ASTM D3828-16a(2021)

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: D3828 − 16a (Reapproved 2021)
Standard Test Methods for
Flash Point by Small Scale Closed Cup Tester
This standard is issued under the fixed designation D3828; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
INTRODUCTION
These small scale flash point methods are generally used for testing a sample at a specific
temperature where the specimen being tested and the air–vapor mixture above it are close to thermal
equilibrium.TestMethodD3941coversotherflashpointequipmentoperatedataspecifictemperature.
Flash point values 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. Scope responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.1 These test methods cover procedures for flash point
mine the applicability of regulatory limitations prior to use.
tests, within the range of –30 °C to 300 °C, of petroleum
Warning statements appear throughout. See also the Material
products and biodiesel liquid fuels, using a small scale closed
Safety Data Sheets for the product being tested.
cup tester. The procedures may be used to determine, whether
1.5 This international standard was developed in accor-
a product will or will not flash at a specified temperature
dance with internationally recognized principles on standard-
(flash/no flash Method A) or the flash point of a sample
ization established in the Decision on Principles for the
(Method B). When used in conjunction with an electronic
Development of International Standards, Guides and Recom-
thermal flash detector, these test methods are also suitable for
mendations issued by the World Trade Organization Technical
flash point tests on biodiesels such as fatty acid methyl esters
Barriers to Trade (TBT) Committee.
(FAME).
1.2 The values stated in SI units are to be regarded as the
2. Referenced Documents
standard. The values given in parentheses are for information
2.1 ASTM Standards:
only.
D3941 Test Method for Flash Point by the Equilibrium
1.3 This standard should be used to measure and describe
Method With a Closed-Cup Apparatus
the properties of materials, products, or assemblies in response
D4057 Practice for Manual Sampling of Petroleum and
to heat and flame under controlled laboratory conditions and
Petroleum Products
should not be used to describe or appraise the fire hazard or
D4177 Practice for Automatic Sampling of Petroleum and
fire risk of materials, products, or assemblies under actual fire
Petroleum Products
conditions. However, results of this test may be used as
D6299 Practice for Applying Statistical Quality Assurance
elements of a fire risk assessment which takes into account all
and Control Charting Techniques to Evaluate Analytical
of the factors which are pertinent to an assessment of the fire
Measurement System Performance
hazard of a particular end use.
D6708 Practice for StatisticalAssessment and Improvement
1.4 This standard does not purport to address all of the
of Expected Agreement Between Two Test Methods that
safety concerns, if any, associated with its use. It is the
Purport to Measure the Same Property of a Material
E300 Practice for Sampling Industrial Chemicals
These test methods are under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.08 on Volatility. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2021. Published July 2021. Originally approved contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
in 1979. Last previous edition approved in 2016 as D3828 – 16a. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
D3828-16AR21. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3828 − 16a (2021)
E1137/E1137M Specification for Industrial Platinum Resis- introducedandtested.Thisprocedureisrepeateduntiltheflash
tance Thermometers point is established within 5 °C (9 °F).
4.2.3 The procedure is then repeated at 1 °C (2 °F) intervals
2.2 ISO Standards:
Guide 34 General requirements for the competence of refer- until the flash point is determined to the nearest 1 °C (2 °F).
ence material producers 4.2.4 If improved accuracy is desired the procedure is
Guide 35 Reference materials—General and statistical prin- repeated at 0.5 °C (1 °F) intervals until the flash point is
ciples for certification determined to the nearest 0.5 °C (1 °F).
EN ISO 3679 Determination of Flash Point—Rapid Equilib-
4.3 Test Time and Specimen Volume:
rium Closed Cup Method
4.3.1 For all products, except biodiesel; for test tempera-
EN ISO 3680 Determination of Flash/No Flash—Rapid
tures up to and including 100 °C (212 °F), the test time is
Equilibrium Closed Cup Method
1 min and the specimen volume is 2 mL.
ISO 60751 Industrial Platinum Resistance Thermometers
4.3.2 For all products, except biodiesel; for test tempera-
and Platinum Temperature Sensors
tures over 100 °C (212 °F), the test time is 2 min and the
2.3 Energy Institute Standards:
specimen volume is 4 mL.
IP 523 Determination of Flash Point—Rapid Equilibrium
4.3.3 For biodiesel; for all test temperatures, the test time is
Closed Cup Method
1 min and the specimen volume is 2 mL.
IP 524 Determination of Flash/No Flash—Rapid Equilib-
rium Closed Cup Method
5. Significance and Use
3. Terminology 5.1 Flash point measures the response of the test specimen
to heat and ignition source under controlled laboratory condi-
3.1 Definitions:
tions. It is only one of a number of properties that must be
3.1.1 equilibrium, n—in flash point test methods, the condi-
considered in assessing the overall flammability hazard of a
tion where the vapor above the test specimen, and the test
material.
specimen are at the same temperature at the time the ignition
source is applied. 5.2 Flash point is used in shipping and safety regulations to
3.1.1.1 Discussion—This condition may not be fully define flammable and combustible materials and classify them.
achieved in practice, since the temperature may not be uniform Consult the particular regulation involved for precise defini-
throughout the test specimen, and the test cover and shutter on tions of these classes.
the apparatus can be cooler or warmer.
5.3 Flash point can indicate the possible presence of highly
3.1.2 flash point, n—in flash point test methods, the lowest
volatile and flammable materials in a relatively nonvolatile or
temperature of the test specimen, adjusted to account for
nonflammable material.
variations in atmospheric pressure from 101.3 kPa, at which
5.4 Thesetestmethodsuseasmallersample(2 mLto4 mL)
application of an ignition source causes the vapors of the test
and a shorter test time (1 min to 2 min) than traditional test
specimen to ignite under specified conditions of test.
methods.
4. Summary of Test Methods 5.5 MethodA,IP524andENISO3680aresimilarmethods
for flash no-flash tests. Method B, IP523 and EN ISO 3679 are
4.1 Method A—Flash/No Flash Test—A test specimen is
similar methods for flash point determination.
introduced, by a syringe, into the test cup of the selected
apparatus that is set and maintained at the specified tempera-
6. Apparatus
ture. After a specific time an ignition source is applied and a
determination made as to whether or not a flash occurred.
6.1 Test Cup and Cover Assembly—The essential dimen-
sions and requirements of the apparatus are shown in Fig.A1.1
4.2 Method B—Finite (or Actual) Flash Point—This
and Table A1.1 of Annex A1. The apparatus and accessories
methodessentiallyrepeatsMethodAanumberoftimes,andby
are described in detail in Annex A1. The temperature range is
changing the test temperature and test specimen a number of
from –30 °C to 300 °C. Some versions of the apparatus may
times, determines the flash point.
not cover the full temperature range.
4.2.1 A test specimen is introduced into the test cup of the
selected apparatus that is maintained at the expected flash
6.2 Barometer, accurate to 0.5 kPa. Barometers that have
point.After a specified time an ignition source is applied and a
been pre-corrected for use at weather stations or airports are
determination made whether or not a flash occurred.
not suitable.
4.2.2 The test specimen is removed from the test cup; the
6.3 Draft Shield—A shield located at the back and on two
test cup and cover are cleaned, and the test temperature
sides of the instrument, for use in circumstances where
adjusted 5 °C (9 °F) lower or higher depending on whether or
protection from drafts does not exist.
not a flash occurred previously. A fresh test specimen is
7. Reagents and Materials
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
7.1 Cleaning Solvent—Use only non-corrosive solvents ca-
4th Floor, New York, NY 10036, http://www.ansi.org.
pable of cleaning the test cup and cover. Two commonly used
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
U.K., http://www.energyinst.org.uk. solventsaretolueneandacetone.(Warning—Toluene,acetone
D3828 − 16a (2021)
and many other solvents are flammable and a health hazard. sides with a draft shield (see 6.3) for protection. Do not rely on
Dispose of solvents and waste material in accordance with tests made in a laboratory draft hood unless the extracted air
local regulations.) and vapors can be withdrawn without causing air currents over
the test cup during the ignition source application period.
7.2 Butane, Propane and Natural Gas—For use as a pilot
and ignition source (not required if an electric ignitor is used).
9.2 Read the manufacturer’s instructions on the care and
(Warning—Butane, propane and natural gases are flammable servicing of the instrument and for the correct operation of any
and a health hazard.) controls.
9.3 Prepare the apparatus for operation in accordance with
8. Sampling
the manufacturers’ instructions for calibrating, checking and
8.1 Obtain at least a 50 mL sample from a bulk test site in
operating the equipment, especially the operation of the igni-
accordance with Practices D4057, D4177, E300 or other
tion source. (Warning—An incorrectly set test flame size or
comparable sampling practices.
setting of an electric ignitor can significantly affect the test
result.)
8.2 Store samples in clean, tightly sealed containers at
normal room temperature (20 °C to 25 °C) or colder.
9.4 Clean the test cup, cover and its accessories with an
appropriate solvent (7.1) to remove any traces of gum or
8.3 Do not store samples for an extended period of time in
residue from the previous test. Wipe dry with absorbent paper.
gas permeable containers, such as those made of plastic,
Astream of dry clean air may be used to remove the last traces
because volatile material can diffuse through the walls of the
of solvent used. A pipe cleaner may be used to clean the filler
container. Samples in leaky containers are suspect and not a
orifice.
source of valid results.
9.5 Measure and record the barometric pressure (6.2) before
8.4 Erroneously high flash points can be obtained when
commencing a test.
precautions are not takentoavoidlossofvolatilematerials.Do
not open containers unnecessarily. Do not make a transfer
9.6 Use an electronic thermal flash detector for flash point
unless the sample temperature is at least 10 °C below the
testsonbiodieselssuchasfattyacidmethylesters(FAME)(see
expected flash point.Where possible perform the flash point as
A1.7). The flash detector may be used for other test materials.
the first test on the sample.
9.7 For sub-ambient test temperatures see AnnexA4, unless
8.5 Samples containing dissolved or free water may be
the apparatus has integral test cup cooling facilities.
dehydrated with calcium chloride. (Warning—If the sample is
expected of containing volatile components, the treatment as
10. Verification of Apparatus
described in 8.5 should be omitted.)
10.1 Verify and correct, if necessary, the readings on the
8.6 Cool, or adjust the temperature of the sample and its
temperature measuring device at least every 12 months, ac-
container to at least 10 °C below the expected flash point
cording to the manufacturer’s instructions and that the tem-
beforeopeningtoremovethetestspecimen.Ifanaliquotofthe
perature measuring device is in accordance with A1.2.2 and
original sample is to be stored prior to testing, ensure that the
Annex A5.
container is filled to between 85 % and 95 % of its capacity.
10.2 Verify the performance of the apparatus at least once
NOTE 1—Results of flash point tests can be affected if the sample
volume falls below 50 % of the container’s capacity.
per year by determining the flash point of a certified reference
material (CRM) such as those listed in Annex A2, which is
8.7 If sufficiently fluid, mix samples by gently shaking by
reasonably close to the expected temperature range of the
hand prior to removal of the test specimen, taking care to
samples to be tested. The material shall be tested according to
minimize the loss of volatile components. If the sample is too
Method B, Section 12 and the detected flash point determined
viscous at ambient temperature, gently warm the sample in its
in 12.1.6 and 12.1.6.1 shall be corrected for barometric
container to a temperature not warmer than 10 °C below the
pressure (see Section 13). The flash point obtained shall be
test temperature, such that the sample can be mixed by gentle
within the limits stated in TableA2.1 for the identified CRM or
shaking. Ensure that high pressures do not develop in the
within the limits calculated for an unlisted CRM (see Annex
container when warming.
A2).
8.8 If the sample cannot be made sufficiently fluid to be
10.3 Once the performance of the apparatus has been
introduced into the test cup through the orifice by heating in
verified, the flash point of secondary working standards (SWS)
accordance with 8.7, transfer the test specimen with a solids
can be determined along with their control limits. These
dispenserorspatulawhilethecoverisopen.Thespecimensize
secondary materials can then be utilized for more frequent
can be the mass equivalent of the required volume and the
performance checks (see Annex A2).
specimen should be spread over the bottom of the test cup as
evenly as possible. Precision has not been determined for solid
10.4 When the flash point obtained is not within the limits
samples.
stated in 10.2 or 10.3, check the condition and operation of the
apparatus to ensure conformity with the details listed in Annex
9. Preparation of Apparatus
A1, especially with regard to tightness of the cover (A1.2.1),
9.1 Place the apparatus on a level, stable surface. Unless the action of the shutter, the size or intensity of the ignition
tests are made in a draft-free area, surround the tester on three source, the position of the ignition source (A1.3), the operation
D3828 − 16a (2021)
of the flash detector (if fitted) and correct reading of the ignition source can cause a blue halo or an enlarged flame; this
temperaturemeasuringdevice.Afteranyadjustment,repeatthe is not a flash and should be ignored.
test in 10.2 or 10.3 using a fresh test specimen, with special
11.7 Record the test result as flash (or no flash) and the test
attentiontotheproceduraldetailsprescribedinthetestmethod.
temperature.
METHOD A—FLASH/NO FLASH TEST
11.8 Turn off the pilot and test flames (if used). Remove the
test specimen and clean the test cup and cover. It may be
11. Procedure
necessary to allow the test cup temperature to fall to a safe
11.1 Forspecificationpurposescarryoutaflash/noflashtest
level before cleaning.
at a temperature (actual) that allows for a correction due to the
METHOD B—FLASH POINT DETERMINATION
ambient atmospheric pressure at the time of the test. Use the
following equations to convert a specification flash point test
12. Procedure
requirement to the actual test temperature required for the test
and then round to the nearest 0.5 °C (1 °F).
12.1 This procedure repeats the procedures of Method A
(11.3 through 11.8) a number of times. Each test uses a fresh
Actual test temperature, °C 5 S 2 0.25~101.3 2 A! (1)
c
test specimen and a different temperature. The change of
Actual test temperature, °C 5 S 2 0.03 760 2 B (2)
~ !
c
temperature allows the determination of two temperatures 1 °C
Actual test temperature, °F 5 S 2 0.06 760 2 B (3)
~ !
f
(2 °F) or 0.5 °C (1 °F) apart for which the lower temperature
didnotresultinaflashwhilethehighertemperatureresultedin
where:
a flash (the flash point).
S = specification, or uncorrected target test temperature, °C,
c
12.1.1 Select the expected flash point of the sample as the
S = specification, or uncorrected target test temperature, °F,
f
initial test temperature and follow the procedure 11.3 to 11.8.
B = ambient barometric pressure, mm Hg, and
A = ambient barometric pressure, kPa. 12.1.2 If a flash is detected, repeat the procedure given in
11.3 to 11.8 testing a fresh specimen at a temperature 5 °C
11.2 Inspect the test cup and cover for cleanliness and
(9 °F) lower each time until no flash is detected.
correct operation, especially with regard to tightness of the
12.1.2.1 Proceed to 12.1.4.
cover (A1.2.1), the action of the shutter, the size or intensity of
12.1.3 When no flash was detected, repeat the procedure
the ignition source and the position of the ignition source
given in 11.3 to 11.8 testing a fresh specimen at a temperature
(A1.3). Clean if necessary (9.3). Put the cover in place and
5 °C (9 °F) higher each time until a flash is detected.
close securely.
12.1.4 Having established a flash within two temperatures
11.3 Follow the manufacturer’s instructions to set the test
5 °C (9 °F) apart, repeat the procedure at 1 °C (2 °F) intervals
temperature and the test time, and select the test specimen
fromthelowerofthetwotemperaturesuntilaflashisdetected.
volume in accordance with Table 1.
12.1.5 Record the temperature of the test when this flash
11.4 When the test cup is at the test temperature, fill the
occurs as the flash point, allowing for any known thermometer
appropriate syringe (A1.5, A1.6) with the sample to be tested;
correction.
transfer the syringe to the filling orifice, taking care not to lose
12.1.6 The flash point determined in 12.1.4 will be to the
any sample; discharge the test specimen into the test cup by
nearest 1 °C (2 °F).
fully depressing the syringe plunger; remove the syringe.
12.1.6.1 If improved accuracy is desired (that is, to the
11.5 Start the test timer; light the pilot light and adjust the
nearest 0.5 °C (1 °F)) test a fresh test specimen at a tempera-
test flame (if used) to conform to the 4 mm ( ⁄32 in.) gauge.
ture 0.5 °C (1 °F) below that at which the flash was detected in
12.1.4. If no flash is detected, the temperature recorded in
11.6 When the end of the test time is indicated, apply the
12.1.4 is the flash point to the nearest 0.5 °C (1 °F). If a flash
ignition source by slowly and uniformly opening the shutter
is detected at the lower temperature (12.1.6), record this latter
and closing it completely over a period of 2 ⁄2 s. Watch closely
temperature as the flash point.
foraflashatthe
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