ASTM D92-05 Standard Test Method For Flash and Fire Points by Cleveland Open Cup Tester PDF
ASTM D92-05 Standard Test Method For Flash and Fire Points by Cleveland Open Cup Tester PDF
Designation: D 92 05
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 79C (175F) 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 D 4206, which is a sustained
burning test, open cup type, at a specific temperature of 49C (120F).
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.
1.3 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
only.
1.4 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. For specific
warning statements, see 6.4, 7.1, 11.1.3, and 11.2.4.
1. Scope*
1.1 This test method describes the determination of the flash
point and fire point of petroleum products by a manual
Cleveland open cup apparatus or an automated Cleveland open
cup apparatus.
NOTE 1The precisions for fire point were not determined in the
current interlaboratory program. Fire point is a parameter that is not
commonly specified, although in some cases, knowledge of this flammability temperature may be desired.
2. Referenced Documents
2.1 ASTM Standards: 2
D 93 Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester
D 140 Practice for Sampling Bituminous Materials
D 1310 Test Method for Flash Point and Fire Points of
Liquids by Tag Open-Cup Apparatus
D 4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
D 4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
1
This test method is under the joint jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility. In the IP, this test method is under the jurisdiction of the
Standardization Committee. This test method was adopted as a joint ASTM-IP
standard in 1965.
Current edition approved June 1, 2005. Published July 2005. Originally approved
in 1921. Last previous edition approved in 2002 as D 9202b.
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
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
D 92 05
point, the test is continued until the application of the test flame
causes the test specimen to ignite and sustain burning for a
minimum of 5 s.
D 4206 Test Method for Sustained Burning of Liquid Mixtures Using the Small Scale Open-Cup Apparatus
E 1 Specification for ASTM Liquid-in-Glass Thermometers
E 300 Practice for Sampling Industrial Chemicals3
2.2 Energy Institute Standard:4
Specifications for IP Standard Thermometers
2.3 ISO Standards:5
Guide 34 Quality Systems Guidelines for the Production of
Reference Materials
Guide 35 Certification of Reference MaterialGeneral and
Statistical Principles
3. Terminology
3.1 Definitions:
3.1.1 dynamic, adjin petroleum products, the condition
where the vapor above the test specimen and the test specimen
are not in temperature equilibrium at the time that the ignition
source is applied.
3.1.1.1 DiscussionThis is primarily caused by the heating
of the test specimen at the constant prescribed rate with the
vapor temperature lagging behind the test specimen temperature.
3.1.2 fire point, nin petroleum products, the lowest temperature corrected to a barometric pressure of 101.3 kPa (760
mm Hg), at which application of an ignition source causes the
vapors of a test specimen of the sample to ignite and sustain
burning for a minimum of 5 s under specified conditions of
test.
3.1.3 flash point, nin petroleum products, the lowest
temperature corrected to a barometric pressure of 101.3 kPa
(760 mm Hg), at which application of an ignition source causes
the vapors of a specimen of the sample to ignite under specified
conditions of test.
3.1.3.1 DiscussionThe test specimen is deemed to have
flashed when a flame appears and instantaneously propagates
itself over the entire surface of the test specimen.
3.1.3.2 DiscussionWhen the ignition source is a test
flame, the application of the test flame can cause a blue halo or
an enlarged flame prior to the actual flash point. This is not a
flash point and shall be ignored.
6. Apparatus
6.1 Cleveland Open Cup Apparatus (manual)This apparatus consists of the test cup, heating plate, test flame applicator, heater, and supports described in detail in the Annex A1.
The assembled manual apparatus, heating plate, and cup are
illustrated in Figs. 1-3, respectively. Dimensions are listed with
the figures.
6.2 Cleveland Open Cup Apparatus (automated)This apparatus is an automated flash point instrument that shall
perform the test in accordance with Section 11 Procedure. The
apparatus shall use the test cup with the dimensions as
described in Annex A1 and the application of the test flame
shall be as described in Annex A1.
6.3 Temperature Measuring DeviceA thermometer having the range as shown below and conforming to the requirements prescribed in Specification E 1 or in the Specifications
for IP Standard Thermometers, or an electronic temperature
measuring device, such as a resistance thermometer or thermocouple. The device shall exhibit the same temperature
response as the mercury thermometers.
Withdrawn.
Available from Energy Institute, 61 New Cavendish St., London, W1M 8AR,
U.K.
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036.
Temperature Range
6 to +400C
20 to 760F
Thermometer Number
ASTM IP
11C 28C
11F
D 92 05
A
B
C
DDiameter
EDiameter
FDiameter
min
6
0.5
6
55
69.5
146
millimetres
max
7
1.0
7
56
70.5
159
inches
min
0.236
0.020
0.236
2.165
2.736
5.748
max
0.276
0.039
0.276
2.205
2.776
6.260
D 92 05
as the ignition source. The gas flame device is described in
detail in Annex A1. (WarningGas pressure supplied to the
apparatus must not be allowed to exceed 3 kPa (12 in.) of water
pressure.)
9. Preparation of Apparatus
9.1 Support the manual or automated apparatus on a level
steady surface, such as a table.
9.2 Tests are to be performed in a draft-free room or
compartment. Tests made in a laboratory hood or in any
location where drafts occur are not to be relied upon.
NOTE 6A draft shield is recommended to prevent drafts from disturbing the vapors above the test cup. This shield should cover at least three
sides of the test cup vicinity. Some apparatus may already include a
built-in draft shield.
NOTE 7With some samples whose vapors or products of pyrolysis are
objectionable, it is permissible to place the apparatus along with a shield
into a hood, the draft of which is adjusted so that the vapors may be
withdrawn without causing air currents over the test cup during the final
56C (100F) rise in temperature prior to the flash point.
8. Sampling
8.1 Obtain a sample in accordance with the instructions
given in Practices D 140, D 4057, D 4177 or E 300.
8.2 At least 70 mL of sample is required for each test. Refer
to Practice D 4057.
8.3 Erroneously high flash points may be obtained if precautions are not taken to avoid the loss of volatile material. Do
not open containers unnecessarily; this will prevent loss of
volatile material and possible introduction of moisture. Do not
make a transfer of the sample unless the sample temperature is
at least 56C (100F) below the expected flash point. When
possible, flash point should be the first test performed on a
sample and the sample should be stored at low temperature.
9.3 Wash the test cup with the cleaning solvent to remove
any test specimen or traces of gum or residue remaining from
a previous test. If any deposits of carbon are present, they
should be removed with a material such as a very fine grade of
steel wool. Ensure that the test cup is completely clean and dry
before using again. If necessary, flush the test cup with cold
water and dry for a few minutes over an open flame or a hot
plate to remove the last traces of solvent and water. Cool the
test cup to at least 56C (100F) below the expected flash point
before using.
9.4 Support the temperature measuring device in a vertical
position with the bottom of the device located 6.4 6 0.1 mm
(14 6 150 in.) up from the bottom of the inside of the test cup
and located at a point halfway between the center and the side
of the test cup on a diameter perpendicular to the arc (or line)
of the sweep of the test flame and on the side opposite to the
test flame applicator mounting position.
NOTE 8The immersion line engraved on the ASTM or IP thermometer will be 2 6 0.1 mm (564 6 150 in.) below the level of the rim of the
cup when the thermometer is properly positioned.
NOTE 9Some automated apparatus is capable of positioning the
temperature measuring device automatically. Refer to the manufacturers
instructions for proper installation and adjustment.
9.5 Prepare the manual apparatus or the automated apparatus for operation according to the manufacturers instructions
for calibrating, checking, and operating the equipment.
10. Calibration and Standardization
10.1 Adjust the automated flash point detection system,
when used, according to the manufacturers instructions.
10.2 Calibrate the temperature measuring device according
to the manufacturers instructions.
10.3 Verify the performance of the manual apparatus or the
automated apparatus at least once per year by determining the
flash point of a certified reference material (CRM), such as
those listed in Annex A2, which is reasonably close to the
expected temperature range of the samples to be tested. The
material shall be tested according to the procedure of this test
method and the observed flash point obtained in 11.1.10 or
11.2.5 shall be corrected for barometric pressure (see Section
12). The flash point obtained shall be within the limits stated in
Table A2.1 for the identified CRM or within the limits
calculated for an unlisted CRM (see Annex A2).
D 92 05
10.4 Once the performance of the apparatus has been
verified, the flash point of secondary working standards
(SWSs) can be determined along with their control limits.
These secondary materials can then be utilized for more
frequent performance checks (see Annex A2).
NOTE 11With low flash point material or with highly viscous material, it is advised to use the 5 to 6C/min heating rate from the start of the
test to the end.
11.1.5 Apply the test flame when the temperature of the test
specimen is approximately 28C below the expected flash
point and each time thereafter at a temperature reading that is
a multiple of 2C. Pass the test flame across the center of the
test cup at right angles to the diameter, which passes through
the temperature measuring device. With a smooth, continuous
motion, apply the test flame either in a straight line or along the
circumference of a circle having a radius of at least 150 6 1
mm (6.00 6 0.039 in.). The center of the test flame shall move
in a horizontal plane not more than 2 mm (564 in.) above the
plane of the upper edge of the test cup and passing in one
direction only. At the time of the next test flame application,
pass the test flame in the opposite direction of the preceding
application. The time consumed in passing the test flame across
the test cup in each case shall be approximately 1 6 0.1 s.
10.5 When the flash point obtained is not within the limits
stated in 10.3 or 10.4, check the condition and operation of the
apparatus to ensure conformity with the details listed in Annex
A1, especially in regard to the position of the temperature
measuring device, the application of the test flame, and the
heating rate. After adjustment of the apparatus, repeat the test
with a fresh test specimen (see 10.3) with special attention to
the procedural details prescribed in Section 11.
11. Procedure
11.1 Manual Apparatus:
11.1.1 Fill the test cup with the sample so that the top of the
meniscus of the test specimen is level with the filling mark, and
position the test cup on the center of the heating plate. The
temperature of the test cup and the sample shall not exceed
56C (100F) below the expected flash point. If too much test
specimen has been added to the cup, remove the excess using
a syringe or similar device for withdrawal of fluid. However, if
there is test specimen on the outside of the test cup, empty,
clean, and refill it. Destroy any air bubbles or foam on the
surface of the test specimen with a sharp knife or other suitable
device and maintain the required level of test specimen. If a
foam persists during the final stages of the test, terminate the
test and disregard any results.
11.1.2 Solid material shall not be added to the test cup. Solid
or viscous samples shall be heated until they are fluid before
being poured into the test cup; however, the temperature of the
sample during heating shall not exceed 56C (100F) below the
expected flash point.
11.1.3 Light the test flame and adjust it to a diameter of 3.2
to 4.8 mm (18 to 316 in.) or to the size of the comparison bead,
if one is mounted on the apparatus (see Annex A1).
(WarningGas pressure supplied to the apparatus must not be
allowed to exceed 3 kPa (12 in.) of water pressure.)
(WarningExercise care when using a gas test flame. If it
should be extinguished it will not ignite the vapors in the test
cup, and the gas for the test flame that then enters the vapor
space can influence the result.) (WarningThe operator shall
exercise care and take appropriate safety precautions during the
initial application of the test flame since test specimens
containing low-flash material can give an abnormally strong
flash when the test flame is first applied.) (WarningThe
operator shall exercise care and take appropriate safety precautions during the performance of this test method. The temperatures attained during this test, up to 400C (752F), are
considered hazardous.)
11.1.4 Apply heat initially at such a rate that the temperature
as indicated by the temperature measuring device increases 5 to
NOTE 12When determining the flash point of asphalt, it is recommended to carefully move fully to one side, such as with a spatula, any
surface film formed before each application of the ignition source.
Available data indicate that higher flash point is observed for asphalt
samples when surface film formed is not moved aside, compared to the
flash point observed when the surface film is moved aside prior to the
application of the ignition source.
NOTE 13An alternative to the moving aside of the formed surface
film can be found in Appendix X1.
D 92 05
being poured into the test cup; however, the temperature of the
sample during heating shall not exceed 56C (100F) below the
expected flash point.
11.2.4 Light the test flame, when necessary, and adjust it to
a diameter of 3.2 to 4.8 mm (18 to 316 in.) or to the size of the
comparison bead, if one is mounted on the apparatus.
(WarningGas pressure supplied to the apparatus must not be
allowed to exceed 3 kPa (12 in.) of water pressure.)
(WarningExercise care when using a gas test flame. If it
should be extinguished it will not ignite the vapors in the test
cup, and the gas for the test flame that then enters the vapor
space can influence the result.) (WarningThe operator shall
exercise care and take appropriate safety precautions during the
initial application of the test flame since test specimens
containing low-flash material can give an abnormally strong
flash when the test flame is first applied.) (WarningThe
operator shall exercise care and take appropriate safety precautions during the performance of this test method. The temperatures attained during this test, up to 400C (752F), are
considered hazardous.)
NOTE 16Some automated apparatus can light the test flame automatically and the size of the flame is preset.
11.2.5 Start the automated apparatus according to the manufacturers instructions. The apparatus shall follow the procedural details described in 11.1.4 through 11.1.15.
12. Calculations
12.1 Observe and record the ambient barometric pressure
(see Note 17) at the time of the test. When the pressure differs
from 101.3 kPa (760 mm Hg), correct the flash point or fire
point, or both, as follows:
Corrected flash point 5 C 1 0.25 ~101.3 2 K!
(1)
(2)
(3)
where:
C = observed flash point, C,
F = observed flash point, F,
P = ambient barometric pressure, mm Hg, and
K = ambient barometric pressure, kPa.
NOTE 17The barometric pressure used in this calculation is the
ambient pressure for the laboratory at the time of test. Many aneroid
barometers, such as those used at weather stations and airports, are
precorrected to give sea level readings and would not give the correct
reading for this test.
D 92 05
14. Precision and Bias
14.1 PrecisionThe precision of this test method as determined by the statistical examination of the interlaboratory test
results is as follows:
14.1.1 RepeatabilityThe difference between successive
results, obtained by the same operator with the same apparatus
under constant operating conditions on identical test material,
would in the long run, in the normal and correct operation of
the test method, exceed the following values in 1 case in 20.
Flash point
Fire point
NOTE 20The precision for asphalt type samples which have utilized
the procedure in Appendix X1 have not been determined.
8C (15F)
8C (15F)
18C (32F)
14C (25F)
14.2 The precision data for fire point is not known to have
been developed in accordance with Precision Manual RR:D021007.6
NOTE 18The precisions for fire point were not determined in the
current interlaboratory program. Fire point is a parameter that is not
commonly specified, although in some cases, this temperature may be
desired.
NOTE 19The precision for asphalt type samples which have had any
formed surface film removed has not been determined.
15. Keywords
15.1 automated Cleveland open cup; Cleveland open cup;
fire point open cup for flash point; flammability; flash point;
petroleum products
6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: D021007.
7
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S15-1009.
ANNEXES
(Mandatory Information)
A1. CLEVELAND OPEN CUP TESTER
A1.5 Temperature Measuring Device SupportAny convenient device that will hold the temperature measuring device
7
D 92 05
in the specified position during a test and that will permit easy
removal of the temperature measuring device from the test cup
upon completion of a test may be used.
Purity (mole %)
99 +
99 +
Limits (C)
68.0
68.0
9
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S151010.
10
MNL7, Manual on Presentation of Data and Control Chart Analysis, 6th ed.,
ASTM International, 1990.
8
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S151008.
APPENDIX
(Nonmandatory Information)
X1. TECHNIQUE TO PREVENT SURFACE SKIN FORMATION WHEN TESTING FLASH POINT OF ASPHALTS BY TEST
METHOD D 92
X1.1 Introduction
X1.1.1 This technique to prevent surface skin formation
when testing flash point of asphalts by Test Method D 92 was
developed by Imran Hussami of Frontier El Dorado Refining
Company.
D 92 05
NOTEUse 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 D 92
X1.3 Procedure
X1.3.1 Determine the center of the filter paper by means of
a ruler. Using the single-hole punch, punch a 6-mm diameter
hole in the center of the 7.5 cm diameter qualitative filter paper.
X1.3.2 Curl up the sides of the filter paper, about 6 mm all
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).
X1.3.3 Place the restraining tension-ring snugly over the
curved portion of the filter paper in the base of the cup. (The
tension-ring prevents the filter paper from moving upward
during the test.)
D 92 05
SUMMARY OF CHANGES
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D 9202b) that may impact the use of this standard.
(3) Revise 11.1.4 and add Note 11.
(4) Revise A1.2.
(1) Deleted Note 3 and replace Note 6 with a generic description of a draft shield.
(2) Revise 11.1.1 and 11.2.2.
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