EXPERIMENT NO: 01

NAME OF EXPERIMENT: Penetration Test of Bitumen.

OBJECTIVE: To determine the Penetration Value of bitumen.

THEORY:
The consistency of bituminous materials vary depending upon several factors such as
constituents, temperature etc. At temperature ranges between 25 and 500C most of the paving
bitumen grades remain in semi or in plastic states and their viscosity is so high that they do not
flow as liquid. But the viscosity of most of the tars and cutbacks are sufficiently low at this
temperature range to permit these bituminous materials to be in a liquid state, enabling some of
the grades to be mixed with aggregates even without heating.

Determination of absolute viscosity of bituminous materials is not so simple. Therefore

the consistency of these materials are determined by indirect methods; the consistency of
bitumen is determined by Penetration test which is a very simple test; the viscosity of tars and
cutback bitumen’s are determined indirectly using an orifice viscometer in terms of time
required for a specified quantity of materials to flow through an orifice. There is a certain range
of consistency of bituminous materials, where in the material is too soft for penetration test, but
the viscosity is so high that the material can not flow through the orifice of the viscometer; the
consistency of such materials is measured by ‘float test’.

Various types and grades of bituminous materials are available depending on their and
refining process. The penetration test determines the consistency of these materials for the
purpose of grading them, by measuring the depth (in units of one tenth of a millimeter or one
hundredth of a centimeter) to which a standard needle will penetrate vertically under specified
conditions of standard load, duration and temperature. Thus the basic principle of the
penetration test is the measurement of the penetration (in units of one tenth of a mm) of a
standard needle in a bitumen sample maintained at 250C during five seconds, the total weight of
the needle assembly being 100 kg. the softer the bitumen, the greater will be the penetration.

The penetration test is widely used world over for classifying the bitumen into different
grades. The ISI has standardized the penetration test equipment and the test procedure, fig. ……
Even though it is recognized that the empirical tests like penetration, softening point etc. can not
fully qualify the paving binder for its temperature susceptibility characteristics, the simplicity
and quickness of operation of this test can not be ignored for common use.

APPARATUS: -
It consists of items like container, needle, water bath penetration, stop watch
etc. Following are the standard specifications as per ISI for the above apparatus.

(a) Container: A flat bottomed cylindrical metallic container 55 mm in diameter and 35 mm or

57 mm in height.

(b) Needle: A straight, highly polished cylindrical hard steel needle with conical end, having
the shape and dimensions as given in Fig. …… The needle is provided with a shank
approximately 3.0 mm in diameter into which it is immovably fixed.
(c) Water-bath: A water bath is maintained at 25±10C containing not less than 10 litres of
water; the sample is immersed to depth not less than 100 mm from the top and supported on a
perforated shelf not less than 50mm the bottom of the bath.

(d) Penetrometer: It is an apparatus which allows the needle assembly of gross weight 100 g to
penetrate without appreciable friction for the desire duration of time. The dial is accurately
calibrated to give penetration value in units of one tenth of a mm. Electrically operated
automatic Penetrometer are also available. Typical sketch of penetrometer is shown in fig…..

(e) Transfer tray: A small tray, which can the container fully immersed in water during the
test.

Fig. 1.a Penetration Test concept Fig 1.b Penetration Needle

PROCEDURE:
The bitumen is softened to a pouring consistency between 750C and 1000C above the
approximate temperature at which bitumen softens. The sample material is thoroughly stirred to
make it homogenous and free from air bubbles and water. The sample material is then poured
into the container to a depth at least 15mm more than the expected penetration. The sample
containers are cooled in atmosphere of temperature not lower than 130C for one hour. Then they
are placed in temperature controlled water bath at a temperature of 250C for a period of one
hour.

The sample container is placed in the transfer tray with water from the water Bath and
placed under the needle of the penetrometer. The weight of needle, shaft and additional weight
are checked. The total weight of this assemble should be 100g. Using the adjusting screw, the
needle assembly is lowered and the tip of the needle is made to just touch the top surface of the
sample; the needle assembly is clamped in this position. The contract of the tip of the needle is
checked using the mirror placed on the rear of the needle. The initial reading of the penetrometer
dial is either adjusted to zero or the initial reading is taken before releasing the needle. The
needle is released exactly for a period of 5.0 seconds by pressing the knob and the final reading
is taken on the dial. At least three measurements are made on this sample by testing at distance
of not less than 100 mm apart. After each test the needle is disengaged and cleaned with
benzene and carefully dried. The sample container is also transferred in the water bath before
next testing is done so as to maintain a constant temperature of 250C. The test is repeated with
sample in the other containers.
 Fig. 1.c. Penetrometer

RESULTS:
The difference between the initial and final penetration readings is taken as the
penetration value. The mean value of three consistent penetration measurements is reported as
the penetration value. It is further specified by ISI that results of each measurement should not
vary from the mean value reported above by more than the following:

Penetration grade Repeatability

0-80 4 percent
80-225 5 percent
Above 225 7 percent

Discussion:

It may be noted that the penetration value is influence by any inaccuracy as regards:
(i) Proving temperature
(ii) Size of needle
(iii) Weight placed on the needle
(iv) Test temperature
(v) Duration of releasing the penetration needle

It is obvious to obtain high values of penetration if the test temperature and / or weight
(placed over the needle) are / is increased. Higher pouring temperature than that specified may
result in hardening of bitumen and may give lower penetration values. The duration of releasing
the penetration needle be exactly 5.0 seconds. It is also necessary to keep the needle clean
before testing in order to get consistent results. The penetration needle should not be placed
closer than 10mm from the side of the dish.

Application of Penetration Test:

Penetration test is the most commonly adopted test on bitumen to grade the material in
terms of its hardness. Depending upon the climatic condition and type of construction,
bitumen’s of different of different penetration grades are used, 80/100 bitumen denotes that the
penetration value ranges between 80 and 100. The penetration values of various types of
bitumen used in pavement construction in this country range between 20 and 225. For
bituminous macadam and penetration macadam Indian road Congress suggests bitumen grades
30/40, 60/70 and 80/100. In warmer regions lower penetration grades are preferred and in colder
regions bitumen with higher penetration values are used.

The penetration test is not intended to estimate the consistency of softer materials like
cutback or tar, which are usually graded by a viscosity test in an orifice viscometer.
The Indian Standards Institution has classified paving bitumen available in this country
into the following six categories depending on the penetration values. Grades designated ‘A’
(such as A 35) are from Assam Petroleum and those designated ‘S’ (such as S 35) are from other
sources.

Bitumen grade A 25 A35 & S 35 A45 & S 45 A65 & S 65 A90 & S 90 A200 & S
200
Penetration 20 to 30 to 40 40 to 50 60 to 70 80 to 100 175 to 225
value 30

OBSERVATION SHEET- PENETRATION TEST

(i) Pouring Temperature, 0C =

(ii) Period of cooling in atmosphere, minutes =
(iii) Room temperature, 0C =
(iv) Period of cooling in water bath, minutes =
(v) Actual test temperature, 0C =
 Readings Sample No. Sample No.
Test 1 Test 2 Test 3 Mean Test 1 Test 2 Test 3 Mean
Value Value
Penetrometer dial reading (i) initial
(ii) final
Penetration value
Repeatability, percent

Mean Penetration value =

Remarks:

REFERENCE:-
1. IS: 1203-1978, Methods for testing of tar and bituminous materials: Determination
of Penetration (First Revision).

EXPERIMENT NO: 02

NAME OF EXPERIMENT: Determination of Softening Point of Bitumen.

OBJECTIVE: To determine the Softening Point of Bitumen.

THEORY:
This test is conducted to determine the softening point of bitumen. The temperature
at which the substance attains a particular degree of softening under specified condition of test
is called the softening point.

APPARATUS:
The apparatus as per IS: 1205-1978 for this test are as follows:

1) Ring and Ball Apparatus:

i) Steel Balls: - Two, each 9.5mm in diameter and weighting 3.50±0.05g.

ii) Brass Rings:- Two, the ring shall be tapered and shall conform to the following
dimensions:

Depth 6.4 ± 0.1 mm

Inside diameter at bottom 15.9 ± 0.1 mm
Inside diameter at top 17.5 ± 0.1 mm
Outside diameter 20.6 ± 0.1 mm
 The out side diameter of the ring at the bottom may be smaller, but shall be not
less than 19.0mm.

iii) Ball Guide: - A convenient form of ball centering guide. A recommended form of
ball guide is shown in fig.
iv) Supports:- Any means supporting the rings may be used provided the following
conditions are observed:
a) The ring shall be supported in a horizontal position with the upper
surface of the rings 50 mm below the surface of the bath liquid.
b) There shall be a distance of exactly 25mm between the bottom of the
rings and the top surface of the bottom plate of the supports, if any, or
the bottom of the bath.
c) The thermometer shall be suspended so that the bottom of the bulb is
level with the bottom of the rings, and within 10mm of the rings, but
not touching them.

Fig.2.a Assembly of apparatus for determination of Softening Point (Ring

and Ball- Two Rings)
Fig 2.b. Ball Centering Guide Fig 2.c. Tapered Ring

Fig.2.d. Ring Holder ( All dimension are in mm)

v) Thermometer: It shall be of the mercury-in-glass type, nitrogen filled, with the stem
made of lead glass or other suitable glass. It shall; be engraved and enameled
at the back and provided with an expansion chamber and glass ring at the top.
The bulb shall be cylindrical, made of suitable thermometric glass. The
dimensions, tolerances and graduations of the thermometer shall be as
follows:

Low temperature High temperature

Range -20Cto 800C 30 to 2000C
Graduation at each 0.20C 0.50C
Longer lines at each 10C 10C
Figured at each 20C 50C
Immersion, mm Total Total
Overall length 378 to 384 378 to 384
Length of graduated portion 243 to 279 243 to 279
Length of bulb, Max 9 to 14 Not larger than stem 9 to 14 Not larger than stem
diameter diameter
Stem diameter 6.0 to 7.0 mm 6.0 to 7.0 mm
Distance from bottom of bulb to 00C 75 to 90 mm 75 to 90 mm
Scale error, Max ± 0.20C ± 0.20C
 vi) Bath: - A heat resistance glass vessel not less than 85 mm in diameter and
120 mm in depth. The bath liquid shall be freshly boiled with distilled water
when testing materials having softening points below 800C.
vii) Stirrer: - Manual or mechanical, which operates smoothly to ensure uniform
heat distribution at all times throughout the bath. The stirrers shall be so
placed that the moulds are not disturbed when the stirrer is in operation.

PROCEDURE:
i) Preparation of Test Sample: - Heat the material to a temperature between 750C and
1000C above its softening point, stir until it is completely fluid and free air bubbles
and water, and filter, if necessary, through IS Sieve 30. Place the rings, previously
heated to a temperature approximating to that of the molten material, on a metal plate
which has been coated with a mixture of equal parts of glycerine and dextrine, and
fill with sufficient melt to give an excess above the level of the ring when cooled.
After cooling for 30 minutes in air, level the material in the ring by removing the
excess with a warmed, sharp knife.

ii) Material of softening point above 800C: - The procedure for materials of softening
point above 800C is similar to that described above with the difference that glycerine
is used in place of water in the bath and the starting temperature of the test is 350C.
Make the determination in duplicate.

REPORT: -

i. Record for each ring and ball, the temperature shown by the thermometer at the
instant the sample surrounding the ball touches the bottom plate of the support, if
any, or the bottom of the bath.
ii. Report to the nearest 0.50C the mean of the temperature recorded in duplicate
determinations, without correction for the emergent stem of the thermometer, as the
softening point.

PRECISION:-
Test results shall not differ from the mean by more than the following:

Softening Point (0C) Repeatability(0C) Reproducibility(0C)

40 to 60 1.0 5.5
61 to 80 1.5 5.5
81 to 100 2.0 5.5
101 to 120 2.5 5.5
121 to 140 3.0 5.5
PRECAUTIONS:
i) Only fresh boiled distilled water shall be used in the test, as otherwise air bubbles
may form on the specimen and affect the accuracy of the results.
ii) The prescribed rate of heating shall be rigidly adhered to for ensuring accuracy of
results.
iii) A sheet of filter paper or thin amalgamated sheet, placed on the bottom of the glass
vessel and conveniently weighted would prevent the material from sticking to the
glass vessel and considerable time and trouble in cleaning would thereby be saved.

REFERENCES
1) IS: 1205-1978

EXPERIMENT NO: 03

NAME OF EXPERIMENT: Determination of Ductility of Tar and

Bituminous Materials.

OBJECTIVE: To determine the Ductility of Tar and Bituminous Materials.

THEORY:
This test is conducted to determine the ductility of distillation residue of cutback
bitumen, blown type bitumen and other bituminous products. The ductility of a bituminous
material is measured by the distance in centimeters to which it will elongate before breaking
when a briquette specimen of the material of the form describe in Mould (below) are pulled
apart at a specified speed and at a specified temperature.

APPARATUS:-
1) Mould:- Made of brass with the shape , dimensions and tolerances as shown in
fig. The ends b and b′ are known as clips, and the parts a and a′ as sides of the
mould. The dimensions of the mould shall be such that when properly assembled,
it will form a briquette specimen having the following dimensions:

Total length = 75.0 ± 0.5 mm

Distance between clips = 30.0 ± 0.3 mm
Width at mouth of clip = 20.0 ± 0.2 mm
Width at minimum cross- section = 10.0 ± 0.1 mm
(Half way between clips)

Thickness throughout = 10.0 ± 0.1 mm

2) Water Bath :- A bath preferably with a thermostat maintained within ±0.10C

of the specified test temperature, containing not less than 10 liters of water, the
specimen being immersed to a depth of not less than 100 mm and supported on a
perforated shelf not less than 50 mm from the bottom of the bath.

3) Testing machine:- For pulling the briquette of bituminous material apart, any
apparatus may be used which is so constructed that the specimen will be
continuously immersed in water at the specified temperature for about 85 to 95
minutes while the two clips are pulled apart horizontally with minimum
vibrations at a uniform speed, as specified and with suitable arrangement for
stirring the water for attaining uniformity in temperature.

4) Thermometer: Conforming to the following requirements:

Fig.3. Mould for Ductility Test

Characteristics Requirement
Range 0 to 440C
Graduations 0.20C
Immersion 65mm
Overall length 340 ± 10 mm
Stem diameter 5.5 to 8.0mm
Bulb length 10 to 60mm
Bulb diameter Not larger than stem diameter
Length of graduated portion 150 to 190 mm
Longer lines at each 10C and 50C
Figures at each 50C
Scale ± 0.20C
PROCEDURE:-
1) Unless otherwise specified, the test shall be conducted at a temperature of 27.0 ±
0.50C and at a rate of pull of 50.0 ± 2.5 mm/min
2) When a low temperature ductility test is desired, the test shall be made at a
temperature of 4.0 ± 0.50C and at a rate of pull of 10.0 ± 0.5 mm/min
3) Completely melt the bituminous material to be tested to a temperature of 75 to
1000C above the approximately softening point until it becomes thoroughly fluid.
Assemble the mould on a brass plate and in order to prevent the material under
test from sticking, thoroughly coat the surface of the plate and interior surfaces of
the sides of the mould ( a and a′ in fig) with a mixture of equal parts of glycerin
and dextrin. In filling, pour the material in a thin stream back and forth from to
end to end of the mould until it is more than level full. Leave it to cool at the
room temperature for 30 to 40 min, and then place in a water bath maintain at the
specified temperature for 30 min after which cutoff the excess bitumen by means
of a hot, straight edged putty knife or spatula so that the mould shall be just level
full.
4) Testing:- Place the brass plate and mould with briquette specimen, in the water
bath and keep at the specified temperature for about 85 to 95 minutes. Then
remove the briquette from the plate, detach the side pieces, and test the briquette
immediately.
5) Attach the rings at each end of the clips to the pins or hooks in the testing
machine and pull the two clips apart horizontally at a uniform speed as specified
until the briquette ruptures. Measure the distance in centimeters through which
the clips have been pulled to produce rupture. While the test is being made, make
sure that the water in the tank of the testing machine covers the specimen both
above and below it by at least 25mm and is maintained continuously within ±
0.50C of the specified temperature.

REPORT:-
1) A normal test is one in which the material between the two clips pulls out to a
pointy or to a thread and rupture occurs where the cross-sectional area is a
minimum. Report the average of three normal tests as the ductility of the sample,
provided the three determinations be within ± 5 percent of their mean value.
2) If the value of the three determinations do not lie within ± 5 percent of their mean
value but the two higher values are within ± 5 percent of their mean then record
the mean of the two higher values as test result.
3) If the bituminous material comes in contact with the surface of the water or the
bottom of the bath, the test shall not be considered normal. Adjust the specific
gravity of the water in the bath by addition of either methyl alcohol or sodium
chlorides so that the bituminous material does not either come to the surface of
the water, or touch the bottom of the bath at any time during the test.
4) If a normal test is not obtainable on three successive tests, report the ductility as
being unobtainable under the condition of test.

PRECESSION:-
 The test results shall not differ by more than the following:
Repeatability 10 percent of the mean
Reproducibility 20 percent of the mean

PRECAUTIONS:-
1) The plate upon which the mould is placed shall be perfectly flat and level so that
the bottom surface of the mould touches it throughout.
2) In filling the mould, care shall be taken not to disarrange the parts and thus distort
the briquette and to see that no air pocket shall be within the moulded sample.

REFERENCE:-
1. IS: 1208-1978, Methods for testing of tar and bituminous materials: Determination
of Ductility

EXPERIMENT NO: 04

NAME OF EXPERIMENT: Determination of Specific Gravity of Tar and

Bituminous Materials.

OBJECTIVE: To determine the Specific Gravity of Tar and Bituminous Materials.

THEORY:
This test is conducted to determine the Specific Gravity of asphalt, bitumen,
bituminous products, road tar, coal tar, coal tar pitch, and creosote and anthracene oil. The ratio
of the mass of a given volume of the substance to the mass of an equal volume of water, the
temperature of both being specified. If the temperature of the substance is t1 and that of water is
t2 the specific gravity S, is denoted by St1/t2; t1 and t2 shall be specified clearly. The specific
gravity of bitumens, fluxed native asphalt, road tars, coal tar pitch and blown bitumen shall be
determined at 270C and that of creosote oil and anthracene oil at 380C and shall be expressed as
specific gravity 270C/270C or 380C/380C.

( Pycnometer Method):

This method covers the determination of specific gravity for semi solid bitumen road tar and
creosote and anthracene oil.

APPARATUS:-

1) Specific gravity bottles:- Specific gravity bottles of 50ml capacity shall be used. One of the
two types of Specific Gravity bottles, namely (a) the ordinary capillary type specific gravity
bottle with a neck of 6mm diameter and (b) the wide mouthed capillary type specific gravity
 bottle with a neck of 25mm diameter shall be used. The ordinary specific gravity bottle shall
be used for materials which remain absolutely fluid at 270C while the wide mouth capillary
type shall be used for materials which remain semisolid or high viscous at 270C.
2) Constant Temperature bath:- A water bath having a depth greater than that of
Pycnometer capable of being maintained within 0.20C of the desired temperature.
3) Bath Thermometer:- It shall conform the following requirements:
Characteristics Requirement
Range 0 to 440C
Graduations 0.20C
Immersion 65mm
Overall length 340 ± 10 mm
Stem diameter 5.5 to 8.0mm
Bulb length 10 to 60mm
Bulb diameter Not larger than stem diameter
Length of graduated portion 150 to 190 mm
Longer lines at each 10C and 50C
Figures at each 50C
Scale ± 0.20C

Fig. 4.a. Showing the Specific gravity bottle

PROCEDURE:-

1) Clean, dry and weight the specific gravity bottle together with the stopper (a). Fill it with
freshly boiled and cooled distilled water and insert the stopper firmly. Keep the bottle up to
its neck for not less than half an hour in a beaker of distilled water maintained at a
temperature of 27.0 ± 0.10C or any other temperature at which specific gravity is to be
determined; wipe all surplus moisture from the surface with a clean, dry cloth and weight
again(b). After weighing the bottle and water together (b) the bottle shall be dried again.
2) In the case of solid and semisolids, bring a small amount of the material to a fluid condition
by gentle application of heat, care being taken to prevent loss by evaporation. When the
material is sufficiently fluid, pour a quantity into the clean, dry specific gravity bottle
mentioned at step1 to fill at least half. Slightly warm the bottle before filling. Keep the
material away from touching the sides above the final level of the bottle and avoid the
inclusion of air bubbles. The use of a small funnel will prevent contamination of the neck of
the bottle. To permit escape of entangle air bubbles, allow the partly filled bottle to stand
foe half an hour at a suitable temperature, then cool to the specified temperature and weigh
with the stopper(c).
3) Fill the specific gravity bottle containing the asphalt with freshly boiled distilled water
placing the stopper loosely in the specific gravity bottle. Do not allow any air bubble to
remain in the specific gravity bottle. Place the specific gravity bottle in the water bath and
press the stopper firmly in place. Allow the specific gravity bottle to remain in the water
bath for a period of not less than 30 minutes. Remove the specific gravity bottle from the
water bath, wipe all surplus moisture from the surface with a clean dry cloth and weigh it
along with the stopper.
4) In case of liquids such as creosote and anthracene oil, fill the bottle up to the brim and insert
the stopper firmly. Keep the filled bottle for not less than half an hour in a beaker of
distilled water maintained at a temperature of 27.0 ± 0.10C, remove the bottle from the
beaker, wipe all surplus water from the surface with a clean, dry cloth and weigh again.

CALCULATION:-
Calculate the specific gravity of the material as follows:

a) Specific gravity (solid and semi solid) = c – a________

( b - a) – (d - c)

b) Specific gravity ( liquid ) = c – a______

( b - a)

Where
a = mass of the specific gravity bottle,
b = mass of the specific gravity bottle filled with distilled water,
c = mass of the specific gravity bottle about half filled with the material
d = mass of the specific gravity bottle about half filled with the material and the rest with
distilled water, and
e = mass of the specific gravity bottle completely filled with the material.

REPORT:
Results of the test shall be expressed as the ratio of a given volume of the
material at a temperature specified ( i.e. for bitumen 270C and that of creosote oil and
anthracene oil at 380C) to the mass of the same volume of water at the same temperature.

PRECESSION:-
 With samples which are neither very volatile nor very viscous and using
a Pyknometer of at least 25ml capacity, the results of duplicate tests should not be differ by the
following:

Repeatability Reproducibility
0.002 0.005

PRECAUTIONS:-
When making the specific gravity determination, it is important that:

i. Only fresh boiled and cooled distilled water shall be used,

ii. At no time of weighing shall the temperature of the apparatus be allowed to exceed the
specified temperature;
iii. Precautions shall be taken to prevent expansion and over flow of the contents resulting
from the heat of the hand when wiping the surface of the apparatus;
iv. All air bubble shall be eliminated in filling the apparatus and inserting the stopper;
v. Weighing shall be done quickly after filling the apparatus and shall be accurate to 0.1
mg; and
vi. To prevent breakage of the apparatus when cleaning after a determination has been made
upon a very viscous of semisolid material, it is advisable to warm it in an oven at a
temperature not above 1000C, until most of the material is poured out and then a swab it
with a piece of soft cloth or cotton waste. When cool, it may be finally rinsed with
carbon disulphide, benzol or other solvent and wiped clean.

REFERENCE:-

1) IS: 1202-1978, Methods for testing of tar and bituminous materials: Determination
of Specific Gravity (First Revision).