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Chapter 10 Standard Test Procedures

Tests For Bitumen & Bituminous Materials

10.5 Flash Point and Fire Point Tests of Bitumen

10.5.1 Introduction

Flash point of bitumen is the temperature at which, it’s vapour will ignite temporarily
during heating, when a small flame is brought into contact with the vapour. The
knowledge of this point is of interest mainly to the user, since the bitumen must not
be heated to this point. The flash point tells the critical temperature at and above
which suitable precautions are required to be taken to eliminate the danger of fire
during heating. This temperature, however, is well below that at which the bitumen will
burn. The latter temperature is called the fire point.

10.5.2 Definitions

Flash point. It is the lowest temperature at which the vapour of a bituminous material
momentarily takes fire in the form of a flash, under specified conditions of test.

Fire point. It is the lowest temperature at which bituminous materials ignite and burn
under specific conditions of test.

10.5.3 Scope

This method covers the determination of the flash and fire points, by Cleveland Open
Cup Tester, of petroleum products and other liquids, except fuel oils and those
materials having an open cup flash point below (79 C) as determined by the
Cleveland Open Cup Tester.

10.5.4 Apparatus

a) Cleveland Open Cup Apparatus - This apparatus consists of the test cup, heating
plate, test flame applicator and heater, thermometer support, and heating plate
support, all conforming to the following requirement:

Test Cup- of brass conforming to the dimensional requirements shown in Figure


10.5.3. The cup may be equipped with a handle.

Heating Plate - A brass, cast iron, wrought iron, or steel plate with a center hole
sur-rounded by an area of plane depression, and a sheet of hard asbestos board
which covers the metal plate except over the area of plane depression in which
the test cup is supported. The essential dimensions of the heating plate are
shown in Fig. 10.5.2., however, it may the square instead of round, and the metal
plate may have suitable extensions for mounting the test flame applicator device
and the thermometer support. The metal bead, may be mounted on the plate so
that it extends through and slightly above a suitable small hole in the asbestos
board.

Note. The sheet of hard asbestos board which covers the heating plate may
be extended beyond the edge of the heating plate to reduce drafts
around the cup. The F dimension given is intended for gas apparatus.
For electrically heated apparatus the plate shall be of sufficient size to
cover the top of the heater.

Test Flame Applicator - The device for applying the test flame may be of any
suitable design, but the tip shall be 1.6 to 5.0 mm or 0.06 to 0.20 in. in diameter
at the end and the orifice shall have an approximate diameter of 0.8 mm or 0.031
in. The device for applying the test flame shall be so mounted to permit automatic
duplication of the sweep of the test flame, the radius of swing being not less than

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Chapter 10 Standard Test Procedures
Tests For Bitumen & Bituminous Materials

150 mm or 6 in. and the center of the orifice moving in a plane not that 2.5 mm or
0.10 in. above the cup. A bead having a diameter of 3.8 to 5.4 mm or 0.15 to
0.21 in. may be mounted in a convenient position on the apparatus so the size of
the test flame can be compared to it.

Heater - Heat may be supplied form any convenient source. The use of a gas
burner of alcohol lamp is permitted, but under no circumstances are products of
combustion or free flame to be allowed to come up around the cup. An electric
heater controlled by a variable voltage transformer is preferred. The source of
heat shall be centered under the opening of the heating plate with no local
superheating. Flame-type heaters may be protected from drafts or excessive
radiation by any suitable type of shield that does not project above the level of
the upper surface of the asbestos board.

Thermometer Support - Any convenient device may be used which will hold the
thermometer in the specified position during a test and which will permit easy
removal of the thermometer form the test cup upon completion of a test.

Heating Plate Support - Any convenient support will hold the heating plate level
and steady may be employed.

One form of the assembled apparatus, the heating plate, and the cup are
illustrated in Figures 10.5.1, 10.5.2 and 10.5.3 respectively.

Filling Level Gauge - A device to aid in the proper adjustment of the sample
level in the cup. It may be made of suitable metal with at least one projection, but
preferably two for adjusting the sample level in the test cup to 9 to 10 mm (0.35 to
0.39 in.) below the top edge of the cup. A hole 0.8 mm (1 / 32 in.) in diameter, the
center of which is located not more than 2.5 mm or 0.10 in. above the bottom
edge of the gage, shall be provided for use in checking the center position of the
orifice of the test flame applicator with respect to the rim of the cup. (Figure
10.5.4 shows a suitable version.)

b) Shield - A shield 460 mm (18 in.) square and 610 mm (24 in.) high and having an
open front is recommended.
c) Thermometer.

10.5.5 Preparation of apparatus

a) The apparatus is supported on a level steady table in a draft-free room or


compartment. The top of the apparatus is shielded from strong light by any
suitable means to permit ready detection of the flash point. Tests in a laboratory
heed (Note 1.) or any location where drafts occur are not to be relied upon.

Note 1. With some samples whose vapours or products of pyrolysis are


objectionable, it is permissible to place the apparatus with a shield in a
hood, the draft of which is adjustable so that vapours may be withdrawn
without causing air currents over the test cup during the final 56 C (100
F) rise in temperature prior to the flash point.

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Chapter 10 Standard Test Procedures
Tests For Bitumen & Bituminous Materials

THERMOMETER
ASTM NO. 11C
1P 28C
C

D
TEST FLAME RADIUS
APPLICATOR TEST CUP
A

F HEATING
METAL BEAD PLATE

TO GAS
SUPPLY
HEATER (FLAME OR
ELEC. RESIST. TYPE)

MILLIMETRES INCHES
MIN MAX MIN MAX
A - DIA. OF APLICATOR - 5.0 - 0.20
B - DIA. OF TIP 1.6 5.0 0.06 0.20
C - DIA. OF ORIFICE (0.8 APPROX.) (0.031 APPROX.)
D - RADIUS OF SWING 150 - 6 -
E - INSIDE BOTTOM OF
CUP TO BOTTOM OF
THERMOMETER (6.4 APPROX.) (0.25 APPROX.)
F - DIA. OF OPTIONAL
COMPARISON BEAD 3.8 5.4 0.15 0.21

Figure 10.5.1 Cleveland open cup apparatus

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Chapter 10 Standard Test Procedures
Tests For Bitumen & Bituminous Materials

C D
A

B
METAL THERMAL
INSULATION

MILLIMETRES INCHES
MIN MAX MIN MAX
A 6.4 NOMINAL 0.25 NOMINAL
B 0.5 1.0 0.02 0.04
C 6.4 NOMINAL 0.25 NOMINAL
D - DIAMETER 54.5 56.5 2.15 2.22
E - DIAMETER 69.5 70.5 2.74 2.78
F - DIAMETER 150 NOMINAL 6 NOMINAL

Figure 10.5.2 Heating Plate

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Chapter 10 Standard Test Procedures
Tests For Bitumen & Bituminous Materials

J
BRASS
I

45 0
H
G
FILLING E F
MARK
D

B C

MILLIMETRES INCHES
MIN MAX MIN MAX
A 67.5 69 2.66 2.72
B 62.5 63.5 2.46 2.50
C 2.8 3.6 0.11 0.14
D - RADIUS 4 APPROX. 0.16 APPROX.
E 32.5 34 1.28 1.34
F 9 10 0.35 0.39
G 1.8 3.4 0.07 0.13
H 2.8 3.6 0.11 0.14
I 67 70 2.60 2.75
J 97 101 3.8 4.0

Figure 10.5.3 Cleveland Open Cup

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Chapter 10 Standard Test Procedures
Tests For Bitumen & Bituminous Materials

A
C

B
F
G

E
D D

A/2

MILLIMETRES INCHES
A 100 4 NOMINAL
B 20 3/4 NOMINAL
C 3.2 1/8 NOMINAL
D 30 1-1/4 NOMINAL
E 9 - 10 0.35 - 0.39
F 0.8 DIA. 1/32 DIA. NOMINAL
(2.5 MM ABOVE) (0.10 IN. ABOVE
BOT TOM EDGE BOTTOM EDGE) MAXIMUM
G 10 3/8 NOMINAL

Figure 10.5.4 Filling Level Gauge

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Chapter 10 Standard Test Procedures
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b) The test cup is washed with an appropriate solvent to remove any oil or traces of
gum or residue remaining from a previous test. If any deposits of carbon are
present, they should be removed with steel wool. The cup is flashed cold water
and dry for a few minutes over an open flame, on a hot plate, or in an oven to
remove the last traces of solvent and water. The cup is cooled to at least 56 C
(100 F) below the expected flash point before using.
c) The thermometer is supported in a vertical position with the bottom of the bulb
6.4 mm (1/4 in.) from the bottom of the cup and located at a point halfway between
the center and side of the cup on the diameter perpendicular to the arc (or line)
of the sweep of the test flame and on the side opposite to the test frame burner
arm.

10.5.6 Procedure

a) The cup, is filled at any convenient temperature (Note 2) not exceeding 100 C or
180 F above the softening point, so that the top of the meniscus is at the filling
line. To aid in this operation, a Filling Level Gauge (A7) may be used. If too much
sample has been added to the cup, remove the excess, using a pipette or other
suitable device; however, if there is sample on the outside of the apparatus,
empty, clean and refill it. Any air bubbles on the surface of the sample (Note 3)
are destroyed.

Note 2. Viscous samples should be heated until they are reasonably fluid
before being poured into the cup. For asphalt cement, the temperature
during heating must not exceed 100 C or 180 F above the expected
softening point. Extra caution must be exercised with liquid asphalt’s
which should be heated only to the lowest temperature at which they
can be poured.

Note 3. The sample cup may be filled away from the apparatus provide the
thermometer is preset with the cup in place and the sample level is
correct at the beginning of the test. A shim 6.4 mm (1/4 in) thick is useful
in obtaining the correction distance from the bottom of the bulb to the
bottom of the cup.

b) The test flame is lighted and adjusted to a diameter of 3.8 to 5.4 mm (0.15 to
0.21 in.).
c) Heat is applied initially so that the rate of temperature rise of the sample is 14 to
17 C (25 to 30 F) per minute. When the sample temperature is approximately 56
C (100 F) below the anticipated flash point, decrease the heat so that the rate of
temperature rise for the 28 C (50 F) before the flash point is 5 to 6 C (9 to 11 F)
per minute.
d) Starting at least 28 C (50 F) below the assumed flash point, the test flame is
applied when the temperature read on the thermometer reaches each successive
2 C (5 F) mark. The test flame is passed across the center of the cup, at right
angles to the diameter which passes through the thermometer. With a smooth,
continuous motion apply the flame either in a straight line or along the
circumference of a circle having a radius of at least 150 mm or 6 in. The center of
the test flame must move in a plane not more than 2.5 mm or 0.10 in. above the
plane of the upper edge of the cup passing in one direction first, then in the
opposite direction the next time. The time consumed in passing the test flame
across the cup shall be about 1 s. During the last 17 C (30 F ) rise in temperature
prior to the flash point, care must be taken to avoid disturbing the vapours in the
test cup by careless movements or breathing near the cup.

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Note 4. If a skin should form before the flash or fire point is reached, move it
carefully aside with a small spatula or stirring rod and continue the
determination.

e) The observed flash point is recorded as the temperature read on the


thermometer when a flash appears at any point on the surface of the oil, but do
not confuse the true flash with the bluish halo that sometimes surrounds the test
flame.
f) To determine the fire point, continue heating so that the sample temperature
increases at a rate of 5 to 6 C (9 to 11 F). The application of the test flame is
continued at 2 C (5 F) intervals until the oil ignites and continues to burn for at
least 5 s. Record the temperature at this point as the fire point of the oil.

10.5.7 Correction for barometric pressure

If the actual barometric pressure at the time of the tests is less than 715 mm of
mercury, it is recorded and the appropriate correction is added from the following
table to the flash and fire points, as determined.

Barometric Pressure Correction


mm of Mercury deg C deg F
715 to 665 2 -
715 to 635 - 5
664 to 610 4 -
635 to 550 - 10
609 to 550 6

10.5.8 Calculation and report

1. The observed flash point or fire point, or both is corrected in accordance with
10.5.7.
2. The corrected flash point of fire point, or both is reported as the Cleveland Open
Cup Flash Point or Fire Point, or both.

10.5.9 Precision

The following data should be used for judging the acceptability of results (95 percent
confidence.)

Duplicate results by the same operator should be considered suspect if they differ by
more than the following amounts:

Repeatability
Flash point ..................................................................................................8 0C (15
0
F)
Fire point .................................................................................................….8 0C (15
0
F)

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