Flash and Fire Points by Cleveland Open Cup Tester: Standard Test Method For

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Designation: D92 − 12b American Association State

Highway and Transportation Officials Standard


AASHTO No.: T48
DIN 51 376

Standard Test Method for


Flash and Fire Points by Cleveland Open Cup Tester1
This standard is issued under the fixed designation D92; 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

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.

*A Summary of Changes section appears at the end of this standard


Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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D92 − 12b
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
Petroleum Products minimum of 5 s.
D4206 Test Method for Sustained Burning of Liquid Mix-
5. Significance and Use
tures Using the Small Scale Open-Cup Apparatus
E1 Specification for ASTM Liquid-in-Glass Thermometers 5.1 The flash point is one measure of the tendency of the test
E300 Practice for Sampling Industrial Chemicals specimen to form a flammable mixture with air under con-
2.2 Energy Institute Standard:3 trolled laboratory conditions. It is only one of a number of
Specifications for IP Standard Thermometers properties that should be considered in assessing the overall
flammability hazard of a material.
2.3 ISO Standards:4
Guide 34 Quality Systems Guidelines for the Production of 5.2 Flash point is used in shipping and safety regulations to
Reference Materials define flammable and combustible materials. Consult the
Guide 35 Certification of Reference Material—General and particular regulation involved for precise definitions of these
Statistical Principles classifications.
5.3 Flash point can indicate the possible presence of highly
3. Terminology volatile and flammable materials in a relatively nonvolatile or
3.1 Definitions: nonflammable material. For example, an abnormally low flash
3.1.1 dynamic, adj—in petroleum products, the condition point on a test specimen of engine oil can indicate gasoline
where the vapor above the test specimen and the test specimen contamination.
are not in temperature equilibrium at the time that the ignition 5.4 This test method shall be used to measure and describe
source is applied. the properties of materials, products, or assemblies in response
3.1.1.1 Discussion—This is primarily caused by the heating to heat and a test flame under controlled laboratory conditions
of the test specimen at the constant prescribed rate with the and shall not be used to describe or appraise the fire hazard or
vapor temperature lagging behind the test specimen tempera- fire risk of materials, products, or assemblies under actual fire
ture. conditions. However, results of this test method may be used as
3.1.2 fire point, n—in petroleum products, the lowest tem- elements of a fire risk assessment that takes into account all of
perature corrected to a barometric pressure of 101.3 kPa (760 the factors that are pertinent to an assessment of the fire hazard
mm Hg), at which application of an ignition source causes the of a particular end use.
vapors of a test specimen of the sample to ignite and sustain
5.5 The fire point is one measure of the tendency of the test
burning for a minimum of 5 s under specified conditions of
specimen to support combustion.
test.
3.1.3 flash point, n— in petroleum products, the lowest 6. Apparatus
temperature corrected to a barometric pressure of 101.3 kPa 6.1 Cleveland Open Cup Apparatus (manual)—This appa-
(760 mm Hg), at which application of an ignition source causes ratus consists of the test cup, heating plate, test flame
the vapors of a specimen of the sample to ignite under specified applicator, heater, and supports described in detail in the Annex
conditions of test. A1. The assembled manual apparatus, heating plate, and cup
are illustrated in Figs. 1-3, respectively. Dimensions are listed
with the figures.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM 6.2 Cleveland Open Cup Apparatus (automated)—This ap-
Standards volume information, refer to the standard’s Document Summary page on paratus is an automated flash point instrument that shall
the ASTM website.
3
perform the test in accordance with Section 11 Procedure. The
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
U.K., http://www.energyinst.org.uk.
apparatus shall use the test cup with the dimensions as
4
Available from American National Standards Institute (ANSI), 25 W. 43rd St., described in Annex A1 and the application of the test flame
4th Floor, New York, NY 10036. shall be as described in Annex A1.

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D92 − 12b

FIG. 1 Cleveland Open Cup Apparatus

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

FIG. 2 Heating Plate

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

3
D92 − 12b

FIG. 3 Cleveland Open Cup

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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D92 − 12b
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
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

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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
Continue heating the test specimen at 5 to 6°C (9 to 11°F)/min
17°C (9 to 30°F)/min. When the test specimen temperature is and testing the test specimen every 2°C (5°F) as described in
approximately 56°C (100°F) below the expected flash point, 11.1.5 until the flash point is obtained.
decrease the heat so that the rate of temperature rise during the
last 28°C (50°F) before the flash point is 5 to 6°C (9 to NOTE 16—Flash point results determined in an unknown expected flash
11°F)/min. point mode should be considered approximate. This value can be used as
the expected flash point when a fresh specimen is tested in the standard
NOTE 12—With low flash point material or with highly viscous mode of operation.
material, it is advised to use the 5 to 6°C/min heating rate from the start 11.1.10 Record, as the observed flash point, the reading on
of the test to the end.
the temperature measuring device at the time the test flame
11.1.5 Apply the test flame when the temperature of the test causes a distinct flash in the interior of the test cup.
specimen is approximately 28°C below the expected flash 11.1.10.1 The sample is deemed to have flashed when a
point and each time thereafter at a temperature reading that is large flame appears at any point on the surface of the test
a multiple of 2°C. Pass the test flame across the center of the specimen and instantaneously propagates itself over the surface
test cup at right angles to the diameter, which passes through of the test specimen.
the temperature measuring device. With a smooth, continuous 11.1.11 The application of the test flame can cause a blue
motion, apply the test flame either in a straight line or along the halo or an enlarged flame prior to the actual flash point. This is
circumference of a circle having a radius of at least 150 6 1 not a flash point and shall be ignored.
mm (6.00 6 0.039 in.). The center of the test flame shall move 11.1.12 When a flash point or fire point is detected during
in a horizontal plane not more than 2 mm (5⁄64 in.) above the any preliminary test flame application, or on the first applica-
plane of the upper edge of the test cup and passing in one tion of the test flame, see 11.1.5, the test shall be discontinued,
direction only. At the time of the next test flame application, the result discarded, and the test repeated with a fresh test
pass the test flame in the opposite direction of the preceding specimen. The first application of the test flame with the fresh
application. The time consumed in passing the test flame across test specimen shall be at least 28°C (50°F) below the tempera-
the test cup in each case shall be approximately 1 6 0.1 s. ture found when the flash point was detected under the
conditions in 11.1.12.
NOTE 13—Some automated apparatus pass the test flame in one single
11.1.13 When the apparatus has cooled down to a safe
direction. Apparatus that operate in this manner will typically shut off the
test flame gas after each application, return to the starting position without handling temperature, less than 60°C (140°F), remove the test
creating a draft near and over the test cup, and the test flame will be cup and clean the test cup and the apparatus as recommended
relighted in such a manner that no fuel gas enters the cup vapor space by the manufacturer.
before the next test application.
NOTE 14—When determining the flash point of asphalt, it is recom- NOTE 17—Exercise care when cleaning the apparatus so as not to
damage or dislocate the automated flash detection system, when used, or
mended to carefully move fully to one side, such as with a spatula, any
temperature measuring device. See the manufacturer’s instructions for
surface film formed before each application of the ignition source.
proper care and maintenance.
Available data indicate that higher flash point is observed for asphalt
samples when surface film formed is not moved aside, compared to the 11.1.14 To determine the fire point, continue heating the test
flash point observed when the surface film is moved aside prior to the specimen after recording the flash point such that the test
application of the ignition source.
specimen temperature increases at a rate of 5 to 6°C (9 to
NOTE 15—An alternative to the moving aside of the formed surface film
11°F)/min. Continue the application of the test flame at 2°C
can be found in Appendix X1.
(5°F) intervals until the test specimen ignites and sustains
11.1.6 During the last 28°C (50°F) rise in temperature prior burning for a minimum of 5 s. Record the temperature of the
to the expected flash point, care shall be taken to avoid test specimen when the test flame, which caused the test
disturbing the vapors in the test cup with rapid movements or specimen to ignite was applied. Sustain burning as the ob-
drafts near the test cup. served fire point of the test specimen.

6
D92 − 12b
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
temperature of the test cup and the sample shall not exceed K = ambient barometric pressure, kPa.
56°C (100°F) below the expected flash point. If too much test NOTE 21—The barometric pressure used in this calculation is the
specimen has been added to the cup, remove the excess using ambient pressure for the laboratory at the time of test. Many aneroid
a syringe or similar device for withdrawal of fluid; however, if barometers, such as those used at weather stations and airports, are
precorrected to give sea level readings and would not give the correct
there is test specimen on the outside of the test cup, empty, reading for this test.
clean, and refill it. Destroy any air bubbles or foam on the
surface of the test specimen with a sharp knife or other suitable 12.2 Using the corrected flash point or fire point, or both, as
device, and maintain the required level of test specimen. If a determined in 12.1, round the values to the nearest 1°C (2°F)
foam persists during the final stages of the test, terminate the and record.
test, and disregard any results.
11.2.3 Solid material shall not be added to the test cup. Solid 13. Report
or viscous samples shall be heated until they are fluid before 13.1 Report the corrected flash point or fire point value, or
being poured into the test cup; however, the temperature of the both, as the Test Method D92 Cleveland open cup flash point
sample during heating shall not exceed 56°C (100°F) below the or fire point, or both, of the test specimen.
expected flash point.
11.2.4 Light the test flame, when necessary, and adjust it to 14. Precision and Bias
a diameter of 3.2 to 4.8 mm (1⁄8 to 3⁄16 in.) or to the size of the
14.1 Precision—The precision of this test method as deter-
comparison bead, if one is mounted on the apparatus.
mined by the statistical examination of the interlaboratory test
(Warning—Gas pressure supplied to the apparatus must not be
results is as follows:
allowed to exceed 3 kPa (12 in.) of water pressure.)
(Warning—Exercise care when using a gas test flame. If it 14.1.1 Repeatability—The difference between successive
should be extinguished it will not ignite the vapors in the test results, obtained by the same operator with the same apparatus
cup, and the gas for the test flame that then enters the vapor under constant operating conditions on identical test material,
space can influence the result.) (Warning— The operator shall would in the long run, in the normal and correct operation of
exercise care and take appropriate safety precautions during the the test method, exceed the following values in 1 case in 20.
initial application of the test flame since test specimens Flash point 8°C (15°F)
Fire point 8°C (15°F)
containing low-flash material can give an abnormally strong
flash when the test flame is first applied.) (Warning— The 14.1.2 Reproducibility—The difference between two single
operator shall exercise care and take appropriate safety precau- and independent results, obtained by different operators work-
tions during the performance of this test method. The tempera- ing in different laboratories on identical material, would in the
tures attained during this test, up to 400°C (752°F), are long run, in the normal and correct operation of the test
considered hazardous.) method, exceed the following values only in one case in 20.
Flash point 18°C (32°F)
NOTE 18—Some automated apparatus can perform preliminary test Fire point 14°C (25°F)
flame applications during the initial heating phase.
NOTE 19—Some automated apparatus can light the test flame automati- 14.2 The precision data for fire point is not known to have
cally and the size of the flame is preset. been developed in accordance with Precision Manual RR:D02-
NOTE 20—Test samples containing >1% silicones can create an 1007.
insulating deposit on ionization ring flash detectors, as used on most
automated apparatus, that can lead to erroneous results. If test samples are NOTE 22—The precisions for fire point were not determined in the
known to contain silicones, the use of the manual test is recommended. current interlaboratory program. Fire point is a parameter that is not
Ionization ring flash detectors suspected of giving erroneous results can be commonly specified, although in some cases, this temperature may be
cleaned using a suitable solvent. desired.
NOTE 23—The precision for asphalt type samples which have had any
11.2.5 Start the automated apparatus according to the manu- formed surface film removed has not been determined.
facturer’s instructions. The apparatus shall follow the proce- NOTE 24—The precision for asphalt type samples which have utilized
dural details described in 11.1.4 through 11.1.15. the procedure in Appendix X1 have not been determined.

7
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)

A1. CLEVELAND OPEN CUP TESTER

A1.1 Test Cup, conforming to Fig. 3 with dimensions as NOTE A1.1—A test flame relighting device, such as a pilot flame, is
shown with the figure. The cup shall be made of brass or other sometimes used to automatically relight the test flame in the event that it
non-rusting metal of equivalent heat conductivity. The cup may is extinguished during the test. This device should be designed such that
the unburned gas will not spread out over the test cup during the
be equipped with a handle. relighting.
A1.2 Heating Plate, shall be of sufficient dimension and A1.4 Heater—Heat may be supplied from any convenient
materials to ensure that thermal heat to the test cup is only source. The use of a gas burner or alcohol lamp is permitted,
applied to the bottom of the test cup and that extraneous heat but under no circumstances are products of combustion or free
to the test cup other than to the bottom is minimized. An
flame to be allowed to come up around the cup. An electric
example for manual apparatus that utilize Bunsen burners or
heater which can be controlled automatically or controlled by
exposed electric heating elements is shown in Fig. 2.
the user is preferred. The source of heat shall be centered under
A1.3 Ignition Source Applicator—The device for applying the opening of the heating plate with no local superheating.
the test flame may be of any suitable type. When using a test Flame-type heaters may be protected from drafts or excessive
flame, it is suggested that the tip be 1.6 6 0.05 mm (1⁄16 in.) in radiation by any suitable type of shield that does not project
diameter at the end, and that the orifice be approximately 0.8 6 above the level of the upper surface of the heating plate.
0.05 mm (1⁄32 in.) in diameter. The device for operating the test
flame applicator may be mounted in such a manner as to permit A1.5 Temperature Measuring Device Support—Any conve-
automated duplication of the sweep of the test flame, the radius nient device that will hold the temperature measuring device in
of swing being not less than 150 mm (6 in.). The center of the the specified position during a test and that will permit easy
test flame should be supported so that it swings in a plane not removal of the temperature measuring device from the test cup
greater than 2 mm (5⁄64 in.) above the plane of the rim of the upon completion of a test may be used.
cup. It is desired that a bead, having a diameter of 3.2 to 4.8
mm (1⁄8 to 3⁄16 in.), be mounted in a convenient position on the A1.6 Heating Plate Support—Any convenient support that
apparatus so that the size of the test flame can be compared to will hold the heating plate level and steady may be employed.
it.

8
D92 − 12b

A2. VERIFICATION OF APPARATUS PERFORMANCE

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
RR:D02-10076 guidelines or ISO Guide 34 and 35. the flash point in Table A2.1 can be found in research report RR:S15-
A2.1.1 Typical values of the flash point corrected for 1010.7
NOTE A2.2—Materials, purities, flash point values, and limits stated in
barometric pressure for some reference materials and their Table A2.1 were developed in an ASTM interlaboratory program to
typical limits are given in Table A2.1 (see Note A2.2). determine suitability of use for verification fluids in flash point test
Suppliers of CRM’s will provide certificates stating the methods. Other materials, purities, flash point values, and limits can be
method-specific flash point for each material of the current suitable when produced according to the practices of RR:D02-1007 or ISO
production batch. Calculation of the limits for these other Guides 34 and 35. Certificates of performance of such materials should be
consulted before use, as the flashpoint value will vary dependent on the
composition of each CRM batch.
6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1007. A2.2 Secondary Working Standard (SWS)—SWS is a stable,
pure (99 + mole % purity) hydrocarbon, or other petroleum
TABLE A2.1 D92 Typical Flash Point Values and Typical Limits product whose composition is known to remain appreciably
for CRM stable.
Hydrocarbon Purity (mole %) Flash Point (°C) Limits (°C)
n–tetradecane 99 + 115.5 ±8.0
7
n–hexadecane 99 + 138.8 ±8.0 Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:S15-1010.

9
D92 − 12b
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

X1.1 Introduction X1.2 Materials Required


X1.1.1 This technique to prevent surface skin formation X1.2.1 Filter Paper, qualitative, No. 417 (or equivalent), 7.5
when testing flash point of asphalts by Test Method D92 was cm diameter.
developed by Imran Hussami of Frontier El Dorado Refining
Company.

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

10
D92 − 12b
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.)

(1) Added to 9.4.

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.)

(1) Added new warning to 11.1.3. (2) Amended Note 11.

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.)

(1) Added new Note 20 and renumbered subsequent notes.

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11

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