Astm D93 - 19
Astm D93 - 19
Astm D93 - 19
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D93 − 19
Designation: 34/99
INTRODUCTION
This flash point test method is a dynamic test method which depends on specified rates of heating
to be able to meet the precision of the test method. The rate of heating may not in all cases give the
precision quoted in the test method because of the low thermal conductivity of some materials. There
are flash point test methods with slower heating rates available, such as Test Method D3941 (for
paints, resins, and related products, and high viscosity products in the range of 0 °C to 110 °C), where
the test conditions are closer to equilibrium.
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.
3.1 Definitions: 5.3 These test methods should be used to measure and
3.1.1 biodiesel, n—a fuel comprised of mono-alkyl esters of describe the properties of materials, products, or assemblies in
long chain fatty acids derived from vegetable oils or animal response to heat and an ignition source under controlled
fats, designated B100. laboratory conditions and should not be used to describe or
appraise the fire hazard or fire risk of materials, products, or
3.1.2 biodiesel blends, n—a blend of biodiesel fuel with
assemblies under actual fire conditions. However, results of
petroleum-based diesel fuel.
these test methods may be used as elements of a fire risk
3.1.3 dynamic, adj—in petroleum products—in petroleum assessment which takes into account all of the factors which
product flash point test methods—the condition where the are pertinent to an assessment of the fire hazard of a particular
vapor above the test specimen and the test specimen are not in end use.
temperature equilibrium at the time that the ignition source is
applied. 5.4 These test methods provide the only closed cup flash
3.1.3.1 Discussion—This is primarily caused by the heating point test procedures for temperatures up to 370 °C (698 °F).
of the test specimen at the constant prescribed rate with the
vapor temperature lagging behind the test specimen tempera- 6. Apparatus
ture. 6.1 Pensky-Martens Closed Cup Apparatus (manual)
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—This apparatus consists of the test cup, test cover and shutter,
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or stirring device, heating source, ignition source device, air bath,
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM and top plate described in detail in Annex A1. The assembled
Standards volume information, refer to the standard’s Document Summary page on
manual apparatus, test cup, test cup cover, and test cup
the ASTM website.
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., assembly are illustrated in Figs. A1.1-A1.4, respectively. Di-
4th Floor, New York, NY 10036, http://www.ansi.org. mensions are listed respectively.
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Procedure C 13.8 Record as the flash point the reading on the tempera-
ture measuring device at the time the ignition source applica-
13. Procedure tion causes a distinct flash in the interior of the test cup which
13.1 Automated Apparatus—Ensure that the apparatus is is detected by the electronic device.
equipped with an electronic measuring system for the detection 13.9 The application of the test flame can cause a blue halo
of the flash point. or an enlarged flame prior to the actual flash point. This is not
13.2 Ensure that the sample container is filled to the volume a flash and shall be ignored.
capacity requirement specified in 8.2. Fill the test cup with the 13.10 When a flash point is detected on the first application,
test specimen to the filling mark inside of the test cup. The the test shall be discontinued, the result discarded, and the test
temperature of the test cup and test specimen shall be at least repeated with a fresh test specimen. The first application of the
24 °C below the expected flash point. If too much test ignition source with the fresh test specimen shall be approxi-
specimen has been added to the test cup, remove the excess mately 24 °C below the temperature at which a flash point was
using a syringe or similar device for withdrawal of fluid. Place detected on the first application.
ANNEXES
(Mandatory Information)
A1.1 A typical assembly of the apparatus, gas heated, is both, engaging with a corresponding device on the cup. The
shown in Fig. A1.1. The apparatus shall consist of a test cup, upper edge of the cup shall be in close contact with the inner
cover, and stove conforming to the following requirements: face of the cover throughout its circumference.
A1.1.1 Cup—The cup shall be of brass, or other nonrusting A1.1.2.2 Shutter—The cover shall be equipped with a brass
metal of equivalent heat conductivity, and shall conform to the shutter (Fig. A1.1 and Fig. A1.4), approximately 2.4 mm
dimensional requirements in Fig. A1.2. The flange shall be (3⁄32 in.) thick, operating on the plane of the upper surface of
equipped with devices for locating the position of the cup in the the cover. The shutter shall be so shaped and mounted that it
stove. A handle attached to the flange of the cup is a desirable rotates on the axis of the horizontal center of the cover between
accessory. The handle shall not be so heavy as to tip over the two stops, so placed, that when in one extreme position, the
empty cup. openings A, B, and C in the cover are completely closed, and
A1.1.2 Cover: when in the other extreme position, these openings are com-
A1.1.2.1 Cover Proper—The cover shown in Fig. A1.3 shall pletely opened. The mechanism operating the shutter should be
be of brass (A1.1.1) and shall have a rim projecting downward of the spring type and constructed so that when at rest the
almost to the flange of the cup. The rim shall fit the outside of shutter shall exactly close the three openings. When operated
the cup with a clearance not exceeding 0.36 mm (0.014 in.) on to the other extreme, the three cover openings shall be exactly
the diameter. There shall be a locating or locking device, or open and the tip of the exposure tube shall be fully depressed.
A1.1.2.3 Flame-Ignition Device—The flame-ignition device through the center of the larger opening A (Fig. A1.3). An
(Fig. A1.4) shall have a tip with an opening 0.69 mm to electric ignitor is also suitable. The electric ignitors shall be of
0.79 mm (0.027 in. to 0.031 in.) in diameter. This tip shall be the electric resistance (hot-wire) type and shall position the
made preferably of stainless steel, although it may be fabri- heated section of the ignitor in the aperture of the test cover in
cated of other suitable metals. The flame-exposure device shall the same manner as the gas flame device.
be equipped with an operating mechanism which, when the A1.1.2.4 Pilot Flame—A pilot flame shall be provided for
shutter is in the open position, depresses the tip so that the automatic relighting of the exposure flame. A bead 4 mm
center of the orifice is between the planes of the under and (5⁄32 n.) in diameter can be mounted on the cover so that the
upper surfaces of the cover proper at a point on a radius passing size of the test flame can be regulated by comparison. The tip
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mm (in.)
min max (min) (max)
D 12.7 13.5 (0.50) (0.53)
E 4.8 5.6 (0.19) (0.22)
mm (in.) F 13.5 14.3 (0.53) (0.56)
min max (min) (max) G 23.8 24.6 (0.94) (0.97)
H 1.2 2.0 (0.05) (0.08)
A 79.0 79.8 (3.11) (3.14) I 7.9 ... (0.31) (...)
B 1.0 ... (0.04) (...) J 12.00 12.32 (0.472) (0.485)
C 2.8 3.6 (0.11) (0.14) K 16.38 17.00 (0.645) (0.669)
D 21.72 21.84 (0.855) (0.860) L 18.65 19.45 (0.734) (0.766)
E 45.47 45.72 (1.790) (1.800)
F 50.72 50.85 (1.997) (2.002)
FIG. A1.3 Cover Proper
G 55.75 56.00 (2.195) (2.205)
H 3.8 4.0 (0.15) (0.16)
I 53.90 54.02 (2.122) (2.127)
J 2.29 2.54 (0.090) (0.100) The stove shall consist of an air bath and a top plate on which
the flange of the cup rests.
FIG. A1.2 Test Cup
A1.1.2.7 Air Bath—The air bath shall have a cylindrical
interior and shall conform to the dimensional requirements in
of the pilot flame shall have an opening the same size as the tip Fig. A1.1. The air bath may be either a flame or electrically
of the flame exposure device (0.69 mm to 0.79 mm (0.027 in. heated metal casting (A1.1.2.8), or an electric-resistance ele-
to 0.031 in.) in diameter). ment (A1.1.2.9). In either case, the air bath must be suitable for
A1.1.2.5 Stirring Device—The cover shall be equipped with use at the temperatures to which it will be subjected without
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a stirring device (Fig. A1.4) mounted in the center of the cover deformation.
and carrying two 2-bladed metal propellers. In Fig. A1.4 lower A1.1.2.8 Heater, Flame or Electric—If the heating element
propeller is designated by the letters L, M, and N. This is a flame or an electric heater, it shall be so designed and used
propeller shall measure approximately 38 mm from tip to tip, that the temperatures of the bottom and the walls are approxi-
with each of its two blades 8 mm in width with a pitch of 45°. mately the same. In order that the air bath internal surfaces
The upper propeller is designated by the letters A, C, and G. should be at a uniform temperature, it should not be less than
This propeller measures approximately 19 mm, tip to tip, each 6.4 mm (1⁄4 in.) in thickness unless the heating element is
of its two blades is also 8 mm in width with a pitch of 45°. Both designed to give equal heat flux densities over all the wall and
propellers are located on the stirrer shaft in such a manner that, bottom surfaces.
when viewed from the bottom of the stirrer, the blades of one A1.1.2.9 Heater, Electric Resistance—If the heater is of the
propeller are at 0° and 180° while the blades of the other electric resistance type, it shall be constructed so that all parts
propeller are at 90° and 270°. A stirrer shaft may be coupled to of the interior surface are heated uniformly. The wall and
the motor by a flexible shaft or a suitable arrangement of bottom of the air bath shall not be less than 6.4 mm (1⁄4 in.) in
pulleys. thickness unless the resistance heating elements are distributed
A1.1.2.6 Stove—Heat shall be supplied to the cup by means over at least 80 % of the wall and all the bottom of the air bath.
of a properly designed stove which is equivalent to an air bath. A heater having such a distribution shall have the heating
mm (in.)
min max (min) (max)
A 18.3 19.8 (0.72) (0.78)
B 2.38 3.18 (0.094) (0.125)
C 7.6 8.4 (0.30) (0.33)
D 2.0 2.8 (0.08) (0.11)
E 0.69 0.79 (0.027) (0.031)
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A2.1 The low-range thermometer, which conforms also to A2.2 Dimensional requirements are shown in Fig. A2.1.
the specification for the cup thermometer in the tag closed Conformity to these requirements is not mandatory, but is
tester (Test Method D56) and which frequently is fitted with a desirable to users as well as suppliers of Pensky-Martens
metal ferrule intended to fit the collar on the cover of the tag testers.
flash tester, can be supplemented by an adapter (Fig. A2.1) to
be used in the larger diameter collar of the Pensky-Martens
apparatus. Differences in dimensions of these collars, which do
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not affect test results, are a source of unnecessary trouble to
manufacturers and suppliers of instruments, as well as to users.
mm (in.)
min max (min) (max)
A 6.20 6.50 (0.244) (0.256)
B 17.0 18.0 (0.67) (0.71)
C 9.80 9.85 (0.386) (0.388)
D 11.92 12.24 (0.469) (0.482)
E 1.40 1.65 (0.055) (0.065)
F 8.56 8.61 (0.337) (0.339)
G 12.4 13.0 (0.49) (0.57)
H 8.56 8.61 (0.337) (0.339)
I 8.1 8.6 (0.32) (0.34)
J 9.9 10.7 (0.39) (0.42)
K 8.64 8.69 (0.340) (0.342)
L 5.1 5.6 (0.20) (0.22)
M 17.0 17.5 (0.67) (0.69)
N 27.4 28.2 (1.08) (1.11)
O 7.11 7.16 (0.280) (0.282)
P 9.73 9.78 (0.383) (0.385)
FIG. A2.1 Dimensions for Thermometer Adapter, Ferrule, and Packing Ring
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NOTE 1—The stem shall be made with an enlargement having a diameter of 1.5 mm to 2.0 mm greater than the stem and a length of 3 mm to 5 mm,
the bottom of the enlargement being 64 mm to 66 mm from the bottom of the bulb. These dimensions shall be measured with the test gage shown in Fig.
A3.1.
IP 15C IP 16C IP 101C
Name
Pensky-Martens Low Pensky-Martens High Pensky-Martens Medium
Range −5 °C to + 110 °C 90 °C to 370 °C 20 °C to 150 °C
Graduation 0.5 °C 2 °C 1 °C
Immersion, mm 57 57 57
Overall length ±5 mm 290 280 ± 10 290
Stem diameter, mm 6.0 to 7.0 6.0 to 7.0 6.0 to 7.0
Bulb shape cylindrical cylindrical cylindrical
Bulb length, mm 9 to 13 7 to 10 9 to 13
Bulb diameter, mm not less than 5.5 and not less than 4.5 and not less than 5.5 and
not greater than not greater than not greater than
stem stem stem
Length of graduated portion, 140 to 175 143 to 180 140 to 175
mm
Distance bottom of bulb to, 0 °C 90 °C 20 °C
mm 85 to 95 80 to 90 85 to 95
Longer lines at each 1 °C and 5 °C 10 °C and 20 °C 5 °C
Figured at each 5 °C 20 °C 5 °C
Expansion chamber required required required
Top finish ring ring ring
Scale error not to exceed ± 0.5 °C 1 °C to 260 °C 1 °C
2 °C above 260 °C
See notes 1 and Table A3.2 for 1 and Table A3.2 for 1 and Table A3.2 for
emergent stem emergent stem emergent stem
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sion Ice Point Contraction
Graduations Bulb Scale Location Stem Enlargement
Cham- Scale Chamber
ber
ASTM
For Im- Scale Special Total Bot- Bot- Bot-
Number Stem Dis-
Range Test mer- Error, Inscrip- Length tom tom tom Dis- Dis-
and Long Num- OD tance
at sion max tion Permit ±5 of of of tance tance
Name Sub- Lines ber Dis- to
Heat- Length OD Bulb Distance Bulb Range Bulb to OD Length to
divisions at at tance Bot-
ing to to to to Top, Bot-
Each Each tom,
Line Line Ice max tom
min
at at Point
B C D E F G H I J K L M
9C-62 –5 °C to 57 0.5 °C 1 °C 5 °C 0.5 °C ASTM 160 °C 287 6.0 9.0 not 0 °C 85 100 °C 221 7.5 2.5 64
15
greater
than
Pensky- +110 °C 9C or to to stem to to to to to
9F
D93 − 19
A
Martens 57 mm 7.0 13 98 237 8.5 5.0 66
Low- IMM 32 °F 212 °F
Range
Tag (20 °F to 1 °F 5 °F 10 °F 1 °F 320 °F
Closed
Tester 230°F)
B C
10C-62 90 °C to 57 2 °C 10 °C 20 °C ASTM 287 6.0 8.0 4.5 110 °C 86 360 °C 227 7.5 2.5 64
Pensky- 370°C 10C or to to to to to to to to
Martens, 10F 7.0 10.0 6.0 99 245 8.5 5.0A 66
D
A
The length of the enlargement, and the distance from the bottom of the enlargement to the bottom of the bulb shall be measured with the test gage shown in Fig. A3.1.
B
Scale error: 1 °C up to 260 °C; 2 °C over 260 °C.
C
An expansion chamber is provided for relief of gas pressure to avoid distortion of the bulb at higher temperatures. It is not for the purpose of joining mercury separations; and under no circumstances should the
thermometer be heated above the highest temperature reading.
D
Scale error: 2.5 °F up to 500 °F; 3.5 °F over 500 °F.
D93 − 19
TABLE A3.3 Standardization Temperatures
NOTE 1—The emergent column temperatures are those attained when using the thermometers in the test equipment for which the thermometers were
originally designed. In some cases these temperatures are markedly different from those realized during standardization.
Average Average Average Average
Tempera- Tempera- Tempera- Tempera-
Tempera- Tempera- Tempera- Tempera-
ture of ture of ture of ture of
ture ture ture ture
Emergent Emergent Emergent Emergent
Column Column Column Column
Thermometer 9C Thermometer 9F Thermometer 10C Thermometer 10F
(−5 °C to + 100 °C) (20 °F to 230 °F) (90 °C to 370 °C) (200 °F to 700 °F)
0 °C 19 °C 32 °F 66 °F 100 °C 61 °C 212 °F 141 °F
35 °C 28 °C 100 °F 86 °F 200 °C 71 °C 390 °F 159 °F
70 °C 40 °C 160 °F 106 °F 300 °C 87 °C 570 °F 180 °F
105 °C 50 °C 220 °F 123 °F 370 °C 104 °C 700 °F 220 °F
IP 15C (−7 °C to 110 °C) IP 15F (20 °F to 230 °F) IP 16C (90 °C to 370 °C) IP 16F (20 °F to 700 °F)
0 °C 19 °C 32 °F 66 °F 100 °C 61 °C 200 °F 140 °F
20 °C 20 °C 70 °F 70 °F 150 °C 65 °C 300 °F 149 °F
40 °C 31 °C 100 °F 86 °F 200 °C 71 °C 400 °F 160 °F
70 °C 40 °C 150 °F 104 °F 250 °C 78 °C 500 °F 175 °F
100 °C 48 °C 212 °F 118 °F 300 °C 87 °C 600 °F 195 °F
350 °C 99 °C 700 °F 220 °F
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Reference Fig. No. 5
Range 10 °C–200 °C 50 °F–392 °F
For test at
A Immersion, mm 57
Graduations:
Subdivisions 1 °C 2 °F
Long lines at each 5 °C 10 °F
Numbers at each 10 °C 20 °F
Scale error, max 1 °C 2 °F
Special inscription ASTM
88F (88C)
57 mm IMM
Expansion chamber:
Permit heating to 250 °C 490 °F
B Total length, mm 282 to 292
C Stem OD, mm 6.0 to 7.0
D Bulb length, mm 9
E Bulb OD, mm >stem
Scale location:
Bottom of bulb to line at 10 °C 50 °F
F Distance, mm 75 to 90
G Length of graduated portion, mm 143 to 177
Ice-point scale:
Range
H Bottom of bulb to ice-point, mm
Contraction chamber:
I Distance to bottom, min, mm
J Distance to top, max, mm
Stem enlargement:
K OD, mm 7.5 to 8.5
L Length, mm 2.5 to 5.0A
M Distance to bottom, mm 64 to 66
A
Bulb OD shall be greater than 4.5 mm and less than the outside diameter of the stem (C).
A4.1 Certified Reference Material (CRM)—CRM is a TABLE A4.1 D93 Typical Flash Point Values and Typical Limits
stable, pure (99 + mole % purity) hydrocarbon or other stable for CRM
petroleum product with a method-specific flash point estab- NOTE 1—Supporting data for the interlaboratory study to generate the
lished by a method-specific interlaboratory study following flash point in Table A4.1 can be found in research report RR:S15-1010.8
ASTM RR:D02-1007 guidelines or ISO Guide 34 and 35. Tolerance Limits
Hydrocarbon Purity, mole % Flash Point,°C (0.7R),
A4.1.1 Values of the flash point corrected for barometric °C
pressure for some reference materials and their typical limits n–decane 99 + 52.8 2.6
are given in Table A4.18 (see Note A4.1). Suppliers of CRMs n–undecane 99 + 68.7 3.4
n–tetradecane 99 + 109.3 5.4
will provide certificates stating the method-specific flash point n–hexadecane 99 + 133.9 6.7
for each material of the current production batch. Calculation
of the limits for these other CRMs can be determined from the
reproducibility value of these test methods multiplied by 0.7. materials should be consulted before use, as the flashpoint value will vary
This value provides a nominal coverage of at least 90 % with dependent on the composition of each CRM batch.
95 % confidence. A4.2 Secondary Working Standard (SWS)—SWS is a
NOTE A4.1—Materials, purities, flash point values, and limits stated in stable, pure (99 + mole % purity) hydrocarbon, or other petro-
Table A4.1 were developed in an ASTM interlaboratory program to leum product whose composition is known to remain appre-
determine suitability of use for verification fluids in flash point test ciably stable.
methods. Other materials, purities, flash point values, and limits can be
suitable when produced according to the practices of ASTM RR:D02- A4.2.1 Establish the mean flash point and the statistical
1007 or ISO Guides 34 and 35. Certificates of performance of such control limits (3σ) for the SWS using standard statistical
techniques. (See ASTM MNL 7).9
8
Supporting data have been filed at ASTM International Headquarters and may
9
be obtained by requesting Research Report RR:S15-1010. Contact ASTM Customer Manual on Presentation of Data and Control Chart Analysis, ASTM MNL, 6th
Service at [email protected]. ed., ASTM International, W. Conshohocken, 1990.
APPENDIXES
(Nonmandatory Information)
X1.1 A condition during flash point testing can occur with test flame from blue to yellow-orange laminar flame is ob-
certain mixtures whereby the nonflammable component of the served.
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 for
material is masked resulting in the reporting of incorrect high flash point at temperatures above ambient temperature, have
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flash point or no flash point. resulted in significant burning of the ignitable vapor outside the
test cup, often above the test flame. This can be a potential fire
X1.2 This flash point masking phenomenon most frequently hazard if not recognized.
occurs with ignitable liquids that contain certain halogenated
hydrocarbons such as dichloromethane (methylene chloride) X1.5 It is recommended that if this condition is encountered
and trichloroethylene. during the flash point testing of these type of materials, testing
should be discontinued.
X1.3 Under this condition, no distinct flash as defined in
3.1.5 of these test methods is observed. Instead a significant X1.6 Further commentaries regarding flash point test and
enlargement of the test flame and a change in the color of the flammability of mixtures can be found in Test Method E502.
X2.1 While the flash point can be used to indicate the flammable vapors under certain conditions and yet will not
flammability of liquid materials for certain end uses, flash point exhibit a close-cup flash point. This phenomenon is noted
does not represent the minimum temperature at which a when a nonflammable component is sufficiently volatile and
material can evolve flammable vapors. 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.
components, there are cases where this liquid can evolve
SUMMARY OF CHANGES
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D93 – 18) that may impact the use of this standard. (Approved Nov. 1, 2019.)
Subcommittee D02.08 has identified the location of selected changes to this standard since the last issue
(D93 – 16a) that may impact the use of this standard. (Approved July 1, 2018.)
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