ASTM D7094-04

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Designation: D7094 – 04
Standard Test Method for
Flash Point by Modified Continuously Closed Cup
(MCCCFP) Tester
This standard is issued under the fixed designation D7094; 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 bility of regulatory limitations prior to use. For specific
warning statements, see 7.2, 8.5, and 10.1.2.
1.1 This test method covers the determination of the flash
point of fuels, lube oils, solvents and other liquids by a
2. Referenced Documents
continuously closed cup tester utilizing a specimen size of 2
2.1 ASTM Standards:
mL, cup size of 7 mL, with a heating rate of 2.5°C per minute.
D93 Test Methods for Flash Point by Pensky-Martens
1.1.1 Apparatus requiring a specimen size of 1 mL, cup size
Closed Cup Tester
of 4 mL, and a heating rate of 5.5°C per minute must be run
D4057 Practice for Manual Sampling of Petroleum and
according to Test Method D6450.
Petroleum Products
1.2 This flash point test method is a dynamic method and
D4177 Practice for Automatic Sampling of Petroleum and
depends on definite rates of temperature increase. It is one of
Petroleum Products
the many flash point test methods available and every flash
D6450 TestMethodforFlashPointbyContinuouslyClosed
point test method, including this one, is an empirical method.
Cup (CCCFP) Tester
NOTE 1—Flash point values are not a constant physical chemical
D6708 PracticeforStatisticalAssessmentandImprovement
property of materials tested. They are a function of the apparatus design,
of Expected Agreement Between Two Test Methods that
the condition of the apparatus used, and the operational procedure carried
Purport to Measure the Same Property of a Material
out. Flash point can, therefore, only be defined in terms of a standard test
E300 Practice for Sampling Industrial Chemicals
methodandnogeneralvalidcorrelationcanbeguaranteedbetweenresults
2.2 ISO Standards:
obtained by different test methods or where different test apparatus is
specified. ISO Guide 34 Quality Systems Guidelines for the Produc-
tion of Reference Materials
1.3 This test method utilizes a closed but unsealed cup with
ISO Guide 35 Certification of Reference Materials—
air injected into the test chamber.
General and Statistical Principles
1.4 This test method is suitable for testing samples with a
flash point from 35 to 225°C.
3. Terminology
NOTE 2—Flashpointdeterminationsbelow35°Candabove225°Cmay
3.1 Definitions:
be performed; however, the precision has not been determined below and
3.1.1 flash point, n—the lowest temperature corrected to a
above these temperatures.
pressure of 101.3 kPa at which application of an ignition
1.5 If the user’s specification requires a defined flash point
source causes the vapors of a specimen of the sample to ignite
method other than this method, neither this method nor any
momentarily under specified conditions of the test.
other test method should be substituted for the prescribed test
3.1.1.1 Discussion—Forthepurposeofthistestmethod,the
method without obtaining comparative data and an agreement
test specimen is deemed to have flashed when the hot flame of
from the specifier.
the ignited vapor causes an instantaneous pressure increase of
1.6 The values stated in SI are to be regarded as standard.
at least 20 kPa inside the closed measuring chamber.
Temperatures are in degrees Celsius, pressure in kilo-Pascals.
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
responsibility of the user of this standard to establish appro-
Standards volume information, refer to the standard’s Document Summary page on
priate safety and health practices and determine the applica-
the ASTM website.
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036.
1 4
This test method is under the jurisdiction of ASTM Committee D02 on The method of detecting the flash point by monitoring the instantaneous
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee pressure increase is covered by a patent. Interested parties are invited to submit
D02.08 on Volatility. information regarding the identification of an alternative(s) to this patented item to
Current edition approved Nov. 1, 2004. Published November 2004. DOI: the ASTM International Headquarters. Your comments will receive careful consid-
10.1520/D7094-04. eration at a meeting of the responsible technical committee, which you may attend.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7094 – 04
TABLE 1 Volume of Introduced Air as a Function of
5.4 Flash point can also indicate the possible presence of
Sample Temperature
highly volatile and flammable materials in a relatively non-
Sample Temperature Introduced Volume
volatile or nonflammable material, such as the contamination
Range (°C) of Air (mL)
of lubricating oils by small amounts of diesel fuel or gasoline.
below 80 0
Thistestmethodwasdesignedtobemoresensitivetopotential
80 to below 150 0.5 6 0.15
contamination than Test Method D6450.
150 to below 200 1 6 0.2
200 to below 300 1.5 6 0.3
300 and above 2 6 0.4
6. Apparatus
6.1 Flash Point Apparatus, Continuously Closed Cup
Operation—The type of apparatus suitable for use in this test
3.1.2 dynamic, adj—the condition where the vapor above
method employs a lid of solid brass, the temperature of which
the test specimen and the test specimen are not in temperature
is controlled electrically. Two temperature sensors for the
equilibrium at the time at which the ignition source is applied.
specimen and the lid temperatures, respectively, two arc pins
for a high voltage arc, and a connecting tube for the pressure
4. Summary of Test Method
monitoring and the air introduction are incorporated in the lid.
4.1 The lid of the test chamber is regulated to a temperature
Associated equipment for electrically controlling the chamber
at least 18°C below the expected flash point.A2 6 0.2 mLtest
temperature is used, and a digital readout of the specimen
specimen of a sample is introduced into the sample cup. Both
temperatureisprovided.Theapparatusanditscriticalelements
specimen and cup are at a temperature at least 18°C below the
are shown in Figs. A1.1 and A1.2.
expectedflashpoint;cooledifnecessary.Thecupisthenraised
6.1.1 Test Chamber—The test chamber is formed by the
and pressed onto the lid of specified dimensions to form the
samplecupandthetemperaturecontrolledlidandshallhavean
continuously closed but unsealed test chamber with an overall
overall volume of 7 6 0.3 mL. A metal to metal contact
volume of 7.0 6 0.3 mL.
between the lid and the sample cup shall provide good heat
4.2 After closing the test chamber, the temperatures of the
contactbutallowambientbarometricpressuretobemaintained
testspecimenandtheregulatedlidareallowedtoequilibrateto
inside the test chamber during the test. Critical dimensions are
within1°C.Thenthelidisheatedataprescribed,constantrate.
shown in Fig. A1.2. The pressure inside the measuring cham-
For the flash tests, a high voltage arc of defined energy is
ber during the temperature increase is monitored.Aseal that is
discharged inside the test chamber at regular intervals. After
tootightresultsinapressureincreaseaboveambientduetothe
each ignition, a variable amount of air (see Table 1)is
temperature and the vapor pressure of the sample.Apoor heat
introduced into the test chamber to provide the necessary
contact results in a bigger temperature difference between the
oxygen for the next flash test. The pressure inside the continu-
sample and the heated lid.
ously closed but unsealed test chamber remains at ambient
6.1.2 Sample Cup—The sample cup shall be made of
barometric pressure except for the short time during the air
nickel-plated aluminum or other material with similar heat
introduction and at a flash point.
conductivity.Itshallhaveanoverallvolumeof7 60.3mLand
4.3 After each arc application, the instantaneous pressure
shall be capable of containing 2 6 0.2 mL of sample. The
increase above the ambient barometric pressure inside the test
critical dimensions and requirements are shown in Fig. A1.2.
chamber is monitored. When the pressure increase exceeds 20
6.1.3 Specimen Temperature Sensor—The specimen tem-
kPa,thetemperatureatthatpointisrecordedastheuncorrected
perature sensor (Fig. A1.1) shall be a thermocouple (NiCr-Ni
flash point, which is then corrected to barometric pressure.
or similar) in stainless steel of 1 mm diameter with a response
time of t (90) = 3 s. It shall be immersed to a depth of at least
5. Significance and Use
2mmintothespecimen.Itshallhavearesolutionof0.1°Cand
5.1 The flash point temperature is one measure of the
a minimum accuracy of 6 0.2°C, preferably with a digital
tendency of the test specimen to form a flammable mixture
readout.
with air under controlled laboratory conditions. It is only one
6.1.4 Magnetic Stirring—The apparatus shall have provi-
of a number of properties which must be considered in
sions for stirring of the sample. A rotating magnet outside the
assessing the overall flammability hazard of a material.
samplecupshalldriveasmallstirringmagnetwhichisinserted
5.2 Flash point is used in shipping and safety regulations to
into the sample cup after sample introduction. The stirring
define flammable and combustible materials and for classifica-
magnetshallhaveadiameterof3 60.2mmandalengthof12
tion purposes. This definition may vary from regulation to
6 1 mm. The rotation speed of the driving magnet shall be
regulation. Consult the particular regulation involved for pre-
between 250 and 270 rev/min.
cise definitions of these classifications.
6.1.5 Air Introduction—Theapparatusshallhaveprovisions
5.3 This test method can be used to measure and describe
for introduction of air immediately after each flash test.The air
the properties of materials in response to heat and an ignition
source under controlled laboratory conditions and shall not be
used to describe or appraise the fire hazard or fire risk of
The sole source of supply of the continuously closed cup testers meeting these
requirements known to the committee at this time are available from Grabner
materials under actual fire conditions. However, results of this
Instruments,A-1220 Vienna/Austria, Dr. Otto-Neurath-Gasse 1. If you are aware of
test method may be used as elements of a fire risk assessment,
alternative suppliers, please provide this information to ASTM International
which takes into account all of the factors which are pertinent
Headquarters.Your comments will receive careful consideration at a meeting of the
to an assessment of the fire hazard of a particular end use. responsible technical committee, which you may attend.
D7094 – 04
shall be introduced by a short air pulse from a small membrane dodecane, toluene, acetone, and many solvents are flammable
compressor by means of a T-inlet in the connecting tube to the and are health hazards. Dispose of solvents and waste material
pressuretransducer.Thevolumeoftheintroducedair,from0.5 in accordance with local regulations.)
to 2 mL, is dependent on the sample temperature (seeTable 1).
8. Sampling
6.1.6 Electricalheatingandthermoelectriccoolingofthelid
8.1 Obtain at least a 50 mL sample from a bulk test site in
(see the Peltier element shown in Fig. A1.1) shall be used to
accordance with the instructions given in Practice D4057,
regulate the temperature of the test chamber for the duration of
D4177,or E300. Store the sample in a clean, tightly sealed
the test. The temperature regulation shall have a minimum
container at a low temperature.
accuracy of 6 0.2°C.
8.2 Do not store samples for an extended period of time in
6.1.7 A high voltage electric arc shall be used for the
gas permeable containers, such as plastic, because volatile
ignition of the flammable vapor. The energy of the arc shall be
material may diffuse through the walls of the container.
1.3 6 0.3 J (1.3 6 0.3 Ws) per arc and the energy shall be
Discard samples in leaky containers and obtain new samples.
applied within 19 6 2 m/s. (Warning—Because samples
8.3 Erroneously high flash points can be obtained when
containing low flash material or having a flash point below the
precautions are not taken to avoid loss of volatile material. Do
preset initial temperature can oversaturate the vapor inside the
chamber and hence prohibit the detection of a flash point in the not open containers unnecessarily. Do not make a transfer
unless the sample temperature is at least 18°C below the
chosen range, a precautionary arc set at 5°C intervals is
required while the lid and sample cup temperatures are expected flash point.When possible, perform the flash point as
the first test.
equalizing.)
6.1.8 The pressure transducer for the flash point detection 8.4 Samples of very viscous materials may be warmed until
they are reasonably fluid before they are tested. However, do
shall be connected to the connecting tube in the lid and shall
have a minimum operational range from 80 to 177 kPa with a not heat the unsealed sample above a temperature of 18°C
below its expected flash point.
minimum resolution of 0.1 kPa and a minimum accuracy of 6
8.5 Samples containing dissolved or free water may be
0.5 kPa. It shall be capable of detecting an instantaneous
dehydrated with calcium chloride or by filtering through a
pressure increase above barometric pressure of a minimum of
qualitative filter paper or a loose plug of dry absorbent cotton.
20 kPa within 100 m/s.
Warming the sample is permitted, but it should not be heated
NOTE 3—The monitoring of the instantaneous pressure increase above
above a temperature of 18°C below its expected flash point.
barometric pressure is one of several methods to determine a flash inside
(Warning—Because samples containing volatile material will
the test chamber. A pressure increase of 20 kPa corresponds to a flame
lose volatiles and then yield incorrectly high flash points, the
volume of approximately 2.5 mL.
NOTE 4—An automatic barometric correction, which is performed treatment described in 8.4 and 8.5 is not suitable for such
according to the procedure described in 12.1, can be installed in the tester.
samples.)
Theabsolutepressurereadingofthepressuretransducerdescribedin6.1.8
may be used for the correction. 9. Quality Control Checks
6.1.9
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