ASTM D3278-96(2004)e1
(Test Method)Standard Test Methods for Flash Point of Liquids by Small Scale Closed-Cup Apparatus
Standard Test Methods for Flash Point of Liquids by Small Scale Closed-Cup Apparatus
SIGNIFICANCE AND USE
Flash point is one of the properties used to define the flammability of a liquid. It is used to classify liquids according to their flammability by governmental regulatory agencies. It may also be used to determine the presence of impurities or contaminants in a given liquid, such as the presence of residual solvents in solvent-refined drying oils. See Test Methods D 56 and D 93 for alternate flash point testing.
SCOPE
1.1 These test methods cover procedures for determining whether a material does or does not flash at a specified temperature or for determining the lowest finite temperature at which a material does flash when using a small scale closed-cup apparatus. The test methods are applicable to paints, enamels, lacquers, varnishes, and related products having a flash point between 0 and 110C (32 and 230F) and viscosity lower than 150 St at 25C (77F). Note 1Tests at higher or lower temperatures are possible.Note 2
More viscous materials may be tested in accordance with .Note 3
Organic peroxides may be tested in accordance with , which describes the applicable safety precautions.Note 4
The U.S. Department of Labor (OSHA, Hazard Communications), the U.S. Department of Transportation (RSPA), and the U.S. Environmental Protection Agency (EPA) have specified Test Methods D 3278 as one of several acceptable methods for the determination of flash point of liquids in their regulations.Note 5
These test methods are similar to International Standards ISO 3679 and ISO 3680.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.3 This standard should be used to measure and describe the response of materials, products, or assemblies to heat and flame under controlled conditions and should not be used to describe or appraise the fire-hazard or fire-risk of materials, products, or assemblies under actual fire conditions. However, results of the test may be used as elements of a fire-hazard or a fire-risk assessment which takes into account all of the factors which are pertinent to an assessment of the fire hazard or fire risk of a particular end use
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 hazard statements, see and .
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Designation:D3278–96(Reapproved2004)
Standard Test Methods for
Flash Point of Liquids by Small Scale Closed-Cup
Apparatus
This standard is issued under the fixed designation D3278; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
´ NOTE—Warning notes were editorially moved into the text in November 2004.
1. Scope a fire-risk assessment which takes into account all of the
factors which are pertinent to an assessment of the fire hazard
1.1 These test methods cover procedures for determining
or fire risk of a particular end use.
whether a material does or does not flash at a specified
1.4 This standard does not purport to address all of the
temperature or for determining the lowest finite temperature at
safety concerns, if any, associated with its use. It is the
which a material does flash when using a small scale closed-
2 responsibility of the user of this standard to establish appro-
cup apparatus. The test methods are applicable to paints,
priate safety and health practices and determine the applica-
enamels, lacquers, varnishes, and related products having a
bility of regulatory limitations prior to use. For specific hazard
flash point between 0 and 110°C (32 and 230°F) and viscosity
statements, see 8.1 and 11.2.
lower than 150 St at 25°C (77°F).
NOTE 1—Tests at higher or lower temperatures are possible. 2. Referenced Documents
NOTE 2—More viscous materials may be tested in accordance with
2.1 ASTM Standards:
Annex A4.
D56 Test Method for Flash Point byTag Closed CupTester
NOTE 3—Organic peroxides may be tested in accordance with Annex
D93 Test Methods for Flash Point by Pensky-Martens
A5, which describes the applicable safety precautions.
Closed Cup Tester
NOTE 4—The U.S. Department of Labor (OSHA, Hazard Communica-
tions), the U.S. Department of Transportation (RSPA), and the U.S.
D850 Test Method for Distillation of Industrial Aromatic
Environmental Protection Agency (EPA) have specified Test Methods
Hydrocarbons and Related Materials
D3278asoneofseveralacceptablemethodsforthedeterminationofflash
D1015 Test Method for Freezing Points of High-Purity
point of liquids in their regulations.
Hydrocarbons
NOTE 5—These test methods are similar to International Standards
D1078 Test Method for Distillation Range of Volatile Or-
ISO3679 and ISO3680.
ganic Liquids
1.2 The values stated in SI units are to be regarded as the
2.2 ISO Standards:
standard. The values given in parentheses are for information
ISO 3679 Paints, varnishes, petroleum and related
only.
products—Determination of flash point—Rapid equilib-
1.3 This standard should be used to measure and describe
rium method
the response of materials, products, or assemblies to heat and
ISO 3680 Paints, varnishes, petroleum and related
flame under controlled conditions and should not be used to
products—Flash/no flash test—Rapid equilibrium method
describe or appraise the fire-hazard or fire-risk of materials,
products, or assemblies under actual fire conditions. However,
3. Terminology
results of the test may be used as elements of a fire-hazard or
3.1 Definitions:
These test methods are under the jurisdiction of ASTM Committee D01 on
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.21 on Chemical Analysis of Paints and Paint For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Materials. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Nov. 1, 2004. Published November 2004. Originally Standards volume information, refer to the standard’s Document Summary page on
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approved in 1973. Last previous edition approved in 1996 as D3278–96 . DOI: the ASTM website.
10.1520/D3278-96R04E01. Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
Small scale closed-cup apparatus has been found suitable for this purpose. 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.
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D3278–96 (2004)
3.1.1 flash point, n—the lowest temperature, corrected to a 7. Reagents and Materials
pressure of 760 mm Hg (101.3 kPa, 1013 mbar), at which
7.1 p-Xylene, reference standard.
application of an ignition source causes the vapor of the
7.2 n-Butanol, reference standard.
specimen to ignite under specified conditions of test.
7.3 Cooling Mixtures of ice and water or solid CO (dry
ice) and acetone.
4. Summary of Test Methods
7.4 Liquified Petroleum Gas.
4.1 Bymeansofasyringe,2mLofthesampleisintroduced
7.5 Heat Transfer Paste.
through a leakproof entry port into the tightly closed small
scale closed-cup apparatus or directly into the cup that has
8. Sampling
been brought to the required test temperature. As a flash/no
flash test, the expected flash point temperature may be a 8.1 The specimen size for each test is 2 mL. Obtain at least
a25-mLsamplefromthebulksourceandstoreinanearlyfull,
specificationorotheroperatingrequirement.After1min,atest
flameisappliedinsidethecupandnoteistakenwhetherornot tightly closed, clean glass container or in other container
suitable for the type of liquid being sampled. (Warning—
the test specimen flashes. A fresh specimen must be used if a
repeat test is necessary. Erroneously high flash points may be obtained if precautions
are not taken to avoid loss of volatile material. Do not open
4.2 For a finite flash point measurement, the temperature is
sample containers unnecessarily and do not transfer the speci-
sequentially increased through the anticipated range, the test
men to the cup unless the temperature of the specimen is at
flame being applied at 5°C (9°F) intervals until a flash is
least 10°C (20°F) below the expected flash point. Discard
observed. A true determination is then made using a fresh
samplesinleakycontainers.)(Warning—Donotstoresamples
specimen,startingthetestatthetemperatureofthelastinterval
inplasticbottles(polyethylene,polypropylene,etc.),asvolatile
before the flash point of the material and making tests at
material may diffuse through the walls.)
increasing 0.5°C (1°F) intervals.
9. Preparation of Apparatus
5. Significance and Use
9.1 Prior to initial use or after removal of the thermometer,
5.1 Flash point is one of the properties used to define the
insert the thermometer into its pocket (see Fig. A1.1) with a
flammability of a liquid. It is used to classify liquids according
good heat transfer paste.
to their flammability by governmental regulatory agencies. It
9.2 To help in making the necessary settings during a test,
may also be used to determine the presence of impurities or
before the initial use determine the relationship between the
contaminantsinagivenliquid,suchasthepresenceofresidual
temperature control dial and thermometer readings at intervals
solvents in solvent-refined drying oils. See Test Methods D56
not over 5°C (9°F) throughout the scale range of the heater.
and D93 for alternate flash point testing.
9.3 Place the tester in a subdued light and in a position not
6. Apparatus exposed to disturbing drafts. Provide a black-coated shield, if
necessary.
6.1 Test Cup and Cover Assembly —The essential dimen-
9.4 Read the manufacturer’s operating and maintenance
sionsandrequirementsoftheapparatusareshowninFig.A1.1
instructionsonthecareandservicingofthetester.Observethe
and described in Annex A1.
specific suggestions regarding the operation of the various
6.2 Thermometers, low, medium, high temperature small
controls.
scale. Test to determine that the scale error does not exceed
9.5 Check the accuracy of the tester by duplicate determi-
0.25°C(0.5°F).Theuseofamagnifyinglensassistsinmaking
nation of the flash point of the p-xylene reference standard
temperature observations.
(Annex A3). The mean of the results should be 27.2 6 0.8°C
6.3 Glass Syringe,2 6 0.1-mL capacity at 25°C (77°F), to
(81 6 1.5°F). An additional reference standard, n-butanol
provide a means of taking a uniform specimen. Check the
(Annex A3), may be used to check the accuracy at approxi-
capacity by discharging water into a weighing bottle and
matelythetemperaturespecifiedbyU.S.regulatoryagenciesin
weighing.Adjust plunger if necessary.Adisposable syringe of
defining flammable liquids. The mean of duplicates should be
equal precision may be used.
36.7 6 0.8°C (98 6 1.5°F). If not, remove the thermometer
6.4 Aluminum Cooling Block (describing in Annex A2),
andobservewhethersufficientheattransferpastesurroundsthe
thatfitssnuglywithinthetestcupusedforrapidcoolingofthe
thermometer to provide good heat transfer from the cup to the
sample cup.
thermometer.
6.5 Barometer.
p-Xyleneisavailableas“FlashPointCheckFluid”fromSpecialProductsDiv.,
Closed-cupflashpointtestersandtheiraccessoriesmeetingtherequirementsof Chemical Dept., Phillips Petroleum Co., Borger, TX 25303.
the unit shown in Fig. A1.1 are available from ERDCO Engineering Corp., 721 n-Butanol may be obtained from chemical supply companies.
Custer Ave., Evanston, IL 60202 or Stanhope-Seta Ltd., Park Close Englefield Heat transfer paste is available from the suppliers of the Small Scale Tester.
Green, Engham, Surrey, TW20 OXD, England. No. 340 Silicone is available from Dow Corning Corp., 2030 Willard H. Dow
Thermometers may be obtained from the suppliers of the Small Scale Tester. Center, Midland, MI 48674. G641 Heat Transfer Compound is available from
Cooling blocks may be obtained from ERDCO Engineering Corp. GeneralElectricCo.,ProductsDiv.,12CorporateWoodsBlvd.,Albany,NY12211.
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D3278–96 (2004)
TEST METHOD A—FLASH/NO FLASH coolingmixtureintothesamplewell.Drythecupwithapaper
tissue to remove any collected moisture prior to adding the
10. Procedure—Ambient to 110°C (230°F)
specimen using a precooled syringe. (Warning—Be careful in
10.1 Inspect the inside of the test cup, lid, and shutter
handling the cooling mixture and cooling block; wear gloves
mechanism for cleanliness and freedom from contamination.
andgoggles.Mixturessuchasdryiceandacetonecanproduce
Use an absorbent tissue to wipe clean, if necessary. Lock the
severe frost bite.) (Warning—Be careful when inserting the
cover lid tightly in place.
coolingblockintothetestercuptopreventdamagetothecup.)
10.2 Switch the heater on, if not already at stand-by. To
11.3 Introduce the specimen as in 10.4.Allow the tempera-
rapidly approach the specification flash temperature of the
ture to rise under ambient conditions or increase the tempera-
materialundertest,turntheheaterdialfullyclockwise(Note6)
ture of the cup by rotating the heater controller clockwise
causing the heater signal (red) light to glow. When the
slowly until the specification temperature adjusted for baro-
thermometer indicates a temperature of about 3°C (5°F) below
metric pressure is reached. Determine whether the material
the specification or target flash-point temperature, reduce the
flashes as in 10.5 and 10.6.
heat input to the test cup by slowly turning the heater control
11.4 Turn off the test and pilot flames. Clean the apparatus.
dial counter clockwise until the signal light goes out (Note 7).
TEST METHOD B—FINITE FLASH POINT
NOTE 6—When a desired temperature is dialed on the controller, the
elapsedtimetoreachthistemperaturemaybegreaterthanifthecontroller 12. Procedure—Ambient to 110°C (230°F)
is turned“ full on,” but less attention is required.
12.1 Preliminary or Trial Test:
NOTE 7—Thetestcuptemperatureisstablewhenthesignallightslowly
12.1.1 Followsteps10.1-10.5,omittingthebarometricread-
cycles on and off.
ing and using an estimated finite flash point instead of
10.3 Determine the barometric pressure to determine the
specification flash-point temperature.
corrected specification temperature at that barometric pressure
12.1.2 After 1 min has elapsed, observe the temperature.
(see 15.1).
Applythetestflamebyslowlyanduniformlyopeningtheslide
10.4 After the test-cup temperature has stabilized at the
fully and closing completely over a period of 2 ⁄2s(Note 8),
specification or target flash point, charge the syringe with the
watching for a flash (Note 9) while the flame is inserted.
sample being tested and insert the tip of the syringe into the
12.2 If a flash is observed, proceed as in 12.3. If no flash is
filling orifice (Fig.A1.1), taking care not to lose any material.
observed, proceed as in 12.4.
Discharge the specimen into the test cup by completely
12.3 Usingatemperature5°C(9°F)lowerthanthetempera-
depressing the syringe plunger, then remove the syringe. If the
ture observed in 12.1.2, repeat 12.1 (Note 4). If a flash is still
materialhasaviscositygreaterthan45SUSat38°C(100°F)or
observed, repeat at 5°C lower intervals until no flash is
equivalentof9.5cStat25°C(77°F),raisethelidanddischarge
observed.
the contents of the syringe directly into the cup. Immediately
NOTE 10—Nevermakearepeattestonthesamespecimen.Alwaystake
close the lid tightly.
a fresh portion for each test.
10.5 Setthe1-mintimingdevice.Inthemeantime,openthe
gas control valve and light the pilot and test flames.Adjust the 12.3.1 Afterestablishingtheapproximateflashpoint,repeat
12.1 with a new specimen, but stabilizing the test temperature
test flame size with the pinch valve to match the size of the
⁄32-in. (4-mm) diameter flame gage. atwhichnoflashoccurredpreviously.Observeifaflashoccurs
at this temperature. If not, increase the temperature by making
10.6 After 1 min has elapsed, observe the temperature. If at
the specification temperature (accounting for the differences of a small adjustment to the temperature controller so that an
increase of 0.5°C (1°F) occurs within 1 min.Test for a flash at
the barometer reading from 760 mm), apply the test flame by
slowly and uniformly opening the slide fully and closing each 0.5°C interval, recording the temperature at which the
flash actually occurs. Record the barometric pressure. Clean
completely over a period of approximately 2 ⁄2s(Note 8),
the tester.
watching for a flash (Note 9) while the flame is inserted.
12.3.1.1 Repeat 12.3.1 with a new specimen. Calculate the
NOTE 8—When inserted, the nozzle of the ignition device should
corrected mean temperature in accordance with 15.2. Turn off
intersect the plane of the underside of the cover (see A1.1).
pilot and test flames and clean the tester.
NOTE 9—The material is considered to have flashed only if a compara-
12.4 Using a test temperature 5°C (9°F) higher than the
tivelylargeblueflameappearsandpropaga
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