ASTM D6450-16a(2021)
(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
5.1 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.
5.2 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.
5.3 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.
5.4 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 °C 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements appear throughout the standard.
1.8 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D6450 − 16a (Reapproved 2021)
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 mine the applicability of regulatory limitations prior to use.
Specific warning statements appear throughout the standard.
1.1 This flash point test method is a dynamic method and
1.8 This international standard was developed in accor-
depends on definite rates of temperature increase. It is one of
dance with internationally recognized principles on standard-
the many flash point test methods available, and every flash
ization established in the Decision on Principles for the
point test method, including this one, is an empirical method.
Development of International Standards, Guides and Recom-
NOTE 1—Flash point values are not a constant physical-chemical
mendations issued by the World Trade Organization Technical
property of materials tested. They are a function of the apparatus design,
Barriers to Trade (TBT) Committee.
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
2. Referenced Documents
method, and no general valid correlation can be guaranteed between
results obtained by different test methods or with test apparatus different 2
2.1 ASTM Standards:
from that specified.
D4057 Practice for Manual 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
D4177 Practice for Automatic Sampling of Petroleum and
continuously closed cup tester. The measurement is made on a
Petroleum Products
test specimen of 1 mL.
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
1.3 This test method utilizes a closed but unsealed cup with
air injected into the test chamber. Measurement System Performance
D6300 Practice for Determination of Precision and Bias
1.4 This test method is suitable for testing samples with a
Data for Use in Test Methods for Petroleum Products,
flash point from 10 °C to 250 °C.
Liquid Fuels, and Lubricants
NOTE2—Flashpointdeterminationsbelow10 °Candabove250 °Ccan
E300 Practice for Sampling Industrial Chemicals
be performed; however, the precision has not been determined below and
2.2 ISO Standards:
above these temperatures.
ISO Guide 34 General requirements for the competence of
1.5 If the user’s specification requires a defined flash point
reference material producers
methodotherthanthistestmethod,neitherthistestmethodnor
ISO Guide 35 Reference materials—General and statistical
any other method should be substituted for the prescribed
principles for certification
method without obtaining comparative data and an agreement
from the specifier.
3. Terminology
1.6 The values stated in SI units are to be regarded as
3.1 Definitions:
standard. No other units of measurement are included in this
3.1.1 dynamic, adj—the condition in which the vapor above
standard. Temperatures are in degrees Celsius, and pressure is
the test specimen and the test specimen are not in temperature
in kilo-pascals.
equilibrium at the time at which the ignition source is applied.
1.7 This standard does not purport to address all of the
3.1.2 flash point, n—in flash point test methods, the lowest
safety concerns, if any, associated with its use. It is the
temperature of the test specimen, adjusted to account for
responsibility of the user of this standard to establish appro-
variations in atmospheric pressure from 101.3 kPa, at which
priate safety, health, and environmental practices and deter-
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, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee D02.08 on Volatility. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved July 1, 2021. Published July 2021. Originally approved the ASTM website.
in 1999. Last previous edition approved in 2016 as D6450 – 16a. DOI: 10.1520/ Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
D6450-16AR21. 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
D6450 − 16a (2021)
application of an ignition source causes the vapors of the test 6. Apparatus
specimen to ignite momentarily under specified conditions of
6.1 Flash Point Apparatus, Continuously Closed Cup
the test.
Operation—The type of apparatus suitable for use in this test
3.1.2.1 Discussion—For the purpose of this test method, the
method employs a lid of solid brass, the temperature of which
test specimen is deemed to have flashed when the hot flame of
is controlled electrically. Two temperature sensors for the
the ignited vapor causes an instantaneous pressure increase of
specimen and the lid temperatures, respectively, two electri-
at least 20 kPa inside the closed measuring chamber.
cally insulated pins for a high voltage arc, and a connecting
tube for the pressure monitoring and the air introduction are
4. Summary of Test Method
incorporated in the lid. Associated equipment for electrically
4.1 The lid of the test chamber is regulated to a temperature
controlling the chamber temperature is used, and a digital
atleast18 °Cbelowtheexpectedflashpoint.A1 mL 60.1mL
readout of the specimen temperature is provided. The appara-
test specimen of a sample is introduced into the sample cup,
tus and its critical elements are shown in Fig. A1.1 and Fig.
ensuring that both specimen and cup are at a temperature at
A1.2.
least 18 °C below the expected flash point, cooling if neces-
6.1.1 Test Chamber—The test chamber is formed by the
sary.Thecupisthenraisedandpressedontothelidofspecified
samplecupandthetemperaturecontrolledlidandshallhavean
dimensions to form the continuously closed but unsealed test
overall volume of 4 mL 6 0.2 mL. A metal to metal contact
chamber with an overall volume of 4.0 mL 6 0.2 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
within 1 °C. Then the lid is heated at a prescribed, constant
shown in Fig. A1.2. The pressure inside the measuring cham-
rate. For the flash tests, an arc of defined energy is discharged
ber during the temperature increase is monitored.Aseal that is
inside the test chamber at regular intervals.After each ignition,
tootightresultsinapressureincreaseaboveambientduetothe
1.5 mL 6 0.5 mL of air is introduced into the test chamber to
temperature and the vapor pressure of the sample.Apoor heat
provide the necessary oxygen for the next flash test. The
contact results in a bigger temperature difference between the
pressure inside the continuously closed but unsealed test
sample and the heated lid.
chamber remains at ambient barometric pressure, except for
6.1.2 Sample Cup—The sample cup shall be made of
the short time during the air introduction and except at a flash
nickel-plated aluminum or other material with similar heat
point.
conductivity. It shall have an overall volume of 4 mLand shall
be capable of containing 1 mL 6 0.1 mL of sample. The
4.3 After each arc, the instantaneous pressure increase
critical dimensions and requirements are shown in Fig. A1.2.
above the ambient barometric pressure inside the test chamber
6.1.3 Specimen Temperature Sensor—The specimen tem-
is monitored. When the pressure increase exceeds a defined
perature sensor (Fig. A1.1: Ts) shall be a thermocouple
threshold, the temperature at that point is recorded as the
(NiCr-Ni or similar) in stainless steel of 1 mm diameter with a
uncorrected flash point.
response time of t(90)=3s.It shall be immersed to a depth of
5. Significance and Use
at least 2 mm into the specimen. It shall have a resolution of
0.1 °C and a minimum accuracy of 6 0.2 °C, preferably with
5.1 The flash point temperature is one measure of the
a digital readout.
tendency of the test specimen to form a flammable mixture
6.1.4 Magnetic Stirring—The apparatus shall have provi-
with air under controlled laboratory conditions. It is only one
sions for stirring the sample. A rotating magnet outside the
of a number of properties that must be considered in assessing
sample cup shall drive a small stirring magnet, which is
the overall flammability hazard of a material.
inserted into the sample cup after sample introduction. The
5.2 Flash point is used in shipping and safety regulations to
stirring magnet shall have a diameter of 3 mm 6 0.2 mm and
define flammable and combustible materials and classify them.
a length of 12 mm 6 1 mm. The rotation speed of the driving
Thisdefinitionmayvaryfromregulationtoregulation.Consult
magnet shall be between 250 rev/min and 270 rev/min.
the particular regulation involved for precise definitions of
6.1.5 Air Introduction—The apparatus shall have provisions
these classifications.
for introduction of 1.5 mL 6 0.5 mL of air immediately after
5.3 This test method can be used to measure and describe
each flash test. The air shall be introduced by a short air pulse
the properties of materials in response to heat and an ignition
from a small membrane compressor by means of a T-inlet in
source under controlled laboratory conditions and shall not be
the connecting tube to the pressure transducer.
used to describe or appraise the fire hazard or fire risk of
6.1.6 Electricalheatingandthermoelectriccoolingofthelid
materials under actual fire conditions. However, results of this
(Fig.A1.1: PE) shall be used to regulate the temperature of the
test method may be used as elements of a fire risk assessment,
test chamber for the duration of the test. The temperature
which takes into account all of the factors that are pertinent to
regulation shall have a minimum accuracy of 6 0.2 °C.
an assessment of the fire hazard of a particular end use.
6.1.7 A high voltage electric arc shall be used for the
5.4 Flash point can also indicate the possible presence of ignition of the flammable vapor. The energy of the arc shall be
highly volatile and flammable materials in a relatively non- 3mJ 6 0.5 mJ (3 Ws 6 0.5 Ws) per arc, and the energy shall
volatile or nonflammable material, such as the contamination beappliedwithin43 ms 63ms.(Warning—Becausesamples
of lubricating oils by small amounts of diesel fuel or gasoline. containing low flash material or having a flash point below the
D6450 − 16a (2021)
preset initial temperature can oversaturate the vapor inside the 8.2 Do not store samples for an extended period of time in
chamber and hence prohibit the detection of a flash point in the gas permeable containers, such as plastic, because volatile
chosen range, the design of the apparatus should incorporate material may diffuse through the walls of the container.
step-wise ignitions in steps of 10 °C, following the closing of Discard samples in leaky containers and obtain new samples.
the measuring chamber and before the sample reaches the
8.3 Erroneously high flash points can be obtained when
initial temperature of the test.)
precautions are not taken to avoid loss of volatile material. Do
6.1.8 The pressure transducer for the flash point detection
not open containers unnecessarily. Do not make a transfer
shall be connected to the connecting tube in the lid and shall
unless the sample temperature is at least 18 °C below the
have a minimum operational range from 80 kPa to 177 kPa
expected flash point. When possible, perform the flash point as
with a minimum resolution of 0.1 kPa and a minimum
the first test.
accuracy of 60.5 kPa. It shall be capable of detecting an
8.4 Samples of very viscous materials may be warmed until
instantaneous pressure increase above barometric pressure of a
they are reasonably fluid before they are tested. However, do
minimum of 20 kPa within 100 ms.
not heat the unsealed sample above a temperature of 18 °C
NOTE 3—The monitoring of the instantaneous pressure increase above
below its expected flash point.
barometric pressure is one of several methods used to determine a flash
inside the test chamber. A pressure increase of 20 kPa corresponds to a 8.5 Samples containing dissolved or free water may be
flame volume of approximately 1.5 mL.
dehydrated with calcium chloride or by filtering through a
NOTE 4—An automatic barometric correction, which is performed in
qualitative filter paper or a loose plug of dry absorbent cotton.
accordance with the procedure described in 12.1, can be installed in the
Warming the sample is permitted, but do not heat the sample
tester. The absolute pressure reading of the pressure transducer described
above a temperature of 18 °C below its expected flash point.
in 6.1.8 may be used for the correction.
(Warning—Because samples containing volatile material will
6.1.9 The introduction of a test portion of 1.0 mL 6 0.1 mL
lose volatiles and then yield incorrectly high flash points, the
shall be accomplished by the use of a pipette or syringe of the
treatment described in 8.4 and 8.5 is not suitable for such
required accuracy.
samples.)
7. Reagents and Materials
9. Quality Control Checks
7.1 Purity of Reagents—Use only chemicals of purity re-
9.1 Verify the performance of the instrument at least once
quested in Table X1.1. Unless otherwise indicated, it is
per year by determining the flash point of a certified reference
intended that all reagents conform to the specifications of the
material (CRM) such as those listed in Appendix X1, which is
Committee on Analytical Reagents of the American Chemical
reasonably close to the expected temperature range of the
Society where such specifications are available. Other grades
samples to be tested.The material shall be tested in accordance
may be used, provided it is first ascertained that the reagent is
with Section 11 of this test method, and the observed flash
of sufficient purit
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