ASTM D7094-04(2009)
(Test Method)Standard Test Method for Flash Point by Modified Continuously Closed Cup (MCCCFP) Tester
Standard Test Method for Flash Point by Modified Continuously Closed Cup (MCCCFP) Tester
SIGNIFICANCE AND USE
The flash point temperature is one measure of the tendency of the test specimen to form a flammable mixture with air under controlled laboratory conditions. It is only one of a number of properties which must be considered in assessing the overall flammability hazard of a material.
Flash point is used in shipping and safety regulations to define flammable and combustible materials and for classification purposes. This definition may vary from regulation to regulation. Consult the particular regulation involved for precise definitions of these classifications.
This test method can be used to measure and describe 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 materials under actual fire conditions. However, results of this test method may be used as elements of a fire risk assessment, which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.
Flash point can also indicate the possible presence of highly volatile and flammable materials in a relatively nonvolatile or nonflammable material, such as the contamination of lubricating oils by small amounts of diesel fuel or gasoline. This test method was designed to be more sensitive to potential contamination than Test Method D6450.
SCOPE
1.1 This test method covers the determination of the flash point of fuels, lube oils, solvents and other liquids by a continuously closed cup tester utilizing a specimen size of 2 mL, cup size of 7 mL, with a heating rate of 2.5°C per minute.
1.1.1 Apparatus requiring a specimen size of 1 mL, cup size of 4 mL, and a heating rate of 5.5°C per minute must be run according to Test Method D6450.
1.2 This flash point test method is a dynamic method and depends on definite rates of temperature increase. It is one of the many flash point test methods available and every flash point test method, including this one, is an empirical method.
Note 1—Flash point values are not a constant physical chemical property of materials tested. They 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 where different test apparatus is specified.
1.3 This test method utilizes a closed but unsealed cup with air injected into the test chamber.
1.4 This test method is suitable for testing samples with a flash point from 35 to 225°C.
Note 2—Flash point determinations below 35°C and above 225°C may be performed; however, the precision has not been determined below and above these temperatures.
1.5 If the user’s specification requires a defined flash point method other than this method, neither this method nor any other test method should be substituted for the prescribed test method without obtaining comparative data and an agreement from the specifier.
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6.1 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 responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.2, 8.5, and 10.1.2.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D7094 −04(Reapproved 2009)
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 1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the determination of the flash
responsibility of the user of this standard to establish appro-
point of fuels, lube oils, solvents and other liquids by a
priate safety and health practices and determine the applica-
continuously closed cup tester utilizing a specimen size of 2
bility of regulatory limitations prior to use. For specific
mL, cup size of 7 mL, with a heating rate of 2.5°C per minute.
warning statements, see 7.2, 8.5, and 10.1.2.
1.1.1 Apparatus requiring a specimen size of 1 mL, cup size
of 4 mL, and a heating rate of 5.5°C per minute must be run
2. Referenced Documents
according to Test Method D6450.
2.1 ASTM Standards:
1.2 This flash point test method is a dynamic method and
D93 Test Methods for Flash Point by Pensky-Martens
depends on definite rates of temperature increase. It is one of
Closed Cup Tester
the many flash point test methods available and every flash
D4057 Practice for Manual Sampling of Petroleum and
point test method, including this one, is an empirical method.
Petroleum Products
NOTE 1—Flash point values are not a constant physical chemical
D4177 Practice for Automatic Sampling of Petroleum and
property of materials tested. They are a function of the apparatus design,
the condition of the apparatus used, and the operational procedure carried Petroleum Products
out. Flash point can, therefore, only be defined in terms of a standard test
D6450 Test Method for Flash Point by Continuously Closed
methodandnogeneralvalidcorrelationcanbeguaranteedbetweenresults
Cup (CCCFP) Tester
obtained by different test methods or where different test apparatus is
D6708 Practice for StatisticalAssessment and Improvement
specified.
of Expected Agreement Between Two Test Methods that
1.3 This test method utilizes a closed but unsealed cup with
Purport to Measure the Same Property of a Material
air injected into the test chamber.
E300 Practice for Sampling Industrial Chemicals
1.4 This test method is suitable for testing samples with a 3
2.2 ISO Standards:
flash point from 35 to 225°C.
ISO Guide 34 Quality Systems Guidelines for the Produc-
NOTE 2—Flash point determinations below 35°C and above 225°C may
tion of Reference Materials
be performed; however, the precision has not been determined below and
ISOGuide35 CertificationofReferenceMaterials—General
above these temperatures.
and Statistical Principles
1.5 If the user’s specification requires a defined flash point
method other than this method, neither this method nor any
3. Terminology
other test method should be substituted for the prescribed test
3.1 Definitions:
method without obtaining comparative data and an agreement
3.1.1 flash point, n—the lowest temperature corrected to a
from the specifier.
pressure of 101.3 kPa at which application of an ignition
1.6 The values stated in SI units are to be regarded as
source causes the vapors of a specimen of the sample to ignite
standard. No other units of measurement are included in this
momentarily under specified conditions of the test.
standard.
3.1.1.1 Discussion—For the purpose of this test method, the
1.6.1 Temperatures are in degrees Celsius, pressure in
test specimen is deemed to have flashed when the hot flame of
kilo-Pascals.
1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
D02.08 on Volatility. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2009. Published February 2010. Originally the ASTM website.
approved in 2004. Last previous edition approved in 2004 as D7094–04. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D7094-04R09. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7094−04 (2009)
TABLE 1 Volume of Introduced Air as a Function of
regulation. Consult the particular regulation involved for pre-
Sample Temperature
cise definitions of these classifications.
Sample Temperature Introduced Volume
5.3 This test method can be used to measure and describe
Range (°C) of Air (mL)
the properties of materials in response to heat and an ignition
below 80 0
80 to below 150 0.5 ± 0.15
source under controlled laboratory conditions and shall not be
150 to below 200 1 ± 0.2
used to describe or appraise the fire hazard or fire risk of
200 to below 300 1.5 ± 0.3
materials under actual fire conditions. However, results of this
300 and above 2 ± 0.4
test method may be used as elements of a fire risk assessment,
which takes into account all of the factors which are pertinent
to an assessment of the fire hazard of a particular end use.
the ignited vapor causes an instantaneous pressure increase of
5.4 Flash point can also indicate the possible presence of
at least 20 kPa inside the closed measuring chamber.
highly volatile and flammable materials in a relatively non-
3.1.2 dynamic, adj—the condition where the vapor above
volatile or nonflammable material, such as the contamination
the test specimen and the test specimen are not in temperature
of lubricating oils by small amounts of diesel fuel or gasoline.
equilibrium at the time at which the ignition source is applied.
Thistestmethodwasdesignedtobemoresensitivetopotential
contamination than Test Method D6450.
4. Summary of Test Method
4.1 The lid of the test chamber is regulated to a temperature
6. Apparatus
at least 18°C below the expected flash point.A2 6 0.2 mLtest
6.1 Flash Point Apparatus, Continuously Closed Cup
specimen of a sample is introduced into the sample cup. Both
Operation—The type of apparatus suitable for use in this test
specimen and cup are at a temperature at least 18°C below the
method employs a lid of solid brass, the temperature of which
expectedflashpoint;cooledifnecessary.Thecupisthenraised
is controlled electrically. Two temperature sensors for the
and pressed onto the lid of specified dimensions to form the
specimen and the lid temperatures, respectively, two arc pins
continuously closed but unsealed test chamber with an overall
for a high voltage arc, and a connecting tube for the pressure
volume of 7.0 6 0.3 mL.
monitoring and the air introduction are incorporated in the lid.
4.2 After closing the test chamber, the temperatures of the
Associated equipment for electrically controlling the chamber
testspecimenandtheregulatedlidareallowedtoequilibrateto
temperature is used, and a digital readout of the specimen
within1°C.Thenthelidisheatedataprescribed,constantrate.
temperatureisprovided.Theapparatusanditscriticalelements
For the flash tests, a high voltage arc of defined energy is
are shown in Figs. A1.1 and A1.2.
discharged inside the test chamber at regular intervals. After
6.1.1 Test Chamber—The test chamber is formed by the
each ignition, a variable amount of air (see Table 1)is
samplecupandthetemperaturecontrolledlidandshallhavean
introduced into the test chamber to provide the necessary
overall volume of 7 6 0.3 mL. A metal to metal contact
oxygen for the next flash test. The pressure inside the continu-
between the lid and the sample cup shall provide good heat
ously closed but unsealed test chamber remains at ambient
contactbutallowambientbarometricpressuretobemaintained
barometric pressure except for the short time during the air
inside the test chamber during the test. Critical dimensions are
introduction and at a flash point.
shown in Fig. A1.2. The pressure inside the measuring cham-
ber during the temperature increase is monitored.Aseal that is
4.3 After each arc application, the instantaneous pressure
increase above the ambient barometric pressure inside the test tootightresultsinapressureincreaseaboveambientduetothe
temperature and the vapor pressure of the sample.Apoor heat
chamber is monitored. When the pressure increase exceeds 20
kPa,thetemperatureatthatpointisrecordedastheuncorrected contact results in a bigger temperature difference between the
sample and the heated lid.
flash point, which is then corrected to barometric pressure.
6.1.2 Sample Cup—The sample cup shall be made of
5. Significance and Use
nickel-plated aluminum or other material with similar heat
conductivity.Itshallhaveanoverallvolumeof7 60.3mLand
5.1 The flash point temperature is one measure of the
shall be capable of containing 2 6 0.2 mL of sample. The
tendency of the test specimen to form a flammable mixture
critical dimensions and requirements are shown in Fig. A1.2.
with air under controlled laboratory conditions. It is only one
6.1.3 Specimen Temperature Sensor—The specimen tem-
of a number of properties which must be considered in
perature sensor (Fig. A1.1) shall be a thermocouple (NiCr-Ni
assessing the overall flammability hazard of a material.
or similar) in stainless steel of 1 mm diameter with a response
5.2 Flash point is used in shipping and safety regulations to
time of t(90)=3s.It shall be immersed to a depth of at least
define flammable and combustible materials and for classifica-
tion purposes. This definition may vary from regulation to
The sole source of supply of the continuously closed cup testers meeting these
The method of detecting the flash point by monitoring the instantaneous requirements known to the committee at this time are available from Grabner
pressure increase is covered by a patent. Interested parties are invited to submit Instruments,A-1220 Vienna/Austria, Dr. Otto-Neurath-Gasse 1. If you are aware of
information regarding the identification of an alternative(s) to this patented item to alternative suppliers, please provide this information to ASTM International
the ASTM International Headquarters. Your comments will receive careful consid- Headquarters.Your comments will receive careful consideration at a meeting of the
eration at a meeting of the responsible technical committee, which you may attend. responsible technical committee, which you may attend.
D7094−04 (2009)
2mmintothespecimen.Itshallhavearesolutionof0.1°Cand where such specifications are available. Other grades may be
a minimum accuracy of 6 0.2°C, preferably with a digital used, provided it is first ascertained that the reagent is of
sufficient purity to permit its use without lessening the accu-
readout.
racy of the determination.
6.1.4 Magnetic Stirring—The apparatus shall have provi-
7.1.1 Anisole—(Warning—See 7.2.)
sions for stirring of the sample. A rotating magnet outside the
7.1.2 Dodecane—(Warning—See 7.2.)
samplecupshalldriveasmallstirringmagnetwhichisinserted
7.2 Cleaning Solvents—Use only noncorrosive solvents ca-
into the sample cup after sample introduction. The stirring
pable of cleaning the sample cup and the lid. Two commonly
magnetshallhaveadiameterof3 60.2mmandalengthof12
used solvents are toluene and acetone. (Warning—Anisole,
6 1 mm. The rotation speed of the driving magnet shall be
dodecane, toluene, acetone, and many solvents are flammable
between 250 and 270 rev/min.
and are health hazards. Dispose of solvents and waste material
6.1.5 Air Introduction—The apparatus shall have provisions
in accordance with local regulations.)
for introduction of air immediately after each flash test.The air
shall be introduced by a short air pulse from a small membrane
8. Sampling
compressor by means of a T-inlet in the connecting tube to the
8.1 Obtain at least a 50 mL sample from a bulk test site in
pressuretransducer.Thevolumeoftheintroducedair,from0.5
accordance with the instructions given in Practice D4057,
to 2 mL, is dependent on the sample temperature (see Table 1).
D4177,or E300. Store the sample in a clean, tightly sealed
6.1.6 Electricalheatingandthermoelectriccoolingofthelid
container at a low temperature.
(see the Peltier element shown in Fig. A1.1) shall be used to
8.2 Do not store samples for an extended period of time in
regulate the temperature of the test chamber for the duration of
gas permeable containers, such as plastic, because volatile
the test. The temperature regulation shall have a minimum
material may diffuse through the walls of the container.
accuracy of 6 0.2°C.
Discard samples in leaky containers and obtain new samples.
6.1.7 A high voltage electric arc shall be used for the
8.3 Erroneously high flash points can be obtained when
ignition of the flammable vapor. The energy of the arc shall be
precautions are not taken to avoid loss of volatile material. Do
1.3 6 0.3 J (1.3 6 0.3 Ws) per arc and the energy shall be
not open containers unnecessarily. Do not make a transfer
applied within 19 6 2 m/s. (Warning— Because samples
unless the sample temperature is at least 18°C below the
containing low flash material or having a flash point below the
expected flash point.When possible, perform the flash point as
preset initial temperature can oversaturate the vapor inside the
the first test.
chamber and hence prohibit the detection of a flash point in the
8.4 Samples of very viscous materials may be warmed until
chosen range, a precautionary arc set at 5°C intervals is
they are reasonably fluid before they are tested. However, do
required while the lid and sample cup temperatures are
not heat the unsealed sample above a temperature of 18°C
equalizing.)
below its expected flash point.
6.1.8 The pressure transducer for the flash point detection
8.5 Samples containing dissolved or free water may be
shall be connected to the connecting tube in the lid and shall
dehydrated with calcium chloride or by filtering through a
have a minimum operational range from 80 to 177 kPa with a
qualitative filter paper or a loose plug of dry absorbent cotton.
minimum resolution of 0.1 kPa and a minimum accuracy of 6
Warming the sample is permitted, but it should not be heated
0.5 kPa. It shall be capable of detecting an instantaneous
above a temperature of 18°C below its expected flash point.
pressure increase above barometric pressure of a minimum of
(Warning—Because samples containing volatile materia
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.