Astm D56-05 PDF
Astm D56-05 PDF
Astm D56-05 PDF
Designation: D 56 05
INTRODUCTION
To ensure an acceptable precision, this dynamic flash point test method employs a prescribed rate
of temperature rise for the material under test. The rate of heating may not in all cases give the
precision quoted in the test method because of the low thermal conductivity of certain materials. To
improve the prediction of flammability, Test Method D 3941, which utilizes a slower heating rate, was
developed. Test Method D 3941 provides conditions closer to equilibrium where the vapor above the
liquid and the liquid are at about the same temperature. If a specification requires Test Method D 56,
do not change to Test Method D 3941 or other test method without permission from the specifier.
Flash point values are a function of the apparatus design, the condition of the apparatus used, and
the operational procedure carried out. Flash point can therefore only be defined in terms of a standard
test method, and no general valid correlation can be guaranteed between results obtained by different
test methods, or with test apparatus different from that specified.
1. Scope*
1.1 This test method covers the determination of the flash
point, by tag manual and automated closed testers, of liquids
with a viscosity below 5.5 mm2/s (cSt) at 40C (104F), or
below 9.5 mm2/s (cSt) at 25C (77F), and a flash point below
93C (200F).
1.1.1 For the closed-cup flash point of liquids with the
following properties: a viscosity of 5.5 mm2/s (cSt) or more at
40C (104F); a viscosity of 9.5 mm2/s (cSt) or more at 25C
(77F); a flash point of 93C (200F) or higher; a tendency to
form a surface film under test conditions; or containing
suspended solids, Test Method D 93 can be used.
1.1.2 For cut-back asphalts refer to Test Methods D 1310
and D 3143.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility.
Current edition approved May 1, 2005. Published May 2005. Originally
approved in 1918. Last previous edition approved in 2002 as D 5602a.
2
For information on United States Department of Transportation regulations, see
Codes of United States Regulation 49 CFR Chapter 1 and for information on United
States Department of Labor regulations, see Code of United States Regulation 29
CFR Chapter XVII. Each of these items are revised annually and may be procured
from the Superintendent of Documents, Government Printing Office, Washington,
DC 20402.
D 56 05
3.1.1.1 DiscussionThe specimen is deemed to have
flashed when a flame appears and instantaneously propagates
itself over the entire surface of the fluid.
3.1.1.2 DiscussionWhen the ignition source is a test
flame, the application of the test flame may cause a blue halo
or an enlarged flame prior to the actual flash point. This is not
a flash and should be ignored.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 dynamic (non-equilibrium)in this type of flash point
apparatus, the condition of the vapor above the specimen and
the specimen are not at the same temperature at the time that
the ignition source is applied.
3.2.1.1 DiscussionThis is primarily caused by the heating
of the specimen at the constant prescribed rate with the vapor
temperature lagging behind the specimen temperature. The
resultant flash point temperature is generally within the reproducibility of the test method.
3.2.2 equilibriumin that type of flash point apparatus or
test method, the vapor above the specimen and the specimen
are at the same temperature at the time the ignition source is
applied.
3.2.2.1 DiscussionThis condition may not be fully
achieved in practice, since the temperature is not uniform
throughout the specimen and the test cover and shutter are
generally cooler.
3. Terminology
3.1 Definitions:
3.1.1 flash pointthe lowest temperature corrected to a
pressure of 101.3 kPa (760 mm Hg) at which application of an
ignition source causes the vapors of a specimen of the sample
to ignite under specified conditions of test.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
4
Available from Superintendent of Documents, U.S. Government Printing
Office, Washington, DC 20402.
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036.
D 56 05
7.2 Do not store samples in gas-permeable containers since
volatile materials may diffuse through the walls of the enclosure. Samples in leaky containers are suspect and not a source
of valid results.
7.3 At least 50 mL of sample is required for each test. Refer
to sampling information in Practice D 4057.
8. Preparation of Apparatus (Manual)
8.1 Support the manual apparatus on a level steady surface,
such as a table. Unless tests are made in a draft-free room or
compartment, surround the tester on three sides by the shield
for protection from drafts. Tests are not to be made in a
laboratory draft hood or near ventilators.
8.2 Natural gas and bottled gas flame and electric ignitors
have been found acceptable for use as the ignition source.
(WarningGas pressure supplied to the apparatus must not be
allowed to exceed 3 kPa (12 in.) of water pressure.)
8.3 For flash points below 13C (55F) or above 60C
(140F), use as a bath liquid a 1 + 1 mixture of water and
ethylene glycol (WarningEthylene GlycolPoison. Harmful or fatal if swallowed. Vapor harmful. Avoid contact with
skin.) For flash points between 13C (55F) and 60C (140F),
either water or a water-glycol mixture can be used as bath
liquid. The temperature of the liquid in the bath shall be at least
10C (18F) below the expected flash point at the time of
introduction of the sample into the test cup. Do not cool bath
liquid by direct contact with dry ice (solid carbon dioxide).
NOTE 3Due to possible difficulty in maintaining the prescribed rate of
temperature rise and due to the formation of ice on the lid, results by this
test method for samples having flash points below 0C (32F) may be
unreliable. Trouble due to ice formation on the slide can be minimized by
carefully lubricating the slide shutter with high-vacuum silicone lubricant.
Below 4C (40F)
Use ASTM
ThermometerA
57C or (57F)
At 4 to 49C
(40 to 120F)
9C or (9F)
57C or (57F)
Above 49C
(120F)
9C or (9F)
NOTE 2Whenever thermometers complying with ASTM requirements are not available, thermometers complying with the requirements
for The Institute of Petroleum thermometer IP 15C PM-Low can be used.
7. Sampling
7.1 Erroneously high flash points will be obtained when
precautions are not taken to avoid the loss of volatile material.
Containers should not be opened unnecessarily to prevent loss
of volatile material and possible introduction of moisture.
Transfers should not be made unless the sample temperature is
at least 10C (18F) below the expected flash point. When
possible, flash point shall be the first test performed on a
sample and the sample must be stored at low temperature.
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D 56 05
defined, is observed. Instead a significant enlargement of the
test flame (not halo effect) and change in color of the test flame
from blue to yellowish-orange occurs. Continued heating and
testing of these samples above ambient temperature can result
in significant burning of vapors outside the test cup, and can be
a potential fire hazard. See Appendix X1 and Appendix X2 for
more information.)
9.6 Discontinue the test and remove the source of heat. Lift
the lid and wipe the temperature measuring device bulb.
Remove the test cup, empty, and wipe dry.
9.7 If, at any time between the first introduction of the
ignition source and the observation of the flash point, the rise
in temperature of the specimen is not within the specified rate,
discontinue the test, discard the result and repeat the test,
adjusting the source of heat to secure the proper rate of
temperature rise, or using a modified expected flash point, or
both, as required.
9.8 Never make a repeat test on the same specimen of
sample; always take fresh specimen of sample for each test.
9. Procedure (Manual)
9.1 Using a graduated cylinder and taking care to avoid
wetting the cup above the final liquid level, measure 50 6 0.5
mL of the sample into the cup, both the sample and graduated
cylinder being precooled, when necessary, so that the specimen
temperature at the time of measurement will be 27 6 5C (80
6 10F) or at least 10C (18F) below the expected flash point,
whichever is lower. It is essential that the sample temperature
be maintained at least 10C (18F) below the expected flash
point during the transfers from the sample container to the
cylinder and from the cylinder to the test cup. Destroy air
bubbles on the surface of the specimens by use of knife point
or other suitable device. Wipe the inside of the cover with a
clean cloth or absorbent tissue paper; then attach the cover,
with the temperature measuring device in place, to the bath
collar.
9.2 Light the test flame, when used, adjusting it to the size
of the small bead on the cover. Operate the mechanism on the
cover in such a manner as to introduce the ignition source into
the vapor space of the cup, and immediately bring it up again.
The time consumed for the full operation should be 1 s,
allowing equal time periods for the introduction and return.
Avoid any hesitation in the operation of depressing and raising
the ignition source. When a flash is observed on the initial
operation of the mechanism, discontinue the test and discard
the result. In this case, a fresh sample shall be cooled an
additional 10C (18F), below the original specimen installation temperature.
9.2.1 Exercise care when using a test flame, if the flame is
extinguished it cannot ignite the specimen and the gas entering
the vapor space can influence the result. When the flame is
prematurely extinguished the test shall be discontinued and any
result discarded.
9.3 Flash Points Below 60C (140F)When the flash
point of the sample is known to be below 60C (140F), apply
and adjust the heat so that the temperature of the portion will
rise at a rate of 1C (2F)/min 6 6 s. When the temperature of
the specimen in the test cup is 5C (10F) below its expected
flash point, apply the ignition source in the manner just
described in 9.2 and repeat the application of the ignition
source after each 0.5C (1F) rise in temperature of the
specimen.
9.4 Flash Points at 60C (140F) or AboveIf the flash
point of the sample is known to be 60C (140F) or higher,
apply and adjust the heat so that the temperature of the
specimen will rise at a rate of 3C (5F)/min 6 6 s. When the
temperature of the specimen in the test cup is 5C (10F) below
its expected flash point, apply the ignition source in the manner
just described in 9.2 and repeat the application of the ignition
source each 1C (2F) rise in temperature of the specimen.
9.5 When the application of the ignition source causes a
distinct flash in the interior of the cup, as defined in 3.1.1,
observe and record the temperature of the specimen as the flash
point. Do not confuse the true flash with the bluish halo that
sometimes surrounds the ignition source during applications
immediately preceding the actual flash. (WarningFor certain mixtures containing halogenated hydrocarbons, such as,
methylene chloride or trichloroethylene, no distinct flash, as
D 56 05
be discarded and the test repeated with a fresh specimen.
(WarningFor certain mixtures containing halogenated hydrocarbons, such as, methylene chloride or trichloroethylene,
no distinct flash, as defined, is observed. Instead a significant
enlargement of the test flame (not halo effect) and change in
color of the test flame from blue to yellowish-orange occurs.
Continued heating and testing of these samples above ambient
temperature can result in significant burning of vapors outside
the test cup, and can be a potential fire hazard. See Appendix
X1 and Appendix X2 for more information.)
12.6 When the apparatus has cooled down to a safe handling
temperature (less than 55C (130F)) remove the cover and the
test cup and clean the apparatus as recommended by the
manufacturer.
13. Report
(1)
(2)
(3)
where:
C = observed flash point, C,
F = observed flash point, F,
p = ambient barometric pressure, kPa, and
P = ambient barometric pressure, mm Hg.
13.2 The barometric pressure used in this calculation shall
be the ambient pressure for the laboratory at the time of test.
Many aneroid barometers, such as those used at weather
stations and airports, are precorrected to give sea level readings; these shall not be used.
13.3 Report the corrected flash point to the nearest 0.5C (or
1F).
14. Precision and Bias
14.1 PrecisionThe following criteria shall be used for
judging the acceptability of results (95 % probability):
14.1.1 RepeatabilityThe difference between successive
test results, obtained by the same operator with the same
apparatus under constant operating conditions on identical test
material, would in the long run, in the normal and correct
operation of the test method, exceed the following values only
in one case in twenty:
NOTE 6Care should be taken when cleaning and positioning the lid
assembly so as not to damage or dislocate the flash detection system or
temperature measuring device. See manufacturers instructions for proper
care and maintenance.
Repeatability, C (F)
1.2C (2.0F)
1.6C (3.0F)
D 56 05
Flash Point, C (F)
Reproducibility, C (F)
4.3C (8F)
5.8C (10F)
14.2 BiasThe procedure in Test Method D 56 for measuring flash point has no bias since the tag flash point can be
defined only in terms of this test method. The current interlaboratory tests confirm that there is no relative bias between
manual and automated procedures. In any case of dispute the
flash point as determined by the manual procedure shall be
considered the referee test.
15. Keywords
15.1 combustible; fire risk; flammable; flash point; tag
closed cup
NOTE 7Mixtures such as, but not limited to, those that are chlorinated
or include water may cause significant differences in the results obtained
by manual and automatic instruments. For these mixtures, the precision
statement may not apply.
6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S151007.
ANNEXES
(Mandatory Information)
A1. APPARATUS
D 56 05
mm
0.03
0.13
4.78
7.15
9.84
Inch-Pound Equivalents
in.
mm
0.001
10.32
0.005
11.92
0.188
15.10
0.281
18.0
0.387
20.6
in.
0.406
0.469
0.594
0.71
0.81
D 56 05
Inch-Pound Equivalents
mm
6.4
82.6
95.3
in.
0.25
3.25
3.75
D 56 05
TABLE A2.1 D 56 Typical Flash Point Values and Typical Limits
for CRM
Hydrocarbon
ndecane
nundecane
Purity
(mole %)
99+
99+
Flash
Point(C)
50.9
67.1
Limits
(C)
62.3
62.3
7
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S15-1010.
A3.1 The cup temperature measuring device, which conforms also to the specifications for the low-range temperature
measuring device used in the Pensky-Martens flash tester, Test
Method D 93, is frequently supplied by the temperature measuring device manufacturer with a metal or polytetrafluoroethylene ferrule intended to fit the collar on the lid of the flash
tester. This ferrule is frequently supplemented by an adapter
that is used in the larger-diameter collar of the Pensky-Martens
apparatus. Differences in dimensions of these collars, which
are immaterial in their effect on the result of tests, are a source
A3.2 Subcommittee E01.21 on Reference Material Planning, Proficiency Testing, and Laboratory Accreditation, has
studied this problem and has established some dimensional
requirements which are shown, suitably identified, in Fig.
A1.1, Fig. A3.1, and Fig. A3.2. Conformity to these requirements is not mandatory but is desirable to users as well as
suppliers of tag closed testers.
D 56 05
Inch-Pound Equivalents
mm
0.05
5.3
7.1
in.
0.002
0.21
0.28
mm
8.6
9.8
17.3
in.
0.34
0.385
0.68
10
D 56 05
Inch-Pound Equivalents
mm
1.5
7.23
8.40
in.
0.06
0.284
0.330
APPENDIXES
(Nonmandatory Information)
X1. FLASH POINT MASKING PHENOMENON
flame and a change in the color of the test flame from blue to
yellow-orange laminar flame is observed.
X1.2 This flash point masking phenomenon most frequently occurs with ignitable liquids that contain certain
halogenated hydrocarbons such as dichloromethane (methylene chloride) and trichloroethylene.
X1.5 It is recommended that if this condition is encountered during the flash point testing of these type of materials,
testing should be discontinued.
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D 56 05
X2. FLASH POINT TEST AND FLAMMABILITY OF MIXTURES
SUMMARY OF CHANGES
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D 5602a) that may impact the use of this standard.
(2) Deleted test cup weight in A1.1.2.
(3) Deleted reference to MNL7 in A2.2.1.
(4) Deleted Note A2.4.
(1) Changed thermometer to temperature measuring device in 6.3, 9.1, 9.6, A1.1.3.1, A1.1.3.4, A3.1, Table A1.1, Fig.
A1.2, Fig. A3.1, and Fig. A3.2.
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