D7467-09 38722
D7467-09 38722
D7467-09 38722
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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).
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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)
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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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“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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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).
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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
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
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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TABLE X3.1 Tenth Percentile Minimum Ambient Air Temperatures for the United States (except Hawaii)
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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 7467–08) that may impact the use of this standard.
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