ASTM E502-84(2000)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E502–84(Reapproved2000)
Standard Test Method for
Selection and Use of ASTM Standards for the Determination
of Flash Point of Chemicals by Closed Cup Methods
This standard is issued under the fixed designation E502; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope Liquids by Tag Open-Cup Apparatus
D3278 TestMethodforFlashPointofLiquidsbySetaflash
1.1 This test method covers the determination of the flash
Closed Tester
point of liquid and solid chemical compounds flashing from
D3827 Test Method for Estimation of Solubility of Gases
below−10 to 370°C (16 to 700°F). The procedures and
in Petroleum and Other Organic Liquid
apparatus in Test Methods D56, D93, D3278, D3828, and
D3828 Test Method for Flash Point by Setaflash Closed
D3941 are to be used. Modification to these procedures are
Tester
specified for tests on solids and viscous liquids. The signifi-
D3934 Test Method for Flash/No Flash Test Equilibrium
cance of the results obtained is discussed along with possible
Method by a Closed-Cup Apparatus
sources of error and factors that might cause interference.
D3941 Test Method for Flash Point by the Equilibrium
1.2 Suggestions for adapting this procedure to mixtures of
Method with a Closed-Cup Apparatus
chemicals are included (see Appendix X2).
E681 Test Method for Limits of Flammability of Chemi-
1.3 Thistestmethodshouldbeusedtomeasureanddescribe
cals
the properties of materials, products, or assemblies in response
to heat and flame under controlled laboratory conditions and
3. Terminology
shouldnotbeusedtodescribeorappraisethefirehazardorfire
3.1 Definition:
risk of materials or assemblies under actual fire conditions.
3.1.1 flash point—the lowest temperature, corrected to a
However, results of this test method may be used as elements
pressure of 760 mm Hg (101.3 kPa) (1013 mbar) at which
ofafireriskassessmentthattakeintoaccountallofthefactors
application of an ignition source causes the vapors of a
that are pertinent to an assessment of the fire hazard of a
specimen to ignite under specified conditions of test.
particular end use.
1.4 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 The specimen is placed in a closed cup and in the
responsibility of the user of this standard to establish appro-
Setaflash method equilibrated at a test temperature, in the
priate safety and health practices and determine the applica-
Pensky-Martens Method heated at a controlled rate with
bility of regulatory limitations prior to use. See also Section 8.
stirring, and in the Tag Method also heated at a controlled rate
but without stirring. A small flame is directed into the vapor
2. Referenced Documents
space of each cup at specified intervals, with simultaneous
2.1 ASTM Standards:
2 interruption of stirring in the Pensky-Martens Method, to
D56 Test Method for Flash Point by Tag Closed Tester
determine whether a flash occurs or not. In Test Method
D92 Test Method for Flash and Fire Points by Cleveland
2 D3941, the specimen is heated at a slower rate than in the
Open Cup
othercontrolledheatingmethods,maintainingasmalltempera-
D93 Test Methods for Flash Point by Pensky-Martens
2 ture differential between bath and specimen.
Closed Tester
D270 Method of Sampling Petroleum and Petroleum Prod-
5. Significance and Use
ucts
5.1 The flash point measures the response of the sample to
D1310 Test Method for Flash Point and Fire Points of
heat and flame 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.
This test method is under jurisdiction of ASTM Committee E27 on Hazard
Potential of Chemicals and is the direct responsibility of Subcommittee E27.04 on
Flammability and Ignitability of Chemicals.
Current edition approved July 27, 1984. Published September 1984. Annual Book of ASTM Standards, Vol 06.03.
2 5
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 05.03.
3 6
Discontinued, See 1983 Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 14.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
E502
5.2 As a result of physical factors inherent in the apparatus testing. Certain toxic or unusual materials, however, may
and procedure, the closed cup flash point does not necessarily require an air-supplied respirator and extreme cases may
represent the minimum temperature at which a material can require complete protective coverage such as an air-supplied
evolveflammablevapors,andtheabsenceofaflashpointdoes plastic suit. (Two examples of the latter type of material are
not guarantee nonflammability (see Appendix X1 and Appen- dimethyl sulfate and pure mercaptans.) Tests on these highly
dix X2). toxic or obnoxious materials may also be conducted in com-
5.3 Flash point is used in shipping and safety regulations to pletely isolated, closed systems, such as glove boxes. In this
define flammable and combustible materials. Test Methods case, procedures should ensure an uncontaminated air system
D56, D93, and D3278 are specified as test methods for in the box, and should prevent a buildup of vapors from the
determining the flash point of these materials. material under test.
5.4 Setaflashmethodsinvolvingequilibriumproceduresand 8.2 Dry Ice Use:
only one flame pass per specimen are preferred. 8.2.1 Exercise care in the use of dry ice for sample and
apparatus cooling. Avoid contact with dry ice to prevent
6. Interferences
frostbite. Glass bottles or vials of chemicals should not be
6.1 Incorrect flash points can be obtained when testing placed directly in dry ice or dry ice baths because of the
possibility of breakage due to thermal shock.
chemicalscorrosivetothematerialsofconstructionofthecup.
(For example, certain amines and acid chlorides react with the 8.3 Tests of Explosives and Propellants:
8.3.1 Flash tests should not be conducted on potential or
standardaluminumSetaflashcupcausingerroneouslylowflash
points, perhaps due to hydrogen formation.) Cups employing known explosive or propellant materials without complete
prior knowledge that burning will not result in propagation to
alternative materials of construction, electroplating or plastic
coating can provide corrosion resistance. Results in non- an explosive decomposition. Properly barricaded or remotely
operatedautomatictestersshouldbeusedifpreciseflashpoints
standard cups, particularly in non-equilibrium tests, may differ
slightly from those obtained in this test method. are needed.
8.4 Pyrophoric Materials:
7. Apparatus
8.4.1 Flash point apparatus is not applicable for the evalu-
ation of pyrophoric materials and should not be used for this
7.1 Tag Closed-Cup Tester, including thermometers, shall
be as shown in Test Methods D56 and D3941. purpose.
7.2 Penksy-Martens Closed-Cup Tester, including ther-
9. Preparation of Sample
mometers, shall be as shown in Test Methods D93.
9.1 Obtain samples representative of the batch under test.
7.3 Setaflash Closed Tester, including thermometers, shall
be as shown in Test Methods D3278 or D3828. Test Method D270 can be used as a reference on sampling
techniques. With mixtures and with samples containing impu-
NOTE 1—Some automatic flash point testers may save testing time and
rities,takecaretoavoidthelossofvolatilecomponentsduring
permit the use of small samples. If automatic testers are used, the user
sampling and handling for testing. When heating viscous or
must be certain that all instructions for calibration and operation are
solid materials for ease of pouring, samples must be held at
followed to ensure that the results are equivalent to those obtained on the
ASTMstandardequipment.Forregulationpurposesorincasesofdispute, temperatures below, or as close as possible to, those specified
the flash point as determined on the manual tester shall be the accepted
in the various test methods. Discard samples from leaking or
value.
contaminated containers. Samples that are hygroscopic should
NOTE 2—ASTM thermometers 33C or 33F may be used in the Tag
not be exposed to moisture or moist air.
Tester instead of those specified in Test Method D56 when conducting
9.2 Samples should not be stored in plastic (polyethylene,
testsattemperaturesbelow−10°C(14°F).Slightstemcorrectionsmaybe
polypropylene, etc.) bottles, since volatile materials may dif-
necessary and care should be taken to avoid freezing the mercury in the
thermometer by cooling below−40°C (−40°F). fuse through the walls of the bottle.
7.4 Shield, as described in Test Method D3941 or Test Method D1310.
10. Preparation of Apparatus
8. Hazards
10.1 Support the appropriate flash-point tester on a level,
8.1 Toxicity of Chemical and Combustion Products:
steady work surface in a draft-free location. If a draft-free
8.1.1 Isolate or control operations on toxic or corrosive
location is not available, use a shield surrounding the tester on
materials to prevent exposure to any personnel.
three sides. The shield should be approximately 460 mm (18
8.1.2 Sinceflashpointtestsareconductedinstillair,theuse
in.) wide and 610 mm (24 in.) high.
of forced circulation for removal of toxic or nuisance fumes or
NOTE 3—An area capable of being partially darkened is advantageous
combustion products is restricted. However, a laboratory fume
since it aids in the detection of the relatively nonluminous flames
hood equipped with an exhaust damper that can be completely
sometimes encountered in flash-point testing.
closed provides an ideal location for maintaining draft-free
NOTE 4—Test Method D1310 gives a design for a draft shield suitable
conditions and provides the ability to readily exhaust danger-
for standard flash-point testers.
ous vapors and combustion products when necessary.
11. Calibration
8.1.3 Use respiratory and splash protective devices as ap-
propriate with toxic or corrosive materials. In most cases, 11.1 Check the condition and operation of the Tag, Pensky-
approved cartridge respirators are adequate respiratory protec- Martens and Setaflash testers as specified in Test Methods
tion for the concentrations normally encountered in flash-point D56, D93, D3278, or D3828, respectively.
E502
NOTE 9—Testing time may be reduced by initially heating samples at
12. Procedure
higher rates than those specified in the test procedures, provided that the
12.1 Follow the procedures outlined in Test Methods D56
specified heating rates are maintained in the temperature range in the
or D3941 (Tag Closed Cup), D3278 or D3827 (Setaflash
vicinityoftheflashpoint.Thisispermissibleprovidedthat,duringthefast
Closed Cup), and D93 (Pensky Martens Closed Cup), as is
heat-up period, the highest temperature of the material (next to the cup
necessary. Certain explanatory notes and procedure modifica- wall) never exceeds a temperature 11°C (20°F) below the flash point for
the Pensky-Martens method. Use extreme care when using fast heat-up in
tions not contained in the individual methods are given below.
the Pensky-Martens method since there are no provisions for bath
Occasionally, particularly near the temperature of the actual
temperature measurement.12.5 For liquids with a viscosity equal to or
flashpoint,theapplicationofthetestflamewillcauseahaloor
−3 2
greater than 15 310 m /s (150 cSt at 25°C) (77°F) and solid materials
test flame enlargement that should be ignored. In some cases
that flash while solid (Note 11), the following procedures apply:
this test flame enlargement will not lead to a flash point on an
12.4.2 Use the Setaflash Test Methods D3278 or Test
increase in temperature.
−6 2
Method D3828 with the following modification:
12.2 For liquids with a viscosity less than 5.8 310 m /s
−6 2
12.4.2.1 DeterminetheflashpointintheSetaflashunitusing
(5.8cSt)at38°C(100°F),or9.5 310 m /s(9.5cSt)at25°C
a holding time of 6 min at the test temperature instead of 1 or
(77°F), observe the following:
2 min normally employed.
12.2.1 If the flash point is below 93°C (200°F), use the
12.4.2.2 Methods for loading the sample cup with highly
Setaflash(TestMethodD3278orD3828)orTag(TestMethod
viscous liquids or solids are given in Test Methods D3278.
D56) apparatus and procedures.
Solid materials can be loaded with a spoon.
12.2.2 If the flash point is 93°C (200°F) or above, use the
12.5 For equilibrium flash point method using the Tag
Setaflash (Test Method D3828) or Pensky-Martens (Test
Closed Cup Tester, the following applies:
Methods D93) apparatus and procedures.
12.5.1 For liquids with a viscosity equal to or greater than
−6
2 −6 2
NOTE 5—The electric heaters on some Tag Testers may be of insuffi-
5.8 310 m /s (5.8 cSt at 38°C (100°F) or 9.5 310 m /s
cientcapacitytomaintainthespecifiedheatingrateswhenoperatinginthe
(9.5 cSt) at 25°C (77°F) and a flash point below 93°C (200°F),
upperrangesofthispractice.Heatinputcanbeincreasedslightlybyusing
Test Method D3941 may be used using the Tag Closed Cup.
a variable transformer to increase the voltage slightly on the heaters.
12.5.2 Test Method D3941 may also be used for the high
Insulation can be applied to the exterior of the bath to reduce heat losses.
viscosityliquidsandsolidscoveredin12.5(Note11).Observe
NOTE 6—With low temperature operation in the Setaflash methods,
equilibrium may be difficult to maintain due to heating by natural the temperature differences between bath and sample specified
convection. It, therefore, will be necessary to cool the cup and sample
in Test Method D3941. (The Tag tester is very inefficient for
below the anticipated flash point before specimen introduction (see Test
testing these materials since large sample quantities and very
Methods D3278).
long testing times are required.)
NOTE 7—IntheTagMethod(TestMethodD56),naturalwarmingrates
sometimes exceed 1°C (2°F)/min. These rates can be reduced by insulat- NOTE 10—With highly viscous materials it may be advantageous to fill
ing the outside of the bath container. A laboratory refrigerated circulator thetagclosedcupvesseldirectlytoa50-mLlineonthesamplecuprather
may be used. One advantage of this system is that circulation of the than to use the graduated cylinder specified in Test Method D56.
refrigerant bath with the system gradually warming up can serve as a Significant quantities of a viscous material may adhere to the walls of the
control on heating rate. graduated cylinder when the transfer is made. Certain manufacturers
N
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