EXPERIMENT: - SOFTENING POINT OF BITUMEN

1.1 SCOPE: -
An alternative to the penetration test for checking the consistency of bitumen, is the ring and
ball softening point test. The scope of this test is to provide a method for determining the
consistency of semi-solid and bituminous materials in which the sole or major constituent is
either bitumen or tar pitch.

1.2 DESIGNATION: -
D 36 – 95

1.3 DEFINITION: -
The softening point of a bituminous material is the temperature at which the material attains a
certain degree of softness under specified conditions of test.

1.4 EQUIPMENT: -
The equipment required to carry the penetration test in the laboratory are listed below:
a) A steel ball having a diameter of 9.3 mm and weighing 3.5g ± 0.05g.
b) Tapped ring, made of brass shall be used for referee purposes. For other purposes either a
straight ring or a shouldered ring may be used.
c) A convenient form of ball contouring guide
d) Ring holder made of brass or other metal
e) Bottom plate made of brass or other metal
f) A thermometer (capacity 1000C and accuracy 0.1 0C)
g) A water bath of heat-resistant glass and conforming to the dimensions given in Figure
10.2.7, the rings being supported in a horizontal position. The bottom of the bulb of the
thermometer shall be level with the bottom of the rings and within 10mm of them but not
touching them. A 600 ml beaker is suitable.
h) Distilled water for materials of softening points of 800C and glycerol for materials of higher
softening point. i) Stirrer.

1.5 SAMPLE PREPARATION: -

The sample obtained in accordance with section 2.7 is heated carefully in an oven or on a
hotplate until it has become sufficiently fluid to pour. When using a hotplate, the bitumen
should be stirred as soon as possible, to prevent local over-heating. In no case should the
temperature be raised more than 900C above the expected softening point and samples must not
be heated for more than 30 minutes. The brass rings to be used for the test are placed on a flat
smooth brass plate, which has been coated immediately prior to use, with a thin covering of a
mixture of glycerin and china clay. The coating is to prevent the bitumen sticking to the plate.
When the bitumen is sufficiently fluid to pour, the rings should be filled with bitumen. A tight
excess of bitumen should be used. The bitumen is allowed to cool for a minimum of 30
minutes. If the bitumen is soft at room temperature, it must be cooled artificially for a further
30 minutes. After cooling the excess material on the top of the specimen must be cut off cleanly
using a moral palette knife.
If further specimens are to be prepared or the test repeated, it is essential to use clean containers
and to use bitumen which has not been previously heated.

1.6 PROCEDURE: -
Softening point denotes the temperature at which the bitumen attains a particular degree of
softening under the specifications of test. The test is conducted by using Ring and Ball
apparatus. A brass ring containing test sample of bitumen is suspended in liquid like water at a
given temperature, A steel ball is placed upon the bitumen sample and the liquid medium is
heated at a rate of 5 C per minute. Temperature is noted when the softened bitumen touches the
metal plate which is at a specified distance (25 mm) below. Generally, higher softening point
indicates lower temperature susceptibility and is preferred in hot climates.

1.7 OBSERVATION AND CALCULATION: -

Test property No of observation

1. 2.
Temperature in ℃ at which
1st ball touch the bottom
plate
Temperature in ℃ at which
2nd ball touch the bottom
plate
Mean value
Final softening point
temperature
2 DETERMINATION OF FIRE POIINR AND FLASH
POINT OF BITUMEN

2.1 OBJECTIVES:
 Flash and Fire point test is conducted on bitumen to know the safe mixing and
application temperature values of particular bitumen grade.
 This test is done to determine the flash point and the fire point of asphaltic bitumen and
fluxed native asphalt, cutback bitumen and blown type bitumen as per IS: 1209 – 1978

2.2 SCOPE:
At higher temperatures bituminous materials leave out volatiles. These volatile vapors contains
hydro carbons. So, they can catch the fire easily and will cause flash at one point and if it is
further prone to heat the material may ignite and burn.

Catching fire is very dangerous during mixing of bitumen especially during its application. So,
it is necessary to recognize the safe temperature values of bitumen grades for mixing as well as
for applying. The limited values of temperature can be determined by conducting Flash point
and Fire point test on bitumen.

2.3 THEORY:
Bituminous materials leave out volatiles at high temperatures depending upon their grade.
These volatile catch fire causing a flash. The flash point is the lowest temperature at which
flash occurs due to ignition of volatile vapors when a small flame is brought in contact with the
vapors of a bituminous product, gradually heated under standardized condition then bituminous
material is further heated to a high temperature, the material itself catches and
continues to burn, the l o w e s t t e m p e r a t u r e c a u s i n g t h i s i s t h e f i r e p o i n t . T h i s
c o n d i t i o n i s v e r y h a z a r d o u s a n d i t i s therefore essential to qualify this temperature
for each bitumen grade.
Flash point: The Flash point of a material is the lowest temperature at which vapor of
substance quickly catches fire in the form of flash under definite conditions of the test. So, at
this point fire will not last longer, just a flash will appear for a fraction of second.

The existence of highly volatile and inflammable materials in a particular grade of bitumen can
be indicated by the Flash point.

Fire Point: The fire point of a material is the lowest temperature at which material catches fire
and burns under definite conditions of test.

The presence of combustible materials in a bituminous material can be indicated by the Fire
point.
 2.4 APPARATUS:

 Pensky-Martens closed tester

 Thermometer
Pensky-Martens closed cup tester contains testing cup, lid, stirrer device, shutter, and flame
exposure device. Thermometer of specified range generally 0oC to 350oC with sensitivity of
0.1oC should be used.

2.5 PROCEDURE:
1. Heat the bitumen to above its softening point generally 75 oC to 100oC and stir this softened
bitumen thoroughly to remove air bubbles.
2. Fill the cup with softened bitumen up to the filling mark provided on the cup. Now place the lid
and close the cup.

3. Other accessories like thermometer and flame exposure are suitably fixed in their respective
positions. Now lit up the flame and set the size of flame to 4mm in diameter.

4. The bitumen getting heated and preferred rate of heating should be 5oC to 6oC per minute.
5. Stirring of sample should be simultaneously done along with heating using stirrer device.

6. The rate of stirring should be approximately 60 revolutions per minute.

7. Observe the thermometer carefully and when the temperature is 17 oC below the actual flash
point (175OC) lit up the test flame.
8. The test flame size should be of 4mm diameter and carry it close to the heating sample.

9. Apply the test flame for every 1OC rise from this point and remember during application of test
flame the stirring should be stopped.
10. When the sample catches the flame and forms Flash, note town the temperature at that point
which is Flash point of the bitumen.
11. Heat the sample further with the same previous rate and apply the test flame for every 2 OC rise
when the material catches the fire and burns at least for 5 seconds, note the temperature at this
point which is the fire point of the bitumen.
12. Repeat the experiment for 2 more times and the average of the three readings should be taken
as Flash point and Fire point of the given sample.

2.6 RESULTS:
 Flash point of the bitumen = _______   OC
 Fire point of the bitumen   =    _______   OC

2.7 RECOMMENDED VALUES:

For any type of Bitumen grade, Minimum Flash point value should be = 175 OC

2.8 PRECAUTIONS:

 The test flame should neither be larger than stipulated nor be applied more frequently than
specified as the surface layer may get super-heated.     
  The bluish halo that sometimes surrounds the test flame should not be confused with the true
flash.
3 TESTS FOR BITUMEN & BITUMINOUS MATERIALS

3.1 SCOPE: -
This is a basic test for determining the grades of bitumen. In effect, the test is an indirect
determination of high temperature viscosity and low temperature stiffness. The scope of this is
to provide a method for determining the consistency of semi-solid and solid bituminous
materials in which the sole or major constituent is either bitumen or tar pitch.

3.2 DEFINITION: -
The penetration of bituminous material is its consistency expressed as the distance in tenths of
a millimeter that a standard needle penetrates vertically into a specimen of the material under
specified conditions of temperature, load and duration of loading.
Grades of straight-run bitumen are designated by two penetration values, for example, 40/50,
60/80, 80/100 etc.; the penetration of an actual sample of the bitumen in any grade should fall
between the lower and upper value given.

3.3 APPARATUS
The test apparatus consists of a right frame which holds the needle spindle in a vertical position
and allows it to slide freely without friction. A dial gauge calibrated in millimeters measures
the penetration. The total weight of the needle and spindle must be 50  0.05 grams and
facilities for adding additional weights of 50  0.05 grams and 100  0.05 grams must be
provided. The surface on which the sample container rests must be flat and at right angles to
the needle.
A penetration needle made of fully hardened and tempered stainless steel of 1.00mm in
diameter and 50mm in length, with one end ground to a truncated cone as shown in Figure
10.1.1. The needle is held by brass or stainless-steel ferrule. The test is shown diagrammatically
in Figure 10.1.1.
The sample is placed in a metal or glass flat bottom container of the following dimensions: -
For penetrations below 200 mm:
Diameter 55 mm
Internal depth 35 mm

For penetrations between 200- and 350-

mm Diameter 70 mm
Internal depth 45 mm
The sample and dish are brought to the required temperature in a water bath which is
maintained at a temperature within 0.1/oC of the test temperature. The sample container must
be placed on a perforated shelf which is between 50 and 100 mm below the surface of the
water.
 100 gms.

100 gms.

To maintain the sample at the correct temperature during the test, a glass transfer dish is used.
This dish of at least 350 ml capacity is fitted with a suitable support to hold the sample
container firm and level during testing.
A stopwatch is required to measure the time of penetration.

3.4 SAMPLE PREPARATION

a) A sample of bitumen is first heated carefully in an oven or on a hotplate until it has
become sufficiently fluid to pour. When using a hotplate, the bitumen should be stirred
as soon as possible to prevent local overheating. In no case should the temperature be
raised more than 900C above the softening point, and samples must not be heated for
more than 30 minutes.
b) When sufficiently fluid a portion of the sample is poured into the sample container to a
depth of at least 10mm greater than the depth to which the needle is expected to
penetrate.
c) The sample is then covered loosely to protect against dust, and allowed to cool in the
atmosphere between 15 and 300C for 1 to 1½ hours for the small container and 1½ to 2
hours for the large container.
d) After cooling in air, the sample containers together with the transfer dishes should be
placed in the water bath at the required temperature, for a period of 1 to 1½ hours for
the small container and 1½ to 2 hours for the large container.

8040’ to 9040’ 0.14 to 0.16 mm

1.00 to 1.02 mm

Approx.
Approximately 6.35 mm
50.8 mm (2’)
3.5 CONDITIONS OF TEST
The test is normally carried out at a temperature of 25 0C with the total weight of the
needle, spindle and added weights being 100 grams, the needle is released for a
period of 5 seconds. If it is not possible to obtain these conditions or if there are
special circumstances, one of the following alternative conditions may be used:-

Temperature,
0
Total sliding Time,
C (0F) weights, grams seconds
0 (32) 200 60
4 (39.2) 200 60
46.1 (115) 50 5
It will be noted that, to obtain the standard temperature of 250C in Bangladesh, cooling of the
water bath is normally required, it may, therefore, be more convenient in many cases to use a
temperature of 46.10C

3.6 TEST PROCEDURE: -

a) The needle should be examined for damage or surface roughness; it should be dry and
clean. To ensure the needle is perfectly cleaned, it should be wiped with a cloth soaked
in toluene or another suitable bitumen solvent and then dried with a clean cloth.
b) The clean needle should be inserted into the penetrometer apparatus and the total
sliding weight made up to the required value, if necessary by adding additional weights.
For example, if 100 grams is required, and the needle and spindle weigh 50 grams, an
additional weight of 50 grams must be added.
c) The sample container is then placed in the transfer dish complete with water at the
required temperature from the constant temperature bath, the sample being completely
covered with water at all times. The transfer dish is then placed on the stand of the
apparatus.
d) The penetrometer needle is then slowly lowered until it just touches the surface of the
sample. This point is best judged by using a strong source of light and determining the
point where the tip of the needle just meets its image reflected by the surface of the
sample. The initial dial gauge reading is taken.
e) The needle is then released for the specified time and re-locked immediately at the end
of the period. Care should be taken not to disturb or jolt the apparatus when releasing
the needle, if this occurs or the sample moves, the test must be repeated. The final dial
gauge reading is taken.
f) The transfer dish should then be returned to the water bath and a clean needle fitted to
the machine. The test is then repeated on the same sample. This procedure is repeated so
that at least 3 determinations are made on each sample, taking care that each point is at
least 10mm from the side of the sample container and at least 10mm from the other
determinations. If the penetration exceeds 200mm, the needles should be left in the
sample until all three determinations have been completed.

3.7 CALCULATION
The penetration is given by:

Penetration = (Initial dial gauge reading (mm) - Final dial gauge reading (mm)) x 10

A typical worksheet is shown as Form 10.1.1.

The three penetration values obtained on the sample must agree to within the
following limits: -

Penetration 0 to 49 50 to 149 150 to 249 250

Maximum difference between highest
and lowest determination 2 4 6
8
If the differences exceed the above values, the results are ignored and the test must
be repeated on the second sample. If the differences are again exceeded by the
second sample, the results must be ignored and the test completely repeated.

If the determinations are within the above tolerances, the penetration is quoted as
the average of the individual results.