Flash Point by Tag Closed Cup Tester: Standard Test Method For

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An American National Standard

Designation: D 56 – 05

Standard Test Method for


Flash Point by Tag Closed Cup Tester1
This standard is issued under the fixed designation D 56; 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 (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

INTRODUCTION

To ensure an acceptable precision, this dynamic flash point test method employs a prescribed rate
of temperature rise for the material under test. The rate of heating may not in all cases give the
precision quoted in the test method because of the low thermal conductivity of certain materials. To
improve the prediction of flammability, Test Method D 3941, which utilizes a slower heating rate, was
developed. Test Method D 3941 provides conditions closer to equilibrium where the vapor above the
liquid and the liquid are at about the same temperature. If a specification requires Test Method D 56,
do not change to Test Method D 3941 or other test method without permission from the specifier.
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* point under 37.8°C (100°F) are flammable as determined by this test
method for those liquids that have a viscosity less than 5.5 mm2/s (cSt) at
1.1 This test method covers the determination of the flash 40°C (104°F) or 9.5 mm2/s (cSt) or less at 25°C (77°F), or do not contain
point, by tag manual and automated closed testers, of liquids suspended solids or do not have a tendency to form a surface film while
with a viscosity below 5.5 mm2/s (cSt) at 40°C (104°F), or under test. Other flash point classifications have been established by these
below 9.5 mm2/s (cSt) at 25°C (77°F), and a flash point below departments for liquids using this test method.
93°C (200°F). 1.2 This test method can be used to measure and describe
1.1.1 For the closed-cup flash point of liquids with the the properties of materials, products, or assemblies in response
following properties: a viscosity of 5.5 mm2/s (cSt) or more at to heat and flame under controlled laboratory conditions and
40°C (104°F); a viscosity of 9.5 mm2/s (cSt) or more at 25°C cannot be used to describe or appraise the fire hazard or fire
(77°F); a flash point of 93°C (200°F) or higher; a tendency to risk of materials, products, or assemblies under actual fire
form a surface film under test conditions; or containing conditions. However, results of this test method can be used as
suspended solids, Test Method D 93 can be used. elements of fire risk assessment that takes into account all of
1.1.2 For cut-back asphalts refer to Test Methods D 1310 the factors that are pertinent to an assessment of the fire hazard
and D 3143. of a particular end use.
NOTE 1—The U.S. Department of Transportation (RSTA)2 and U.S. 1.3 Related standards are Test Methods D 93, D 1310,
Department of Labor (OSHA) have established that liquids with a flash D 3828, D 3278, and D 3941.
1.4 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information
1
This test method is under the jurisdiction of ASTM Committee D02 on only.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility. 1.5 This standard does not purport to address all of the
Current edition approved May 1, 2005. Published May 2005. Originally safety concerns, if any, associated with its use. It is the
approved in 1918. Last previous edition approved in 2002 as D 56–02a. responsibility of the user of this standard to establish appro-
2
For information on United States Department of Transportation regulations, see
Codes of United States Regulation 49 CFR Chapter 1 and for information on United
priate safety and health practices and determine the applica-
States Department of Labor regulations, see Code of United States Regulation 29 bility of regulatory limitations prior to use. For specific hazard
CFR Chapter XVII. Each of these items are revised annually and may be procured statements see 8.2, 8.3, 9.5, 12.5, and refer to Material Safety
from the Superintendent of Documents, Government Printing Office, Washington, Data Sheets.
DC 20402.

*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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D 56 – 05
2. Referenced Documents 3.2.1 dynamic (non-equilibrium)—in this type of flash point
2.1 ASTM Standards: 3 apparatus, the condition of the vapor above the specimen and
D 93 Test Methods for Flash Point by Pensky-Martens the specimen are not at the same temperature at the time that
Closed Cup Tester the ignition source is applied.
D 1310 Test Method for Flash Point and Fire Point of 3.2.1.1 Discussion—This is primarily caused by the heating
Liquids by Tag Open-Cup Apparatus of the specimen at the constant prescribed rate with the vapor
D 3143 Test Method for Flash Point of Cutback Asphalt temperature lagging behind the specimen temperature. The
with Tag Open-Cup Apparatus resultant flash point temperature is generally within the repro-
D 3278 Test Methods for Flash Point of Liquids by Small ducibility of the test method.
Scale Closed-Cup Apparatus 3.2.2 equilibrium—in that type of flash point apparatus or
D 3828 Test Methods for Flash Point by Small Scale Closed test method, the vapor above the specimen and the specimen
Cup Tester are at the same temperature at the time the ignition source is
D 3941 Test Method for Flash Point by the Equilibrium applied.
Method with a Closed-Cup Apparatus 3.2.2.1 Discussion—This condition may not be fully
D 4057 Practice for Manual Sampling for Petroleum and achieved in practice, since the temperature is not uniform
Petroleum Products throughout the specimen and the test cover and shutter are
D 6299 Practice for Applying Statistical Quality Assurance generally cooler.
Techniques to Evaluate Analytical Measurement System
Performance 4. Summary of Test Method
D 6300 Practice for Determination of Precision and Bias 4.1 The specimen is placed in the cup of the tester and, with
Data for Use in Test Methods for Petroleum Products and the lid closed, heated at a slow constant rate. An ignition source
Lubricants is directed into the cup at regular intervals. The flash point is
E 1 Specification for ASTM Liquid-in-Glass Thermometers taken as the lowest temperature at which application of the
E 502 Test Method for Selection and Use of ASTM Stan- ignition source causes the vapor above the specimen to ignite.
dards for the Determination of Flash Point of Chemicals by
Closed Cup Methods 5. Significance and Use
2.2 Federal Test Method Standards:4 5.1 Flash point measures the tendency of the specimen to
Method 1101, Federal Test Method Standard No. 791b form a flammable mixture with air under controlled laboratory
Method 4291, Federal Test Method Standard No. 141A conditions. It is only one of a number of properties that shall be
2.3 ISO Standards:5 considered in assessing the overall flammability hazard of a
Guide 34 General Requirements for the Competence of material.
Reference Material Producers 5.2 Flash point is used in shipping and safety regulations to
Guide 35 Certification of Reference Materials—General define flammable and combustible materials. One should
and Statistical Principles consult the particular regulation involved for precise defini-
tions of these classes.
3. Terminology 5.3 Flash point can indicate the possible presence of highly
3.1 Definitions: volatile and flammable materials in a relatively nonvolatile or
3.1.1 flash point—the lowest temperature corrected to a nonflammable material. For example, an abnormally low flash
pressure of 101.3 kPa (760 mm Hg) at which application of an point on a sample of kerosene can indicate gasoline contami-
ignition source causes the vapors of a specimen of the sample nation.
to ignite under specified conditions of test.
3.1.1.1 Discussion—The specimen is deemed to have 6. Apparatus (Manual Instrument)
flashed when a flame appears and instantaneously propagates 6.1 Tag Closed Tester—The apparatus is shown in Fig. 1
itself over the entire surface of the fluid. and described in detail in Annex A1.
3.1.1.2 Discussion—When the ignition source is a test 6.2 Shield—A shield 460 mm (18 in.) square and 610 mm
flame, the application of the test flame may cause a blue halo (24 in.) high, open in front, is recommended.
or an enlarged flame prior to the actual flash point. This is not 6.3 Temperature Measuring Device—A liquid-in-glass ther-
a flash and should be ignored. mometer, as prescribed in Table 1, or an electronic temperature
3.2 Definitions of Terms Specific to This Standard: measuring device such as a resistance device or thermocouple.
The device shall exhibit the same temperature response as the
liquid-in-glass thermometer.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or NOTE 2—Whenever thermometers complying with ASTM require-
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM ments are not available, thermometers complying with the requirements
Standards volume information, refer to the standard’s Document Summary page on for The Institute of Petroleum thermometer IP 15C PM-Low can be used.
the ASTM website.
4
Available from Superintendent of Documents, U.S. Government Printing 7. Sampling
Office, Washington, DC 20402.
5
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 7.1 Erroneously high flash points will be obtained when
4th Floor, New York, NY 10036. precautions are not taken to avoid the loss of volatile material.

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D 56 – 05
8. Preparation of Apparatus (Manual)
8.1 Support the manual apparatus on a level steady surface,
such as a table. Unless tests are made in a draft-free room or
compartment, surround the tester on three sides by the shield
for protection from drafts. Tests are not to be made in a
laboratory draft hood or near ventilators.
8.2 Natural gas and bottled gas flame and electric ignitors
have been found acceptable for use as the ignition source.
(Warning—Gas pressure supplied to the apparatus must not be
allowed to exceed 3 kPa (12 in.) of water pressure.)
8.3 For flash points below 13°C (55°F) or above 60°C
(140°F), use as a bath liquid a 1 + 1 mixture of water and
ethylene glycol (Warning—Ethylene Glycol—Poison. Harm-
ful or fatal if swallowed. Vapor harmful. Avoid contact with
skin.) For flash points between 13°C (55°F) and 60°C (140°F),
either water or a water-glycol mixture can be used as bath
liquid. The temperature of the liquid in the bath shall be at least
10°C (18°F) below the expected flash point at the time of
introduction of the sample into the test cup. Do not cool bath
liquid by direct contact with dry ice (solid carbon dioxide).
NOTE 3—Due to possible difficulty in maintaining the prescribed rate of
temperature rise and due to the formation of ice on the lid, results by this
test method for samples having flash points below 0°C (32°F) may be
unreliable. Trouble due to ice formation on the slide can be minimized by
carefully lubricating the slide shutter with high-vacuum silicone lubricant.
8.4 Verify the performance of the manual apparatus (or in
11.2.3, 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 9.5
shall be corrected for barometric pressure (see Section 13). 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).
FIG. 1 Tag Closed Flash Tester (Manual) 8.5 Once the performance of the apparatus has been veri-
fied, the flash point of secondary working standards (SWSs)
TABLE 1 Thermometers can be determined along with their control limits. These
At 4 to 49°C Above 49°C secondary materials can then be utilized for more frequent
For tests Below 4°C (40°F)
(40 to 120°F) (120°F)
Use ASTM 57C or (57F) 9C or (9F) 9C or (9F)
performance checks (see Annex A2).
ThermometerA 57C or (57F) 8.6 When the flash point obtained is not within the limits
A
Complete specifications for these thermometers are given in Specification E 1. stated in 8.4 or 8.5, check the condition and operation of the
apparatus to ensure conformity with the details listed in Annex
A1, especially with regard to tightness of the lid (see A1.1.3),
Containers should not be opened unnecessarily to prevent loss the action of the shutter, the position of the ignition source (see
of volatile material and possible introduction of moisture. A1.1.3.3), and the angle and position of the temperature
Transfers should not be made unless the sample temperature is measuring device (see A1.1.3.4). After any adjustment, repeat
at least 10°C (18°F) below the expected flash point. When the test in 8.4 using fresh test specimen, with special attention
possible, flash point shall be the first test performed on a to the procedural details prescribed in the test method.
sample and the sample must be stored at low temperature.
7.2 Do not store samples in gas-permeable containers since 9. Procedure (Manual)
volatile materials may diffuse through the walls of the enclo- 9.1 Using a graduated cylinder and taking care to avoid
sure. Samples in leaky containers are suspect and not a source wetting the cup above the final liquid level, measure 50 6 0.5
of valid results. mL of the sample into the cup, both the sample and graduated
7.3 At least 50 mL of sample is required for each test. Refer cylinder being precooled, when necessary, so that the specimen
to sampling information in Practice D 4057. temperature at the time of measurement will be 27 6 5°C (80

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D 56 – 05
6 10°F) or at least 10°C (18°F) below the expected flash point, in significant burning of vapors outside the test cup, and can be
whichever is lower. It is essential that the sample temperature a potential fire hazard. See Appendix X1 and Appendix X2 for
be maintained at least 10°C (18°F) below the expected flash more information.)
point during the transfers from the sample container to the 9.6 Discontinue the test and remove the source of heat. Lift
cylinder and from the cylinder to the test cup. Destroy air the lid and wipe the temperature measuring device bulb.
bubbles on the surface of the specimens by use of knife point Remove the test cup, empty, and wipe dry.
or other suitable device. Wipe the inside of the cover with a 9.7 If, at any time between the first introduction of the
clean cloth or absorbent tissue paper; then attach the cover, ignition source and the observation of the flash point, the rise
with the temperature measuring device in place, to the bath in temperature of the specimen is not within the specified rate,
collar. discontinue the test, discard the result and repeat the test,
adjusting the source of heat to secure the proper rate of
9.2 Light the test flame, when used, adjusting it to the size
temperature rise, or using a modified “expected flash point,” or
of the small bead on the cover. Operate the mechanism on the both, as required.
cover in such a manner as to introduce the ignition source into 9.8 Never make a repeat test on the same specimen of
the vapor space of the cup, and immediately bring it up again. sample; always take fresh specimen of sample for each test.
The time consumed for the full operation should be 1 s,
allowing equal time periods for the introduction and return. 10. Apparatus (Automated Instrument)
Avoid any hesitation in the operation of depressing and raising
10.1 An automated flash point instrument is used that is
the ignition source. When a flash is observed on the initial
capable of performing the test in accordance with Section 9.
operation of the mechanism, discontinue the test and discard
The apparatus can use a gas test flame or electric ignitor. The
the result. In this case, a fresh sample shall be cooled an
dimensions for the test cup and test cover are shown in Fig.
additional 10°C (18°F), below the original specimen installa- A1.1 and Fig. A1.2.
tion temperature. 10.2 Samples with low flash point may require a source of
9.2.1 Exercise care when using a test flame, if the flame is cooling for the heating area.
extinguished it cannot ignite the specimen and the gas entering
the vapor space can influence the result. When the flame is 11. Preparation of Apparatus (Automated Instrument)
prematurely extinguished the test shall be discontinued and any 11.1 Support the automated apparatus on a level, steady
result discarded. surface, such as a table. Unless tests are made in a draft-free
9.3 Flash Points Below 60°C (140°F)—When the flash compartment, it is a good practice, but not required, to
point of the sample is known to be below 60°C (140°F), apply surround the tester with a shield to prevent draft.
and adjust the heat so that the temperature of the portion will 11.2 The user of the automatic instrument must be sure that
rise at a rate of 1°C (2°F)/min 6 6 s. When the temperature of all of the manufacturer’s instructions for calibrating, checking,
the specimen in the test cup is 5°C (10°F) below its expected and operating the equipment are followed.
flash point, apply the ignition source in the manner just 11.2.1 Adjust the detection system per manufacturer’s in-
described in 9.2 and repeat the application of the ignition structions.
source after each 0.5°C (1°F) rise in temperature of the 11.2.2 Calibrate the temperature measuring device per
specimen. manufacturer’s instructions.
9.4 Flash Points at 60°C (140°F) or Above—If the flash 11.2.3 Verify the performance of the automated apparatus at
point of the sample is known to be 60°C (140°F) or higher, least once per year by determining the flash point of a certified
apply and adjust the heat so that the temperature of the reference material (CRM) such as those listed in Annex A2,
specimen will rise at a rate of 3°C (5°F)/min 6 6 s. When the which is reasonably close to the expected temperature range of
temperature of the specimen in the test cup is 5°C (10°F) below the samples to be tested. The material shall be tested according
its expected flash point, apply the ignition source in the manner to the procedure of this test method and the observed flash
just described in 9.2 and repeat the application of the ignition point obtained in 9.5 shall be corrected for barometric pressure
(see Section 13). The flash point obtained shall be within the
source each 1°C (2°F) rise in temperature of the specimen.
limits stated in Table A2.1 for the identified CRM or within the
9.5 When the application of the ignition source causes a limits calculated for an unlisted CRM (see Annex A2).
distinct flash in the interior of the cup, as defined in 3.1.1, 11.2.4 Once the performance of the apparatus has been
observe and record the temperature of the specimen as the flash verified, the flash point of secondary working standards
point. Do not confuse the true flash with the bluish halo that (SWSs) can be determined along with their control limits.
sometimes surrounds the ignition source during applications These secondary materials can then be utilized for more
immediately preceding the actual flash. (Warning—For cer- frequent performance checks (see Annex A2).
tain mixtures containing halogenated hydrocarbons, such as, 11.2.5 When the flash point obtained is not within the limits
methylene chloride or trichloroethylene, no distinct flash, as stated in 11.2.3 or 11.2.4, check the condition and operation of
defined, is observed. Instead a significant enlargement of the the apparatus to ensure conformity with the details listed in
test flame (not halo effect) and change in color of the test flame Annex A1, especially with regard to tightness of the lid (see
from blue to yellowish-orange occurs. Continued heating and A1.1.3), the action of the shutter, the position of the ignition
testing of these samples above ambient temperature can result source (see A1.1.3.3), and the angle and position of the

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D 56 – 05
temperature measuring device (see A1.1.3.4). After any adjust- no distinct flash, as defined, is observed. Instead a significant
ment, repeat the test in 11.2.3 using fresh test specimen, with enlargement of the test flame (not halo effect) and change in
special attention to the procedural details prescribed in the test color of the test flame from blue to yellowish-orange occurs.
method. Continued heating and testing of these samples above ambient
temperature can result in significant burning of vapors outside
12. Procedure (Automated)
the test cup, and can be a potential fire hazard. See Appendix
12.1 Adjust the external cooling system, if required, to a X1 and Appendix X2 for more information.)
temperature necessary to cool the heating area 10°C below the 12.6 When the apparatus has cooled down to a safe handling
expected flash point. temperature (less than 55°C (130°F)) remove the cover and the
12.2 Place the test cup in position in the instrument. test cup and clean the apparatus as recommended by the
12.3 Enter the Expected Flash Point; this will allow the manufacturer.
heating area to be cooled to the required minimum starting
temperature. 13. Report
NOTE 4—To avoid an abnormal heating rate when the specimen is at a 13.1 Correction for barometric pressure. Observe and
low temperature, it is recommended to precool the test cup and cover. This record the ambient barometric pressure at the time and place of
may be accomplished by placing the assembly into position in the the test. When the pressure differs from 101.3 kPa (760 mm
instrument while it is cooling to 10°C (18°F) below the programmed Hg), correct the flash point as follows:
Expected Flash Point.
NOTE 5—Flash Point results determined in an “unknown Expected Corrected flash point 5 C 1 0.25 ~101.3 2 p! (1)
Flash Point mode” should be considered approximate. This value can be Corrected flash point 5 F 1 0.06 ~760 2 P! (2)
used as the Expected Flash Point when a fresh specimen is tested in the
standard mode of operation. Corrected flash point 5 C 1 0.033 ~760 2 P! (3)

12.4 Using a graduated cylinder and taking care to avoid where:


wetting the cup above the final liquid level, measure 50 6 0.5 C = observed flash point, °C,
mL of the sample into the cup, both the sample and the F = observed flash point, °F,
graduated cylinder being precooled, when necessary, so that p = ambient barometric pressure, kPa, and
the specimen temperature at the time of the measurement is 27 P = ambient barometric pressure, mm Hg.
6 5°C (80 6 10°F) or at least 10°C (18°F) below the expected 13.2 The barometric pressure used in this calculation shall
flash point, whichever is lower. It is essential that the sample be the ambient pressure for the laboratory at the time of test.
temperature be maintained at least 10°C (18°F) below the Many aneroid barometers, such as those used at weather
expected flash point during the transfers from the sample stations and airports, are precorrected to give sea level read-
container to the cylinder and from the cylinder to the test cup. ings; these shall not be used.
Destroy air bubbles on the surface of the specimen by use of 13.3 Report the corrected flash point to the nearest 0.5°C (or
knife point or other suitable device. Wipe the inside of the 1°F).
cover with a clean cloth or absorbent tissue paper; then attach
the cover, with the temperature measuring device in place, to 14. Precision and Bias
the bath collar. Connect the shutter and ignition source activa- 14.1 Precision—The following criteria shall be used for
tor, if so equipped, into the lid housing. When using a gas test judging the acceptability of results (95 % probability):
flame, light the pilot flame and adjust the test flame to 4 mm 14.1.1 Repeatability—The difference between successive
(5⁄32 in.) in diameter. If the instrument is equipped with an test results, obtained by the same operator with the same
electrical ignition device, adjust according to the manufactur- apparatus under constant operating conditions on identical test
er’s instructions. Test the ignition source dipping action, if so material, would in the long run, in the normal and correct
equipped, and observe if the apparatus functions correctly. operation of the test method, exceed the following values only
Press the start key. If a flash is observed upon initial operation, in one case in twenty:
discontinue the test and discard the result. In this case a fresh Flash Point, °C (°F) Repeatability, °C (°F)
specimen shall be cooled to an additional 10°C (18°F) below
Below 60°C (140°F) 1.2°C (2.0°F)
the original specimen installation temperature. At and Above 60°C (140°F) 1.6°C (3.0°F)
NOTE 6—Care should be taken when cleaning and positioning the lid 14.1.2 Reproducibility—The difference between two single
assembly so as not to damage or dislocate the flash detection system or and independent results, obtained by different operators work-
temperature measuring device. See manufacturer’s instructions for proper
care and maintenance.
ing in different laboratories on identical test material, would in
the long run, in the normal and correct operation of the test
12.5 The apparatus shall automatically control the test method, exceed the following values only in one case in
procedure as described in this test method. When the flash twenty:
point is detected, the apparatus will record the temperature and Flash Point, °C (°F) Reproducibility, °C (°F)
automatically discontinue the test. If a flash is detected on the
first application, the test should be discontinued, the result shall Below 60°C (140°F) 4.3°C (8°F)
At and Above 60°C (140°F) 5.8°C (10°F)
be discarded and the test repeated with a fresh specimen.
(Warning—For certain mixtures containing halogenated hy- 14.2 Bias—The procedure in Test Method D 56 for measur-
drocarbons, such as, methylene chloride or trichloroethylene, ing flash point has no bias since the tag flash point can be

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D 56 – 05
defined only in terms of this test method. The current inter- NOTE 8—The precision data were developed in a 1991 cooperative test
laboratory tests confirm that there is no relative bias between program6 using eight (8) samples. Twelve (12) laboratories participated
manual and automated procedures. In any case of dispute the with the manual apparatus and seventeen (17) laboratories participated
with the automatic equipment. Information on the type of samples and
flash point as determined by the manual procedure shall be their average flashpoints are in the research report.
considered the referee test.
NOTE 7—Mixtures such as, but not limited to, those that are chlorinated
15. Keywords
or include water may cause significant differences in the results obtained 15.1 combustible; fire risk; flammable; flash point; tag
by manual and automatic instruments. For these mixtures, the precision closed cup
statement may not apply.

6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR: S15–1007.

ANNEXES

(Mandatory Information)

A1. APPARATUS

A1.1 Tag Closed Tester device shall be designed and constructed so that opening the
A1.1.1 The Tag Closed Tester shall consist of the test cup, shutter depresses the tip to a point approximately 2 mm (0.08
lid with ignition source, and liquid bath conforming to the in.) to the right of the horizontal center of the middle opening
following requirements: of the lid (refer to lower part of Fig. A1.3). This will bring the
A1.1.2 Test Cup, of brass or other nonrusting metal of ignition source to the approximate center of the opening. The
equivalent heat conductivity, conforming to dimensional re- plane of the underside of the lid shall be between the top and
quirements prescribed in Fig. A1.1. bottom of the tip of the ignition source when the latter is fully
A1.1.3 Lid: depressed.
A1.1.3.1 The lid comprises a circle of nonrusting metal with A1.1.3.4 The collar for the cup-temperature measuring de-
a rim projecting downward about 15.9 mm (5⁄8 in.), a slide vice ferrule shall be set at an angle that permits placement of
shutter, a device which simultaneously opens the shutter and the temperature measuring device with its bulb approximately
depresses the ignition source, and a slanting collar in which the in the horizontal center of the cup, at a depth prescribed in
cup-temperature measuring device ferrule is inserted. Fig. A1.2 Table A1.1.
gives a diagram of the upper surface of the lid, showing A1.1.4 Liquid Bath, conforming to the limiting or minimum
dimensions and positions of the three holes opened and closed dimension shown in Fig. A1.3. It shall be of brass, copper, or
by the shutter, and the size and position of the opening for the
other noncorroding metal of substantial construction. Sheet
cup temperature measuring device.
metal of about No. 20 B&S gage (0.812 mm) is satisfactory. It
A1.1.3.2 The rim shall fit the collar of the liquid bath with
may, if desired, be lagged with heat-insulating material to
a clearance not exceeding 0.4 mm (0.002 in.) and shall be
facilitate control of temperature.
slotted in such a manner as to press the lid firmly down on the
top of the cup when the latter is in place in the bath. When this A1.1.5 Heater, of any type (electric, gas, alcohol, and so
requirement is not met, the vertical position of the cup in the forth) capable of controlling temperature as required in Section
bath shall be suitably adjusted, as by placing a thin ring of 9. An external electric heater, controlled by a variable voltage
metal under the flange of the cup. transformer, is recommended.
A1.1.3.3 The shutter shall be of such size and shape that it A1.1.6 Bath Stand—For electric heating, any type of stand
covers the three openings in the lid when in the closed position may be used. For alcohol lamp or gas burner, a stand, as
and uncovers them completely when in the open position. The illustrated in Fig. 1, to protect the ignition source from air
nozzle of the flame-exposure device, when used, shall conform currents (unless tests can be made in a draft-free room) is
to the dimensions given in Table A1.1. The ignition source required.

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FIG. A1.1 Specimen Cup

Inch-Pound Equivalents
mm in. mm in.
0.03 0.001 10.32 0.406
0.13 0.005 11.92 0.469
4.78 0.188 15.10 0.594
7.15 0.281 18.0 0.71
9.84 0.387 20.6 0.81

NOTE—Dimensions relating to the size and position of the temperature


measuring device collar are recommended but not mandatory.
FIG. A1.2 Top of Lid Showing Position and Dimensions of
Openings

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Inch-Pound Equivalents

mm in.
6.4 0.25
82.6 3.25
95.3 3.75
FIG. A1.3 Section of Liquid Bath and Test Cup (Manual
Apparatus)

TABLE A1.1 Dimensional Requirements


Depth of bath liquid surface below top of test cup 27.8 6 0.4 mm (1.094 6 0.016 in.)
Depth of sample surface below top of test cup 29.4 6 0.8 mm (1.156 6 0.031 in.)
Depth of bottom of bulb of test temperature measuring device below top of cup when in place 45.0 6 0.8 mm (1.77 6 0.031 in.)
Inside diameter of specimen cup 54.0 6 0.3 mm (2.125 6 0.010 in.)
Diameter of bead on top of cover 4.0 6 0.8 mm (0.156 6 0.031 in.)
Diameter of opening in tip of test flame nozzle 1.2 6 0.3 mm (0.0496 0.010 in.)
Outside diameter of tip of test flame nozzle 2.0 mm max (0.079 in. max)

A2. VERIFICATION OF APPARATUS PERFORMANCE

A2.1 Certified Reference Material (CRM)—CRM is a A2.1.1 Typical values of the flash point corrected for
stable, pure (99 + mol % purity) hydrocarbon or other stable barometric pressure for some reference materials and their
petroleum product with a method-specific flash point estab- typical limits are given in Table A2.1 (see Note A2.2).
lished by a method-specific interlaboratory study following Suppliers of CRM’s will provide certificates stating the
Practice D 6300 (formerly known as ASTM RR:D02-1007 method-specific flash point for each material of the current
guidelines) or ISO Guide 34 and 35. production batch. Calculation of the limits for these other

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TABLE A2.1 D 56 Typical Flash Point Values and Typical Limits NOTE A2.2—Materials, purities, flash point values and limits stated in
for CRM Table A2.1 were developed in an ASTM interlaboratory program (see
Hydrocarbon Purity Flash Limits RR:S15-10107) to determine suitability of use for verification fluids in
(mole %) Point(°C) (°C) flash point test methods. Other materials, purities, flash point values and
n–decane 99+ 50.9 62.3 limits can be suitable when produced according to the practices of Practice
n–undecane 99+ 67.1 62.3 D 6300 (formerly known as ASTM RR:D02-1007 guidelines) or ISO
Guides 34 and 35. Certificates of performance of such materials should be
consulted before use, as the flash point value will vary dependent on the
composition of each CRM batch.
CRM’s can be determined from the reproducibility value of NOTE A2.3—p-Xylene obtained from any reputable chemical supplier
this test method, reduced by interlaboratory effect and then may be used as calibrating fluid as long as it meets the specifications
multiplied by 0.7 (see Research Report RR:S15–10076). detailed in A2.1.1.

NOTE A2.1—Supporting data for the interlaboratory study to generate A2.2 Secondary Working Standard (SWS)—SWS is a
the flash point in Table A2.1 can be found in research report RR:S15- stable, pure (99 + mol % purity) hydrocarbon, or other petro-
1010.7 leum product with composition known to remain appreciably
stable.
A2.2.1 Establish the mean flash point and the statistical
7
Supporting data have been filed at ASTM International Headquarters and may control limits (3s) for the SWS using standard statistical
be obtained by requesting Research Report RR: S15-1010. techniques. See Practice D 6299.

A3. MANUFACTURING STANDARDIZATION

A3.1 The cup temperature measuring device, which con- of considerable unnecessary trouble to manufacturers and
forms also to the specifications for the low-range temperature suppliers of instruments as well as to users.
measuring device used in the Pensky-Martens flash tester, Test
Method D 93, is frequently supplied by the temperature mea- A3.2 Subcommittee E01.21 on Reference Material Plan-
suring device manufacturer with a metal or polytetrafluoroet- ning, Proficiency Testing, and Laboratory Accreditation, has
hylene ferrule intended to fit the collar on the lid of the flash studied this problem and has established some dimensional
tester. This ferrule is frequently supplemented by an adapter requirements which are shown, suitably identified, in Fig.
that is used in the larger-diameter collar of the Pensky-Martens A1.1, Fig. A3.1, and Fig. A3.2. Conformity to these require-
apparatus. Differences in dimensions of these collars, which ments is not mandatory but is desirable to users as well as
are immaterial in their effect on the result of tests, are a source suppliers of tag closed testers.

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Inch-Pound Equivalents

mm in. mm in.
0.05 0.002 8.6 0.34
5.3 0.21 9.8 0.385
7.1 0.28 17.3 0.68
FIG. A3.1 Dimensions for Temperature Measuring Device Ferrule
(Not Mandatory)

Inch-Pound Equivalents

mm in.
1.5 0.06
7.23 0.284
8.40 0.330
FIG. A3.2 Dimensions for Temperature Measuring Device Packing
Ring (Not Mandatory)

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APPENDIXES

(Nonmandatory Information)

X1. FLASH POINT MASKING PHENOMENON

X1.1 A condition during flash point testing can occur with flame and a change in the color of the test flame from blue to
certain mixtures whereby the nonflammable component of the yellow-orange laminar flame is observed.
sample tends to inert the vapor space above the liquid, thus
preventing a flash. Under this condition, the flash point of the X1.4 Under this condition, continued heating and testing
material is masked resulting in the reporting of incorrect high for flash point at temperatures above ambient temperature,
flash point or no flash point. have resulted in significant burning of the ignitable vapor
outside the test cup, often above the test flame. This can be a
X1.2 This flash point masking phenomenon most fre- potential fire hazard if not recognized.
quently occurs with ignitable liquids that contain certain X1.5 It is recommended that if this condition is encoun-
halogenated hydrocarbons such as dichloromethane (methyl- tered during the flash point testing of these type of materials,
ene chloride) and trichloroethylene. testing should be discontinued.
X1.3 Under this condition, no distinct flash as defined in X1.6 Further commentaries regarding flash point test and
3.1.1 is observed. Instead a significant enlargement of the test flammability of mixtures can be found in Test Method E 502.

X2. FLASH POINT TEST AND FLAMMABILITY OF MIXTURES

X2.1 While the flash point can be used to indicate the components, there are cases where this liquid can evolve
flammability of liquid materials for certain end uses, flash point flammable vapors under certain conditions and yet will not
does not represent the minimum temperature at which a exhibit a close-cup flash point. This phenomenon is noted
material can evolve flammable vapors. when a nonflammable component is sufficiently volatile and
present in sufficient quantity to inert the vapor space of the
X2.2 There are instances with pure materials where the closed cup, thus preventing a flash. In addition, there are
absence of a flash point does not ensure freedom from certain instances where an appreciable quantity of the nonflam-
flammability. Included in this category are materials that mable component will be present in the vapor, and the material
require large diameters for flash propagation, such as trichlo- will exhibit no flash point.
roethylene. This material will not propagate a flame in appa-
ratus the size of a flash point tester, however, its vapors are X2.4 Liquids containing a highly volatile nonflammable
flammable and will burn when ignited in apparatus of adequate component or impurity, which exhibit no flash point because of
size. the influence of the nonflammable material, may form flam-
mable mixtures if totally flash vaporized in air in the proper
X2.3 When a liquid contains flammable and nonflammable proportions.

SUMMARY OF CHANGES

Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D 56–02a) that may impact the use of this standard.

(1) Changed “thermometer” to “temperature measuring de- (2) Deleted test cup weight in A1.1.2.
vice” in 6.3, 9.1, 9.6, A1.1.3.1, A1.1.3.4, A3.1, Table A1.1, Fig. (3) Deleted reference to MNL7 in A2.2.1.
A1.2, Fig. A3.1, and Fig. A3.2. (4) Deleted Note A2.4.

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