ASTM D6450-05(2010)
(Test Method)Standard Test Method for Flash Point by Continuously Closed Cup (CCCFP) Tester
Standard Test Method for Flash Point by Continuously Closed Cup (CCCFP) 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 that 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 classify them. 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 that 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.
SCOPE
1.1 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 with test apparatus different from that specified.
1.2 This test method covers the determination of the flash point of fuel oils, lube oils, solvents, and other liquids by a continuously closed cup tester. The measurement is made on a test specimen of 1 mL.
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 10 to 250°C.
Note 2—Flash point determinations below 10°C and above 250°C can 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 test method, neither this test method nor any other method should be substituted for the prescribed 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. Temperatures are in degrees Celsius, and pressure is 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. Specific warning statements appear throughout the standard.
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Designation: D6450 − 05(Reapproved 2010)
Standard Test Method for
Flash Point by Continuously Closed Cup (CCCFP) Tester
This standard is issued under the fixed designation D6450; 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 flash point test method is a dynamic method and
responsibility of the user of this standard to establish appro-
depends on definite rates of temperature increase. It is one of
priate safety and health practices and determine the applica-
the many flash point test methods available, and every flash
bility of regulatory limitations prior to use. Specific warning
point test method, including this one, is an empirical method.
statements appear throughout the standard.
NOTE 1—Flash point values are not a constant physical-chemical
property of materials tested. They are a function of the apparatus design,
2. Referenced Documents
the condition of the apparatus used, and the operational procedure carried
2.1 ASTM Standards:
out. Flash point can therefore only be defined in terms of a standard test
method, and no general valid correlation can be guaranteed between D4057 Practice for Manual Sampling of Petroleum and
results obtained by different test methods or with test apparatus different
Petroleum Products
from that specified.
D4177 Practice for Automatic Sampling of Petroleum and
1.2 This test method covers the determination of the flash Petroleum Products
point of fuel oils, lube oils, solvents, and other liquids by a
D6299 Practice for Applying Statistical Quality Assurance
continuously closed cup tester. The measurement is made on a and Control Charting Techniques to Evaluate Analytical
test specimen of 1 mL.
Measurement System Performance
D6300 Practice for Determination of Precision and Bias
1.3 This test method utilizes a closed but unsealed cup with
Data for Use in Test Methods for Petroleum Products and
air injected into the test chamber.
Lubricants
1.4 This test method is suitable for testing samples with a
E300 Practice for Sampling Industrial Chemicals
flash point from 10 to 250°C. 3
2.2 ISO Standards:
NOTE 2—Flash point determinations below 10°C and above 250°C can ISO Guide 34 Quality Systems Guidelines for the Produc-
be performed; however, the precision has not been determined below and
tion of Reference Materials
above these temperatures.
ISOGuide35 CertificationsofReferenceMaterial–General
1.5 If the user’s specification requires a defined flash point and Statistical Principles
methodotherthanthistestmethod,neitherthistestmethodnor
3. Terminology
any other method should be substituted for the prescribed
method without obtaining comparative data and an agreement
3.1 Definitions:
from the specifier. 3.1.1 dynamic, adj—the condition in which the vapor above
the test specimen and the test specimen are not in temperature
1.6 The values stated in SI units are to be regarded as
equilibrium at the time at which the ignition source is applied.
standard. No other units of measurement are included in this
standard. Temperatures are in degrees Celsius, and pressure is 3.1.2 flash point, n—the lowest temperature corrected to a
pressure of 101.3 kPa at which application of an ignition
in 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 Lubricants and 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 Oct. 1, 2010. Published November 2010. Originally the ASTM website.
approved in 1999. Last previous edition approved in 2005 as D6450–05. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D6450-05R10. 4th Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6450 − 05 (2010)
source causes the vapors of a specimen of the sample to ignite 5.4 Flash point can also indicate the possible presence of
momentarily under specified conditions of the test. highly volatile and flammable materials in a relatively non-
3.1.2.1 Discussion—For the purpose of this test method, the volatile or nonflammable material, such as the contamination
test specimen is deemed to have flashed when the hot flame of of lubricating oils by small amounts of diesel fuel or gasoline.
the ignited vapor causes an instantaneous pressure increase of
6. Apparatus
at least 20 kPa inside the closed measuring chamber.
6.1 Flash Point Apparatus, Continuously Closed Cup
4. Summary of Test Method
Operation—The type of apparatus suitable for use in this test
method employs a lid of solid brass, the temperature of which
4.1 The lid of the test chamber is regulated to a temperature
at least 18°C below the expected flash point.A1 6 0.1 mLtest is controlled electrically. Two temperature sensors for the
specimen and the lid temperatures, respectively, two electri-
specimen of a sample is introduced into the sample cup,
ensuring that both specimen and cup are at a temperature at cally insulated pins for a high voltage arc, and a connecting
tube for the pressure monitoring and the air introduction are
least 18°C below the expected flash point, cooling if necessary.
incorporated in the lid. Associated equipment for electrically
The cup is then raised and pressed onto the lid of specified
dimensions to form the continuously closed but unsealed test controlling the chamber temperature is used, and a digital
readout of the specimen temperature is provided. The appara-
chamber with an overall volume of 4.0 6 0.2 mL.
tus and its critical elements are shown in Fig. A1.1 and Fig.
4.2 After closing the test chamber, the temperatures of the
A1.2.
testspecimenandtheregulatedlidareallowedtoequilibrateto
6.1.1 Test Chamber—The test chamber is formed by the
within1°C.Thenthelidisheatedataprescribed,constantrate.
samplecupandthetemperaturecontrolledlidandshallhavean
Fortheflashtests,anarcofdefinedenergyisdischargedinside
overall volume of 4 6 0.2 mL. A metal to metal contact
the test chamber at regular intervals.After each ignition, 1.5 6
between the lid and the sample cup shall provide good heat
0.5 mLof air is introduced into the test chamber to provide the
contactbutallowambientbarometricpressuretobemaintained
necessaryoxygenforthenextflashtest.Thepressureinsidethe
inside the test chamber during the test. Critical dimensions are
continuously closed but unsealed test chamber remains at
shown in Fig. A1.2. The pressure inside the measuring cham-
ambient barometric pressure, except for the short time during
ber during the temperature increase is monitored.Aseal that is
the air introduction and except at a flash point.
tootightresultsinapressureincreaseaboveambientduetothe
4.3 After each arc, the instantaneous pressure increase
temperature and the vapor pressure of the sample.Apoor heat
above the ambient barometric pressure inside the test chamber
contact results in a bigger temperature difference between the
is monitored. When the pressure increase exceeds a defined
sample and the heated lid.
threshold, the temperature at that point is recorded as the
6.1.2 Sample Cup—The sample cup shall be made of
uncorrected flash point.
nickel-plated aluminum or other material with similar heat
conductivity. It shall have an overall volume of 4 mLand shall
5. Significance and Use
be capable of containing 1 6 0.1 mL of sample. The critical
5.1 The flash point temperature is one measure of the dimensions and requirements are shown in Fig. A1.2.
tendency of the test specimen to form a flammable mixture
6.1.3 Specimen Temperature Sensor—The specimen tem-
with air under controlled laboratory conditions. It is only one perature sensor (Fig. A1.1: Ts) shall be a thermocouple
of a number of properties that must be considered in assessing
(NiCr-Ni or similar) in stainless steel of 1-mm diameter with a
the overall flammability hazard of a material. response time of t(90)=3s.It shall be immersed to a depth of
at least 2 mm into the specimen. It shall have a resolution of
5.2 Flash point is used in shipping and safety regulations to
0.1°C and a minimum accuracy of 6 0.2°C, preferably with a
define flammable and combustible materials and classify them.
digital readout.
Thisdefinitionmayvaryfromregulationtoregulation.Consult
6.1.4 Magnetic Stirring—The apparatus shall have provi-
the particular regulation involved for precise definitions of
sions for stirring the sample. A rotating magnet outside the
these classifications.
sample cup shall drive a small stirring magnet, which is
5.3 This test method can be used to measure and describe
inserted into the sample cup after sample introduction. The
the properties of materials in response to heat and an ignition
stirring magnet shall have a diameter of 3 6 0.2 mm and a
source under controlled laboratory conditions and shall not be
lengthof12 61mm.Therotationspeedofthedrivingmagnet
used to describe or appraise the fire hazard or fire risk of
shall be between 250 and 270 rev/min.
materials under actual fire conditions. However, results of this
6.1.5 Air Introduction—The apparatus shall have provisions
test method may be used as elements of a fire risk assessment,
for introduction of 1.5 6 0.5 mLof air immediately after each
which takes into account all of the factors that are pertinent to
flash test. The air shall be introduced by a short air pulse from
an assessment of the fire hazard of a particular end use.
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 is Grabner Instruments, A-1220
pressure increase is covered by a patent. Interested parties are invited to submit Vienna, Dr. Otto Neurathgasse 1,Austria. If you are aware of alternative suppliers,
information regarding the identification of an alternative(s) to this patented item to please provide this information to ASTM International Headquarters. Your com-
ASTMHeadquarters.Yourcommentswillreceivecarefulconsiderationatameeting ments will receive careful consideration at a meeting of the responsible technical
of the responsible technical committee, which you may attend. committee , which you may attend.
D6450 − 05 (2010)
a small membrane compressor by means of a T-inlet in the used solvents are toluene and acetone. (Warning—Flammable
connecting tube to the pressure transducer. and a health hazard. Dispose of solvents and waste material in
6.1.6 Electricalheatingandthermoelectriccoolingofthelid accordance with local regulations.)
(Fig.A1.1: PE) shall be used to regulate the temperature of the
test chamber for the duration of the test. The temperature
8. Sampling
regulation shall have a minimum accuracy of 6 0.2°C.
8.1 Obtain at least a 50 mL sample from a bulk test site in
6.1.7 A high voltage electric arc shall be used for the
accordance and instruction given in Practice D4057, D4177,or
ignition of the flammable vapor. The energy of the arc shall be
E300. Store the sample in a clean, tightly sealed container at a
3 6 0.5 mJ (3 6 0.5 Ws) per arc, and the energy shall be
low temperature.
applied within 43 6 3 ms. (Warning—Because samples
8.2 Do not store samples for an extended period of time in
containing low flash material or having a flash point below the
gas permeable containers, such as plastic, because volatile
preset initial temperature can oversaturate the vapor inside the
material may diffuse through the walls of the container.
chamber and hence prohibit the detection of a flash point in the
Discard samples in leaky containers and obtain new samples.
chosen range, the design of the apparatus should incorporate
step-wise ignitions in steps of 10°C, following the closing of
8.3 Erroneously high flash points can be obtained when
the measuring chamber and before the sample reaches the
precautions are not taken to avoid loss of volatile material. Do
initial temperature of the test.)
not open containers unnecessarily. Do not make a transfer
6.1.8 The pressure transducer for the flash point detection
unless the sample temperature is at least 18°C below the
shall be connected to the connecting tube in the lid and shall
expected flash point.When possible, perform the flash point as
have a minimum operational range from 80 to 177 kPa with a
the first test.
minimum resolution of 0.1 kPa and a minimum accuracy of
8.4 Samples of very viscous materials may be warmed until
60.5 kPa. It shall be capable of detecting an instantaneous
they are reasonably fluid before they are tested. However, do
pressure increase above barometric pressure of a minimum of
not heat the unsealed sample above a temperature of 18°C
20 kPa within 100 ms.
below its expected flash point.
NOTE 3—The monitoring of the instantaneous pressure increase above
8.5 Samples containing dissolved or free water may be
barometric pressure is one of several methods used to determine a flash
dehydrated with calcium chloride or by filtering through a
inside the test chamber. A pressure increase of 20 kPa corresponds to a
qualitative filter paper or a loose plug of dry absorbent cotton.
flame volume of approximately 1.5 mL.
NOTE 4—An automatic barometric correction, which is performed in Warming the sample is permitted, but do not heat the sample
accordance with the procedure described in 12.1, can be installed in the
above a temperature of 18°C below its expected flash point.
tester. The absolute pressure reading of the pressure transducer described
(Warning—Because samples containing volatile material will
in 6.1.8 may be used for the correction.
lose volatiles and then yield incorrectly high flash points, the
6.1.9 The introduction of a test portion of 1.0 6 0.1 mL
treatment described in 8.4 and 8.5 is not suitable for such
shall be accomplished by the use of a pipette or syringe of the
samples.)
required accuracy.
9. Quality Control Checks
7. Reagents and Materials
9.1 Verify the performance of the instrument at least once
7.1 Purity of Reagents—Use only chemicals of purity re-
per year by determining the flash point of a certified reference
quested in Table X1.1. Unless otherwise indicated, it is
material (CRM) such as those listed in
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