point, wax appearance point, CFPP, and LTFT to
(5) CFPP was a better predictor than pour point, but both estimate vehicle low temperature operability limits for diesel
methods over-predicted, minimum operating temperatures in fuel. No independent data has been published in recent years to
many vehicles. For this reason, these tests were judged determine test applicability for today’s fuels and vehicles.
inadequate predictors of low-temperature performance and
dismissed from further consideration. X3.2 Maps
(6) Cloud point and LTFT showed varying degrees of X3.2.1 The maps in the following figures were derived from
predictive capability, and offered distinctively different advan- CCL Report No. 316, “A Predictive Study for Defining
tages. Both predicted the performance of the base fuels well, Limiting Temperatures and Their Application in Petroleum
but LTFT more accurately predicted the performance of the Product Specifications,” by John P. Doner. This report was
published by the U.S. Army Mobility Equipment Research and
Development Center (USAMERDC), Coating and Chemical
11 Laboratory, and it is available from the National Technical
CRC Report No. 537, “The Relationship Between Vehicle Fuel Temperature
and Ambient Temperature, 1981 CRC Kapuskasing Field Test,” December 1983.
12
CRC Report No. 528, “1981 CRC Diesel Fuel Low-Temperature Operability
13
Field Test,” September 1983. SAE 962197, SAE 982576, SAE 2000–01–2883.

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D 7467 – 09

FIG. X3.4 January—10th Percentile Minimum Ambient Air Temperatures

Information Service, Springfield, VA 22151, by requesting California, South Coast—Orange, San Diego, San Luis
Publication No. AD0756420. Obispo, Santa Barbara, Ventura, Los Angeles (except that
X3.2.2 Where states are divided the divisions are noted on portion north of the San Gabriel Mountain range and east of the
the maps and table with the exception of California, which is Los Angeles County Aqueduct).
divided by counties as follows: California, Southeast—Imperial, Riverside, San Bernardino,
California, North Coast—Alameda, Contra Costa, Del Los Angeles (that portion north of the San Gabriel Mountain
Norte, Humbolt, Lake, Marin, Mendocino, Monterey, Napa, range and east of the Los Angeles County Aqueduct), Mono,
San Benito, San Francisco, San Mateo, Santa Clara, Santa
Inyo, Kern (that portion lying east of the Los Angeles County
Cruz, Solano, Sonoma, Trinity.
Aqueduct).
California, Interior—Lassen, Modoc, Plumas, Sierra,
Siskiyou, Alpine, Amador, Butte, Calaveras, Colusa, El Do- X3.2.3 The temperatures in CCL Report No. 316 were in
rado, Fresno, Glenn, Kern (except that portion lying east of the degrees Fahrenheit. The degree Celsius temperatures in Ap-
Los Angeles County Aqueduct), Kings, Madera, Mariposa, pendix X3 were obtained by converting the original degree
Merced, Placer, Sacramento, San Joaquin, Shasta, Stanislaus, Fahrenheit temperatures.
Sutter, Tehama, Tulare, Tuolumne, Yolo, Yuba, Nevada.

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D 7467 – 09

FIG. X3.5 February—10th Percentile Minimum Ambient Air Temperatures

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D 7467 – 09

FIG. X3.6 March—10th Percentile Minimum Ambient Air Temperatures

FIG. X3.7 October—10th Percentile Minimum Ambient Air Temperatures

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D 7467 – 09

FIG. X3.8 November—10th Percentile Minimum Ambient Air Temperatures

FIG. X3.9 December—10th Percentile Minimum Ambient Air Temperatures

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D 7467 – 09

FIG. X3.10 January—10th Percentile Minimum Ambient Air Temperatures

FIG. X3.11 February—10th Percentile Minimum Ambient Air Temperatures

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D 7467 – 09

FIG. X3.12 March—10th Percentile Minimum Ambient Air Temperatures

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D 7467 – 09
TABLE X3.1 Tenth Percentile Minimum Ambient Air Temperatures for the United States (except Hawaii)

10th Percentile Temperature°C, min


State
Oct. Nov. Dec. Jan. Feb. March
Alabama 4 −3 −6 −7 −3 −2
Alaska Northern −25 −37 −45 −49 −47 −43
Southern −11 −13 −18 −32 −32 −29
South East −4 −11 −16 −19 −13 −12
Arizona North 34° latitude −4 −12 −14 −17 −16 −12
South 34° latitude 7 0 −2 −4 −3 −1
Arkansas 2 −4 −7 −11 −7 −3
California North Coast 3 0 −2 −2 −1 −1
Interior 2 −3 −4 −7 −6 −6
South Coast 6 2 0 −1 0 2
Southeast 1 −6 −8 −11 −7 −5
Colorado East 105° long −2 −12 −14 −19 −15 −12
West 105° long −8 −18 −25 −30 −24 −16
Connecticut −1 −7 −16 −17 −16 −9
Delaware 2 −3 −10 −11 −10 −6
Florida North 29° latitude 7 1 −2 −3 −1 2
South 29° latitude 14 7 3 3 5 7
Georgia 3 −2 −6 −7 −6 −2
Idaho −4 −13 −18 −21 −18 −13
Illinois North 40° latitude −1 −9 −19 −21 −18 −11
South 40° latitude 1 −7 −16 −17 −15 −8
Indiana −1 −7 −16 −18 −16 −9
Iowa −2 −13 −23 −26 −22 −16
Kansas −2 −11 −15 −19 −14 −13
Kentucky 1 −6 −13 −14 −11 −6
Louisiana 5 −1 −3 −4 −2 1
Maine −3 −10 −23 −26 −26 −18
Maryland 2 −3 −10 −12 −10 −4
Massachusetts −2 −7 −16 −18 −17 −10
Michigan −2 −11 −20 −23 −23 −18
Minnesota −4 −18 −30 −34 −31 −24
Mississippi 3 −3 −6 −6 −4 −1
Missouri 1 −7 −14 −16 −13 −8
Montana −7 −18 −24 −30 −24 −21
Nebraska −3 −13 −18 −22 −19 −13
Nevada North 38° latitude −7 −14 −18 −22 −18 −13
South 38° latitude 8 0 −3 −4 −2 1
New Hampshire −3 −8 −18 −21 −21 −12
New Jersey 2 −3 −11 −12 −11 −6
New Mexico North 34° latitude −2 −11 −14 −17 −14 −11
South 34° latitude 4 −4 −8 −11 −7 −3
New York North 42° latitude −3 −8 −21 −24 −24 −16
South 42° latitude −1 −5 −14 −16 −15 −9
North Carolina −1 −7 −10 −11 −9 −5
North Dakota −4 −20 −27 −31 −29 −22
Ohio −1 −7 −16 −17 −15 −9
Oklahoma 1 −8 −12 −13 −8 −7
Oregon East 122° long −6 −11 −14 −19 −14 −9
West 122° long 0 −4 −5 −7 −4 −3
Pennsylvania North 41° latitude −3 −8 −19 −20 −21 −15
South 41° latitude 0 −6 −13 −14 −14 −8
Rhode Island 1 −3 −12 −13 −13 −7
South Carolina 5 −1 −5 −5 −3 −2
South Dakota −4 −14 −24 −27 −24 −18
Tennessee 1 −5 −9 −11 −9 −4
Texas North 31° latitude 3 −6 −9 −13 −9 −7
South 31° latitude 9 2 −2 −3 −1 2
Utah −2 −11 −14 −18 −14 −8
Vermont −3 −8 −20 −23 −24 −15
Virginia 2 −3 −9 −11 −9 −4
Washington East 122° long −2 −8 −11 −18 −11 −8
West 122° long 0 −3 −3 −7 −4 −3
West Virginia −3 −8 −15 −16 −14 −9
Wisconsin −3 −14 −24 −28 −24 −18
Wyoming −4 −15 −18 −26 −19 −16

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D 7467 – 09
SUMMARY OF CHANGES

Subcommittee D02.E0 has identified the location of selected changes to this standard since the last issue
(D 7467–08) that may impact the use of this standard.

(1) Replaced wording in X1.15.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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