ASTM E502-07(2013)

Standard Test Method for Selection and Use of ASTM Standards for the Determination of Flash Point of Chemicals by Closed Cup Methods

SIGNIFICANCE AND USE
5.1 The flash point measures the response of the sample to 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.  
5.2 As a result of physical factors inherent in the apparatus and procedure, the closed cup flash point does not necessarily represent the minimum temperature at which a material can evolve flammable vapors, and the absence of a flash point does not guarantee nonflammability (see Appendix X1 and Appendix X2).  
5.3 Flash point is used in shipping and safety regulations to define flammable and combustible materials. Test Methods D56, D93, and D3278 are specified as test methods for determining the flash point of these materials.  
5.4 If the process or handling conditions dictate the usage of a flammable material at temperatures ranging upward from 5 to 10°C below the closed-cup flash point, then a flammable vapor might be present above the liquid. In such cases, it may be more appropriate to use the temperature limit of flammability (as determined by Test Method E1232) instead of flash point.  
5.5 Small scale methods involving equilibrium procedures and only one flame pass per specimen are preferred.
SCOPE
1.1 This test method covers the determination of the flash point of liquid and solid chemical compounds flashing from below − 10 to 370°C (16 to 700°F). The procedures and apparatus in Test Methods D56, D93, D3278, D3828, and D3941 are to be used. Modification to these procedures are specified for tests on solids and viscous liquids. The significance of the results obtained is discussed along with possible sources of error and factors that might cause interference.  
1.2 Suggestions for adapting this procedure to mixtures of chemicals are included (see Appendix X2).  
1.3 This test method should be used to measure and describe the properties of materials, products, or assemblies in response to heat and flame under controlled laboratory conditions and should not be used to describe or appraise the fire hazard or fire risk of materials or assemblies under actual fire conditions. However, results of this test method may be used as elements of a fire risk assessment that take into account all of the factors that are pertinent to an assessment of the fire hazard of a particular end use.  
1.4 Warning—Mercury has been designated by EPA and many state agencies as a hazardous material that can cause central nervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Caution should be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet (MSDS) for details and EPA’s website – http://www.epa.gov/mercury/faq.htm - for additional information. Users should be aware that selling mercury and/or mercury containing products into your state may be prohibited by state law.  
1.5 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. See also Section 8.

General Information

• Status: Historical
• Publication Date: 30-Sep-2013
• ICS: 71.080.01 - Organic chemicals in general
• Technical Committee: E27 - Hazard Potential of Chemicals
• Drafting Committee: E27.04 - Flammability and Ignitability of Chemicals

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: E502 − 07 (Reapproved 2013)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. See also Section 8.
1.1 This test method covers the determination of the flash
point of liquid and solid chemical compounds flashing from
2. Referenced Documents
below−10 to 370°C (16 to 700°F). The procedures and
apparatus in Test Methods D56, D93, D3278, D3828, and 2.1 ASTM Standards:
D3941 are to be used. Modification to these procedures are D56Test Method for Flash Point by Tag Closed Cup Tester
specified for tests on solids and viscous liquids. The signifi- D92Test Method for Flash and Fire Points by Cleveland
cance of the results obtained is discussed along with possible Open Cup Tester
sources of error and factors that might cause interference. D93Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester
1.2 Suggestions for adapting this procedure to mixtures of
D270Methods of Sampling Petroleum and Petroleum Prod-
chemicals are included (see Appendix X2).
ucts (Withdrawn 1984)
1.3 Thistestmethodshouldbeusedtomeasureanddescribe
D1310TestMethodforFlashPointandFirePointofLiquids
the properties of materials, products, or assemblies in response
by Tag Open-Cup Apparatus
to heat and flame under controlled laboratory conditions and
D3278Test Methods for Flash Point of Liquids by Small
shouldnotbeusedtodescribeorappraisethefirehazardorfire
Scale Closed-Cup Apparatus
risk of materials or assemblies under actual fire conditions.
D3827Test Method for Estimation of Solubility of Gases in
However, results of this test method may be used as elements
Petroleum and Other Organic Liquids
ofafireriskassessmentthattakeintoaccountallofthefactors
D3828Test Methods for Flash Point by Small Scale Closed
that are pertinent to an assessment of the fire hazard of a
Cup Tester
particular end use.
D3934Test Method for Flash/No Flash Test—Equilibrium
1.4 Warning—Mercury has been designated by EPA and Method by a Closed-Cup Apparatus
many state agencies as a hazardous material that can cause D3941Test Method for Flash Point by the Equilibrium
central nervous system, kidney and liver damage. Mercury, or Method With a Closed-Cup Apparatus
E681TestMethodforConcentrationLimitsofFlammability
its vapor, may be hazardous to health and corrosive to
materials.Cautionshouldbetakenwhenhandlingmercuryand of Chemicals (Vapors and Gases)
E1232Test Method for Temperature Limit of Flammability
mercury containing products. See the applicable product Ma-
terial Safety Data Sheet (MSDS) for details and EPA’s website of Chemicals
– http://www.epa.gov/mercury/faq.htm - for additional infor-
mation. Users should be aware that selling mercury and/or 3. Terminology
mercury containing products into your state may be prohibited
3.1 Definitions:
by state law.
3.1.1 flash point—the lowest temperature, corrected to a
1.5 This standard does not purport to address all of the pressure of 760 mm Hg (101.3 kPa) (1013 mbar) at which
safety concerns, if any, associated with its use. It is the
application of an ignition source causes the vapors of a
responsibility of the user of this standard to establish appro- specimen to ignite under specified conditions of test.
1 2
This test method is under jurisdiction of ASTM Committee E27 on Hazard For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Potential of Chemicals and is the direct responsibility of Subcommittee E27.04 on contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Flammability and Ignitability of Chemicals. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Oct. 1, 2013. Published October 2013. Originally the ASTM website.
ε1 3
approved in 1984. Last previous edition approved in 2007 as E502–07 . DOI: The last approved version of this historical standard is referenced on
10.1520/E0502-07R13. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E502 − 07 (2013)
permit the use of small samples. If automatic testers are used, the user
4. Summary of Test Method
must be certain that all instructions for calibration and operation are
4.1 The specimen is placed in a closed cup and in the small
followed to ensure that the results are equivalent to those obtained on the
scale method equilibrated at a test temperature, in the Pensky-
ASTMstandardequipment.Forregulationpurposesorincasesofdispute,
the flash point as determined on the manual tester shall be the accepted
MartensMethodheatedatacontrolledratewithstirring,andin
value.
the Tag Method also heated at a controlled rate but without
NOTE 2—ASTM thermometers 33C or 33F may be used in the Tag
stirring.Asmall flame is directed into the vapor space of each
Tester instead of those specified in Test Method D56 when conducting
cup at specified intervals, with simultaneous interruption of
testsattemperaturesbelow−10°C(14°F).Slightstemcorrectionsmaybe
stirringinthePensky-MartensMethod,todeterminewhethera necessary and care should be taken to avoid freezing the mercury in the
thermometer by cooling below−40°C (−40°F).
flash occurs or not. In Test Method D3941, the specimen is
7.4 Shield, as described in Test Method D3941 or Test Method D1310.
heated at a slower rate than in the other controlled heating
methods, maintaining a small temperature differential between
8. Hazards
bath and specimen.
8.1 Toxicity of Chemical and Combustion Products:
8.1.1 Isolate or control operations on toxic or corrosive
5. Significance and Use
materials to prevent exposure to any personnel.
5.1 The flash point measures the response of the sample to
8.1.2 Sinceflashpointtestsareconductedinstillair,theuse
heat and flame under controlled laboratory conditions. It is
of forced circulation for removal of toxic or nuisance fumes or
only one of a number of properties that must be considered in
combustion products is restricted. However, a laboratory fume
assessing the overall flammability hazard of a material.
hood equipped with an exhaust damper that can be completely
5.2 As a result of physical factors inherent in the apparatus
closed provides an ideal location for maintaining draft-free
and procedure, the closed cup flash point does not necessarily
conditions and provides the ability to readily exhaust danger-
represent the minimum temperature at which a material can
ous vapors and combustion products when necessary.
evolveflammablevapors,andtheabsenceofaflashpointdoes
8.1.3 Use respiratory and splash protective devices as ap-
not guarantee nonflammability (see Appendix X1 and Appen-
propriate with toxic or corrosive materials. In most cases,
dix X2).
approved cartridge respirators are adequate respiratory protec-
tion for the concentrations normally encountered in flash-point
5.3 Flash point is used in shipping and safety regulations to
testing. Certain toxic or unusual materials, however, may
define flammable and combustible materials. Test Methods
require an air-supplied respirator and extreme cases may
D56, D93, and D3278 are specified as test methods for
require complete protective coverage such as an air-supplied
determining the flash point of these materials.
plastic suit. (Two examples of the latter type of material are
5.4 Iftheprocessorhandlingconditionsdictatetheusageof
dimethyl sulfate and pure mercaptans.) Tests on these highly
aflammablematerialattemperaturesrangingupwardfrom5to
toxic or obnoxious materials may also be conducted in com-
10°Cbelowtheclosed-cupflashpoint,thenaflammablevapor
pletely isolated, closed systems, such as glove boxes. In this
might be present above the liquid. In such cases, it may be
case, procedures should ensure an uncontaminated air system
more appropriate to use the temperature limit of flammability
in the box, and should prevent a buildup of vapors from the
(as determined by Test Method E1232) instead of flash point.
material under test.
5.5 Small scale methods involving equilibrium procedures
8.2 Dry Ice Use:
and 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
chemicalscorrosivetothematerialsofconstructionofthecup.
possibility of breakage due to thermal shock.
(For example, certain amines and acid chlorides react with the
8.3 Tests of Explosives and Propellants:
standard aluminum small scale cup causing erroneously low
8.3.1 Flash tests should not be conducted on potential or
flash points, perhaps due to hydrogen formation.) Cups em-
known explosive or propellant materials without complete
ploying alternative materials of construction, electroplating or
prior knowledge that burning will not result in propagation to
plastic coating can provide corrosion resistance. Results in
an explosive decomposition. Properly barricaded or remotely
non-standard cups, particularly in non-equilibrium tests, may
operatedautomatictestersshouldbeusedifpreciseflashpoints
differ slightly from those obtained in this test method.
are needed.
7. Apparatus
8.4 Pyrophoric Materials:
7.1 Tag Closed-Cup Tester,includingthermometers,shallbe
8.4.1 Flash point apparatus is not applicable for the evalu-
as shown in Test Methods D56 and D3941.
ation of pyrophoric materials and should not be used for this
purpose.
7.2 Penksy-Martens Closed-Cup Tester, including
thermometers, shall be as shown in Test Methods D93.
9. Preparation of Sample
7.3 Small scale Closed Tester,includingthermometers,shall
9.1 Obtain samples representative of the batch under test.
be as shown in Test Methods D3278 or D3828.
Methods D270 can be used as a reference on sampling
NOTE 1—Some automatic flash point testers may save testing time and techniques. With mixtures and with samples containing
E502 − 07 (2013)
NOTE 7—With low temperature operation in the small scale methods,
impurities, take care to avoid the loss of volatile components
equilibrium may be difficult to maintain due to heating by natural
during sampling and handling for testing. When heating
convection. It, therefore, will be necessary to cool the cup and sample
viscousorsolidmaterialsforeaseofpouring,samplesmustbe
below the anticipated flash point before specimen introduction (see Test
held at temperatures below, or as close as possible to, those
Methods D3278).
specified in the various test methods. Discard samples from
NOTE 8—In theTag Method (Test Method D56), natural warming rates
sometimes exceed 1°C (2°F)/min. These rates can be reduced by insulat-
leaking or contaminated containers. Samples that are hygro-
ing the outside of the bath container. A laboratory refrigerated circulator
scopic should not be exposed to moisture or moist air.
may be used. One advantage of this system is that circulation of the
9.2 Samples should not be stored in plastic (polyethylene, refrigerant bath with the system gradually warming up can serve as a
control on heating rate.
polypropylene, etc.) bottles, since volatile materials may dif-
NOTE 9—With low-temperature operation in the Tag and Small scale
fuse through the walls of the bottle.
Methods, difficulties can be created by the formation of frost on the
surface of the tester. If precise flash points are needed in the temperature
10. Preparation of Apparatus
range where frost conditions are encountered, tests can be conducted in a
dryboxoraroomofverylowhumidity.Wheniceformationonthelidand
10.1 Support the appropriate flash-point tester on a level,
cover parts cannot be avoided, the results will be unreliable. Sticking of
steady work surface in a draft-free location. If a draft-free
the slide due to ice formation can be minimized by carefully lubricating
location is not available, use a shield surrounding the tester on
the slide with a high vacuum silicone lubricant. Portions of the cover and
three sides. The shield should be approximately 460 mm (18
slide in the vicinity of the pilot flame and openings should be wiped free
of frost just prior to the initial flame insertion at 5°C (10°F) below the
in.) wide and 610 mm (24 in.) high.
flash point.
NOTE 3—An area capable of being partially darkened is advantageous
12.3 For liquids with a viscosity equal to or greater than
since it aids in the detection of the relatively nonluminous flames
−6
2 −6 2
5.8×10 m /s (5.8 cSt) at 38°C (100°F), or 9.5×10 m /s
sometimes encountered in flash-point testing.
−3 2
NOTE 4—Test Method D1310 gives a design for a draft shield suitable
(9.5 cSt) at 25°C (77°F) and less than 15×10 m /s (150 St)
for standard flash-point testers.
at 25°C (77°F), and a flash point below 110°C (230°F), the
following procedure applies:
11. Calibration
12.3.1 Use of Pensky-Martens Method (Test Methods D93)
11.1 Check the condition and operation of the Tag, Pensky-
or the small scale (Test Method D3278 or D3828) apparatus
Martens and small scale testers as specified in Test Methods
and procedure.
D56, D93, D3278,or D3828, respectively.
12.4 For liquids with a viscosity equal to or greater than
−6
2 −6 2
5.8×10 m /s(5.8cSt)at38°C(100°F)or9.5×10 m /s(9.5
12. Procedure
cSt)at25°C(77°F)andaflashpointof93°C(200°F)orabove,
12.1 FollowtheproceduresoutlinedinTestMethodsD56or
the following procedure applies:
D3941 (Tag Closed Cup), D3278 or D3827 (Small scale
12.4.1 UsethePensky-Martens(TestMethodsD93)andthe
Closed Cup), and D93 (Pensky Martens Closed Cup), as is
small scale (Test Method D3828) apparatus and procedure.
necessary. Certain explanatory notes and procedure modifica-
NOTE 10—Testing time may be reduced by initially heating samples at
tions not contained in the individual methods are given below.
higher rates than those specified in the test procedures, provided that the
Occasionally, particularly near the temperature of the actual
specified heating rates are maintained in the temperature range in the
flashpoint,theapplicationofthetestflamewillcauseahaloor
vicinityoftheflashpoint.Thisispermissibleprovidedthat,duringthefast
test flame enlargement that should be ignored. In some cases heat-up period, the highest temperature of
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