F ASTM D92b
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INTRODUCTION
This flash point and fire point test method is a dynamic method and depends on definite rates of
temperature increases to control the precision of the test method. Its primary use is for viscous
materials having flash point of 79°C (175°F) and above. It is also used to determine fire point, which
is a temperature above the flash point, at which the test specimen will support combustion for a
minimum of 5 s. Do not confuse this test method with Test Method D4206, which is a sustained
burning test, open cup type, at a specific temperature of 49°C (120°F).
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* but significant, concentrations of lower flash point substances that may
escape detection by Test Method D92. Test Method D1310 can be
1.1 This test method describes the determination of the flash employed if the flash point is known to be below 79°C (175°F).
point and fire point of petroleum products by a manual
Cleveland open cup apparatus or an automated Cleveland open 1.3 The values stated in SI units are to be regarded as the
cup apparatus. standard. The values given in parentheses are for information
only.
NOTE 1—The precisions for fire point were not determined in the
current interlaboratory program. Fire point is a parameter that is not 1.4 WARNING—Mercury has been designated by many
commonly specified, although in some cases, knowledge of this flamma- regulatory agencies as a hazardous material that can cause
bility temperature may be desired.
central nervous system, kidney and liver damage. Mercury, or
1.2 This test method is applicable to all petroleum products its vapor, may be hazardous to health and corrosive to
with flash points above 79°C (175°F) and below 400°C materials. Caution should be taken when handling mercury and
(752°F) except fuel oils. mercury containing products. See the applicable product Ma-
NOTE 2—This test method may occasionally be specified for the terial Safety Data Sheet (MSDS) for details and EPA’s
determination of the fire point of a fuel oil. For the determination of the website—http://www.epa.gov/mercury/faq.htm—for addi-
flash points of fuel oils, use Test Method D93. Test Method D93 should tional information. Users should be aware that selling mercury
also be used when it is desired to determine the possible presence of small, and/or mercury containing products into your state or country
may be prohibited by law.
1
This test method is under the joint jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
1.5 This standard does not purport to address all of the
Subcommittee D02.08 on Volatility. In the IP, this test method is under the safety concerns, if any, associated with its use. It is the
jurisdiction of the Standardization Committee. This test method was adopted as a responsibility of the user of this standard to establish appro-
joint ASTM-IP standard in 1965. priate safety and health practices and determine the applica-
Current edition approved Dec. 1, 2012. Published March 2013. Originally
approved in 1921. Last previous edition approved in 2012 as D92–12a. DOI: bility of regulatory limitations prior to use. For specific
10.1520/D0092-12B. warning statements, see 6.4, 7.1, 11.1.3, and 11.2.4.
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2. Referenced Documents 4. Summary of Test Method
2
2.1 ASTM Standards: 4.1 Approximately 70 mL of test specimen is filled into a
D93 Test Methods for Flash Point by Pensky-Martens test cup. The temperature of the test specimen is increased
Closed Cup Tester rapidly at first and then at a slower constant rate as the flash
D140 Practice for Sampling Bituminous Materials point is approached. At specified intervals a test flame is passed
D1310 Test Method for Flash Point and Fire Point of Liquids across the cup. The flash point is the lowest liquid temperature
by Tag Open-Cup Apparatus at which application of the test flame causes the vapors of the
D4057 Practice for Manual Sampling of Petroleum and test specimen of the sample to ignite. To determine the fire
Petroleum Products point, the test is continued until the application of the test flame
D4177 Practice for Automatic Sampling of Petroleum and causes the test specimen to ignite and sustain burning for a
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millimetres inches
min max min max
A 6 7 0.236 0.276
B 0.5 1.0 0.020 0.039
C 6 7 0.236 0.276
D—Diameter 55 56 2.165 2.205
E—Diameter 69.5 70.5 2.736 2.776
F—Diameter 146 159 5.748 6.260
6.3 Temperature Measuring Device—A thermometer having prescribed in Specification E1 or in the Specifications for IP
the range as shown below and conforming to the requirements
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Standard Thermometers, or an electronic temperature measur- at least 56°C (100°F) below the expected flash point. When
ing device, such as a resistance thermometer or thermocouple. possible, flash point should be the first test performed on a
The device shall exhibit the same temperature response as the sample and the sample should be stored at low temperature.
mercury thermometers.
NOTE 3—Typical sample storage temperature is normal room tempera-
Thermometer Number ture or lower.
Temperature Range ASTM IP
−6 to +400°C 11C 28C 8.4 Do not store samples in gas-permeable containers since
20 to 760°F 11F
volatile material may diffuse through the walls of the enclo-
6.4 Test Flame—Natural gas (methane) flame and bottled sure. Samples in leaky containers are suspect and not a source
gas (butane, propane) flame have been found acceptable for use of valid results.
as the ignition source. The gas flame device is described in
detail in Annex A1. (Warning— Gas pressure supplied to the 8.5 Light hydrocarbons may be present in the form of gases,
apparatus must not be allowed to exceed 3 kPa (12 in.) of water such as propane or butane, and may not be detected by testing
pressure.) because of losses during sampling and filling of the test cup.
This is especially evident on heavy residuums or asphalts from
7. Reagents and Materials solvent extraction processes.
7.1 Cleaning Solvents—Use suitable technical grade solvent 8.6 Samples of very viscous materials can be warmed until
capable of cleaning out the test specimen from the test cup and they are reasonably fluid before they are tested. However, no
drying the test cup. Some commonly used solvents are toluene sample shall be heated more than is absolutely necessary. It
and acetone. (Warning—Toluene, acetone, and many solvents shall never be heated above a temperature of 56°C (100°F)
are flammable. Health hazard. Dispose of solvents and waste below its expected flash point. When the sample has been
material in accordance with local regulations.) heated above this temperature, allow the sample to cool until it
is at least 56°C (100°F) below the expected flash point before
8. Sampling transferring.
8.1 Obtain a sample in accordance with the instructions
NOTE 4—Typically, the sample containers for these types of samples
given in Practices D140, D4057, D4177 or E300. will remain closed during the warming process.
8.2 At least 70 mL of sample is required for each test. Refer 8.7 Samples containing dissolved or free water can be
to Practice D4057. dehydrated with calcium chloride or by filtering through a
8.3 Erroneously high flash points may be obtained if pre- qualitative filter paper or a loose plug of dry absorbent cotton.
cautions are not taken to avoid the loss of volatile material. Do Samples of very viscous materials can be warmed until they are
not open containers unnecessarily; this will prevent loss of reasonably fluid before they are filtered, but they shall not be
volatile material and possible introduction of moisture. Do not heated for prolonged periods or above a temperature of 56°C
make a transfer of the sample unless the sample temperature is (100°F) below its expected flash point.
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NOTE 5—If the sample is suspected of containing volatile contaminants, material shall be tested according to the procedure of this test
the treatment described in 8.6 and 8.7 should be omitted. method and the observed flash point obtained in 11.1.10 or
11.2.5 shall be corrected for barometric pressure (see Section
9. Preparation of Apparatus 12). The flash point obtained shall be within the limits stated in
9.1 Support the manual or automated apparatus on a level Table A2.1 for the identified CRM or within the limits
steady surface, such as a table. calculated for an unlisted CRM (see Annex A2).
9.2 Tests are to be performed in a draft-free room or 10.4 Once the performance of the apparatus has been
compartment. Tests made in a laboratory hood or in any verified, the flash point of secondary working standards
location where drafts occur are not to be relied upon. (SWSs) can be determined along with their control limits.
NOTE 6—A draft shield is recommended to prevent drafts from
These secondary materials can then be utilized for more
disturbing the vapors above the test cup. This shield should cover at least frequent performance checks (see Annex A2).
three sides of the test cup vicinity. Some apparatus may already include a
NOTE 10—The verification fluid is a material with a predetermined,
built-in draft shield.
interlaboratory tested, flash point temperature that is used to verify proper
NOTE 7—With some samples whose vapors or products of pyrolysis are
operation of the apparatus. Calibration is undertaken by the operator
objectionable, it is permissible to place the apparatus along with a shield
according to the apparatus manufacturers’ instructions should the result of
into a hood, the draft of which is adjusted so that the vapors may be
the verification be outside the stated reproducibility.
withdrawn without causing air currents over the test cup during the final
56°C (100°F) rise in temperature prior to the flash point. 10.5 When the flash point obtained is not within the limits
9.3 Wash the test cup with the cleaning solvent to remove stated in 10.3 or 10.4, check the condition and operation of the
any test specimen or traces of gum or residue remaining from apparatus to ensure conformity with the details listed in Annex
a previous test. If any deposits of carbon are present, they A1, especially in regard to the position of the temperature
should be removed with a material such as a very fine grade of measuring device, the application of the test flame, and the
steel wool. Ensure that the test cup is completely clean and dry heating rate. After adjustment of the apparatus, repeat the test
before using again. If necessary, flush the test cup with cold with a fresh test specimen (see 10.3) with special attention to
water and dry for a few minutes over an open flame or a hot the procedural details prescribed in Section 11.
plate to remove the last traces of solvent and water. Cool the
test cup to at least 56°C (100°F) below the expected flash point 11. Procedure
before using. 11.1 Manual Apparatus:
9.4 Support the temperature measuring device in a vertical 11.1.1 Fill the test cup with the sample so that the top of the
position with the bottom of the device located 6.4 6 0.1 mm meniscus of the test specimen is level with the filling mark, and
(1⁄4 6 1⁄50 in.) up from the bottom of the inside of the test cup position the test cup on the center of the heating plate. The
and located at a point halfway between the center and the side temperature of the test cup and the sample shall not exceed
of the test cup on a diameter perpendicular to the arc (or line) 56°C (100°F) below the expected flash point. If too much test
of the sweep of the test flame and on the side opposite to the specimen has been added to the cup, remove the excess using
test flame applicator mounting position. It is permissible for a syringe or similar device for withdrawal of fluid. However, if
electronic temperature measuring devices to be mounted in a there is test specimen on the outside of the test cup, empty,
non-vertical position provided that performance is in accor- clean, and refill it. Destroy any air bubbles or foam on the
dance with the requirements given in 6.3. surface of the test specimen with a sharp knife or other suitable
device and maintain the required level of test specimen. If a
NOTE 8—The immersion line engraved on the ASTM or IP thermometer
foam persists during the final stages of the test, terminate the
will be 2 6 0.1 mm (5⁄64 6 1⁄50 in.) below the level of the rim of the cup
when the thermometer is properly positioned. test and disregard any results.
NOTE 9—Some automated apparatus is capable of positioning the 11.1.2 Solid material shall not be added to the test cup. Solid
temperature measuring device automatically. Refer to the manufacturer’s or viscous samples shall be heated until they are fluid before
instructions for proper installation and adjustment. being poured into the test cup; however, the temperature of the
9.5 Prepare the manual apparatus or the automated appara- sample during heating shall not exceed 56°C (100°F) below the
tus for operation according to the manufacturer’s instructions expected flash point.
for calibrating, checking, and operating the equipment. 11.1.3 Light the test flame and adjust it to a diameter of 3.2
to 4.8 mm (1⁄8 to 3⁄16 in.) or to the size of the comparison bead,
10. Calibration and Standardization if one is mounted on the apparatus (see Annex A1).
10.1 Adjust the automated flash point detection system, (Warning—Gas pressure supplied to the apparatus must not be
No reproduction or networking permitted without license from IHS
when used, according to the manufacturer’s instructions. allowed to exceed 3 kPa (12 in.) of water pressure.)
(Warning—Exercise care when using a gas test flame. If it
10.2 Calibrate the temperature measuring device according should be extinguished it will not ignite the vapors in the test
to the manufacturer’s instructions. cup, and the gas for the test flame that then enters the vapor
10.3 Verify the performance of the manual apparatus or the space can influence the result.) (Warning—The operator shall
automated apparatus at least once per year by determining the exercise care and take appropriate safety precautions during the
flash point of a certified reference material (CRM), such as initial application of the test flame since test specimens
those listed in Annex A2, which is reasonably close to the containing low-flash material can give an abnormally strong
expected temperature range of the samples to be tested. The flash when the test flame is first applied.) (Warning—As a
D92 − 12b
safety practice, it is strongly advised, when using automated or 11.1.7 When a foam persists on top of the test specimen
manual apparatus, before heating the test cup and specimen, to during the last 28°C (50°F) rise in temperature prior to the
pass the test flame across the specimen in the test cup to check expected flash point, terminate the test and disregard any
for the presence of unexpected volatile material.) (Warning— results.
The operator shall exercise care and take appropriate safety 11.1.8 Meticulous attention to all details relating to the test
precautions during the performance of this test method. The flame, size of the test flame, rate of temperature increase, and
temperatures attained during this test, up to 400°C (752°F), are rate of passing the test flame over the test specimen is required
considered hazardous.) for proper results.
11.1.9 When testing a sample whose expected flash point
NOTE 11—Some further preliminary test flame applications during the
temperature is not known, bring the test specimen in the test
initial heating phase may be useful in detecting whether unexpected
volatile material is present in the sample. A typical interval is at the cup to a temperature no greater than 50°C (122°F), or if the
beginning of the initial heating phase and then every 10°C up to the sample required heating to be transferred into the test cup,
standard test flame application temperature. See 11.1.5. bring the test specimen in the test cup to that temperature.
Apply the test flame, in the manner described in 11.1.5,
11.1.4 Apply heat initially at such a rate that the temperature
beginning at least 5°C (9°F) above the starting temperature.
as indicated by the temperature measuring device increases 5 to
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11.1.15 When the apparatus has cooled down to a safe 12. Calculations
handling temperature, less than 60°C (140°F), remove the test
12.1 Observe and record the ambient barometric pressure
cup and clean the test cup and the apparatus as recommended
(see Note 21) at the time of the test. When the pressure differs
by the manufacturer.
from 101.3 kPa (760 mm Hg), correct the flash point or fire
11.2 Automated Apparatus: point, or both, as follows:
11.2.1 The automated apparatus shall be capable of per- Corrected flash point 5 C10.25 ~ 101.3 2 K ! (1)
forming the procedure as described in 11.1, including control
Corrected flash point 5 F10.06 ~ 760 2 P ! (2)
of the heating rate, application of the test flame, detection of
the flash point, or fire point, or both, and recording the flash Corrected flash point 5 C10.033 ~ 760 2 P ! (3)
point or fire point, or both. where:
11.2.2 Fill the test cup with the sample so that the top of the C = observed flash point, °C,
meniscus of the test specimen is level with the filling mark, and F = observed flash point, °F,
position the test cup on the center of the heating plate. The P = ambient barometric pressure, mm Hg, and
D92 − 12b
14.3 Bias—The procedure of this test method has no bias 14.5 The precision data for flash point were developed in a
because flash point and fire point can be defined only in terms 1991 cooperative test program using seven samples of base
of this test method. oils, asphalt, and lubricating oils. Five laboratories participated
with the manual apparatus and eight laboratories participated
14.4 Relative Bias—Statistical evaluation of the data did not with the automated equipment. Information on the type of
detect any significant difference between the reproducibility samples and their average flash point are in the research report
variances of manual and automated Cleveland flash point available at ASTM Headquarters.5
results for the samples studied with the exception of multi-
viscosity lubricating oil and white mineral oil. Evaluation of 15. Keywords
the data did not detect any significant difference between 15.1 automated Cleveland open cup; Cleveland open cup;
averages of manual and automated Cleveland flash point for fire point open cup for flash point; flammability; flash point;
the samples studied with the exception of multi-viscosity petroleum products
lubricating oil, which showed some bias. In any case of
dispute, the flash point as determined by the manual procedure 5
Supporting data have been filed at ASTM International Headquarters and may
shall be considered the referee test. be obtained by requesting Research Report RR:S15-1009.
ANNEXES
(Mandatory Information)
D92 − 12b
A2.1 Certified Reference Material (CRM)—CRM is a CRM’s can be determined from the reproducibility values of
stable, pure (99 + mole % purity) hydrocarbon or other stable this test method, reduced by interlaboratory effect and then
petroleum product with a method-specific flash point estab- multiplied by 0.7.
lished by a method-specific interlaboratory study following NOTE A2.1—Supporting data for the interlaboratory study to generate
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A2.2.1 Establish the mean flash point and the statistical
control limits (3σ) for the SWS using standard statistical
techniques.8
8
MNL7, Manual on Presentation of Data and Control Chart Analysis, 6th ed.,
ASTM International, 1990.
APPENDIX
(Nonmandatory Information)
X1. TECHNIQUE TO PREVENT SURFACE SKIN FORMATION WHEN TESTING FLASH POINT OF ASPHALTS BY TEST
METHOD D92
NOTE 1—Use of this alternate technique may cause bubbling in some samples. Bubbling could interfere with automatic flash detection devices, and
it also may cause a slower heating rate in some samples.
FIG. X1.1 Technique to Prevent Surface Skin Formation When Testing Flash Point of Asphalts by Test Method D92
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X1.2.2 Restraining Tension Ring, metal wire, circular, but X1.3.3 Place the restraining tension-ring snugly over the
with its 15 mm straight ends folded inwards, parallel to each curved portion of the filter paper in the base of the cup. (The
other (see Fig. X1.1). Dimensions: wire about 2 mm thick, 62 tension-ring prevents the filter paper from moving upward
to 63 outside diameter with bent ends 15 mm apart along the during the test.)
circumference of the circle. Total length of wire is about 210
mm. An ordinary metal coat hanger or similar material can be X1.3.4 Fill the cup with the sample 4 to 5 mm below the
used to make the tension-ring. filling mark (this is to compensate for the sample that is
absorbed by the filter paper which will be released during the
X1.2.3 Single-Hole Punch, (or equivalent) capable of mak-
test). (Warning—Filling all the way to the filling mark could
ing a 6 mm diameter hole in the center of the filter paper.
produce premature flash point results.)
X1.3 Procedure X1.3.5 Start the test either using a manual tester or an
X1.3.1 Determine the center of the filter paper by means of automatic unit (following manufacturer’s instructions) and
a ruler. Using the single-hole punch, punch a 6-mm diameter determine the flash point.
hole in the center of the 7.5 cm diameter qualitative filter paper.
X1.3.6 Report the flash point corrected for bariometric
X1.3.2 Curl up the sides of the filter paper, about 6 mm all pressure to the nearest 1°C.
around, and place it in the base of the Cleveland open cup flash
point test cup, with the 6-mm skirt facing upward (see Fig.
X1.1).
SUMMARY OF CHANGES
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D92–12a) that may impact the use of this standard. (Approved Dec. 1, 2012.)
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D92–12) that may impact the use of this standard. (Approved Nov. 1, 2012.)
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D92–11) that may impact the use of this standard. (Approved April 15, 2012.)
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