CE 342

Transportation Engineering-I
(Sessional
 EXPERIMENT No. 5
Solubility of Bituminous Materials
AASHTO DESIGNATION: T 44-93' (ASTM DESIGNATION: D 2042-81)
SCOPE :
This method covers the determination of the
degree of solubility in trichloroethylene or 1,1
trichloroethylene of asphalt minerals having
little or no mineral matter.
SUMMARY OF METHOD
The sample is dissolved in trichloroethylene or
1,1,1 trichloroethylene and filtered through a
filter mat. The insoluble material is washed,
dried, and weighed.
 .
SIGNIFICANCE AND USE
This method is a measure of the solubility of asphalt in
trichloroethylene or 1,1 trichloroethylene. The portion that is soluble
in trichloroethylene or 1,1,1 trichloroethylene represents the active
cementing constituents.
APPARATUS AND MATERIALS:
• Gooch Crucible, glazed inside and outside with the exception of
outside bottom surface. The approximate dimensions shall be a
diameter of 44 mm at top, tapering to 36 mm at bottom, and a
depth of 28 mm.
• Glass Fibre Pad
• Filter Flask
• Filter Tube
• Rubber Tubing or Adapter
• Erlenmeyer Flask
• Oven
• Desiccators
• Analytical Balance
SOLVENT
Technical grade, Type 1, Trichloroethylene or technical grade 1.1.1
trichloroethylene.
SAFETY PRECAUTIONS
“Trichloroethylene and 1,1,1 trichloroethylene are toxic materials and
strict adherence to instructions in Material Safety Data Sheets are to be
followed" Caution: Trichloroethylene and 1,1,1 trichloroethylene in the
presence of heat and moisture may form acids that are extreme corrosive”.
PREPARATION OF GOOCH CRUCIBLE
Assemble the filtering apparatus. Place filter pad into the gooch crucible,
moisten the pad with solvent and seat firmly in the bottom of the crucible
with light suction. Place in an oven at 110 ± 5°C (230 ± 9°F) for at least 20
minutes, cool in desiccators and weigh to the nearest 0.1 mg. Repeat the
drying and weighing until constant mass (± 0.3 trig) is obtained. Store in a
desiccator until ready for use.
SAMPLE PREPARATION
If the sample is not fluid, heat to any convenient temperature, but in any
case not more than 100°C or 180°F above the softening point.
 PROCEDURE
• Note safety precautions in Section 6. Transfer approximately 2 g of the
sample into a tared 25 ml. Erlenmeyer flask or other suitable container,
allow the container and its contents to cool to ambient temperatures
and weigh to the nearest 1 mg. Add 100 ml of the trichloroethylene or
1,1,1 trichloroethylene to the container in small portions with
continuous agitation until all lumps disappear and no undissolved
sample adhere to the container. Stopper the flask or otherwise cover
the container and set aside for at least 15 minutes. Normally the
temperature at which this test is run is not critical and it may be
performed at the laboratory air temperature. For referee tests,
however, the flask and sample in solution shall be placed in a water
bath maintained at 37.8 ± 0.25°C (100 ± 0.5°F), for 1 hour before
filtering.
• Place the previously prepared and weighed Gooch crucible in the
filtering tube.
• Wet the filter pad with a small portion of clean solvent and decant the
solution through the filler pad of the crucible with light suction.
• When the insoluble matter is appreciable, retain as much
of it as possible in the container until the solution has
drained through the filter pad. Wash the container with a
small amount of solvent and, using a stream of solvent
from a wash bottle, transfer all insoluble matter to the
crucible. Use a "policeman" if necessary to remove any
insoluble, matter adhering to the container, rinse the
policeman and the container, thoroughly wash the
insoluble -matter in the crucible with solvent until the
filtrate is substantially color less, then apply strong suction
to remove the remaining solvent. Remove the crucible
from the tube and wash the bottom free of any dissolved
matter.
• Place in an oven at 110 ± 5°C (230 ± 9°F) for at least 20
min. Cool in a desiccator and weigh to the nearest 0.1 mg.
Repeat the drying and weighing until constant weight (±
0.3 mg) is obtained.

• Fibre glass filter pads should be used only one time.

 CALCULATIONS
• Calculate either the total percentage of insoluble
matter or the percentage of the sample soluble in the
solvent used as follows:

Insoluble, percent = A/B x 100

Soluble, percent = 100- (A/B x 100)
where,
A = total weight insoluble, and
B = total weight of sample.

• For percentage of insoluble less than 1.0, report to the

nearest 0.01 percent; for percentage of insoluble 1 .0
or more report to the nearest 0.1 percent.
 Experiment No.6
LOSS ON HEATING OF OIL AND ASPHALTIC COMPOUNDS
AASHTO DESIGNATION: f 47-83 (1993)
(ASTM DESIGNATION: D 6-80)
• SCOPE:
This method covers the determination of the loss in mass
(exclusive of water) of oil and asphaltic compounds when
heated as herein after prescribed.
• REFERENCED DOCUMENTS:
ASTM Standards:
E1 Specification for ASTM Thermometers
E 145 Specification for Gravity-Convection
and forced-Ventilation Ovens
 APPARATUS
• Oven: The oven shall be electrically heated and shall conform to the
performance requirements of ASTM specification E 145. The oven shall be
rectangular with minimum interior dimensions of 350 mm (13 in.) in each
direction. The oven shall have in front a tightly fitting hinged door, which
shall provide a clear opening substantially the same as the interior height
and width of the oven. The door may contain a window with dimensions of
a least 100 by 100 mm (4 by 4 in), and with two sheets of glass separated by
an air space, through which a vertical thermometer located in the oven,
may be read without opening the door, or the oven may be provided with
an inner glass door, through which the thermometer may be observed on
opening the outer door momentarily.
• Rotating Shelf: The oven shall be provided with a circular metal shelf having
a minimum diameter of 250 mm (9.8in.). The shelf shall suspended by a
vertical shaft and centered with respect to the horizontal interior
dimensions. The shelf shall be provided with a mechanical means for
rotating it at the rate of 5 to 6 rpm. The shelf shall be vertically located as
close to the center of the oven as permitted by compliance with the
requirements regarding to thermometer placement.
• Thermometer (having a range from 155 to 170°C)
• Container
 PROCEDURE:
• First test the material under examination for water and if water
is present, remove it by suitable methods of dehydration before
subjecting the material to the loss on heating test, or obtain
another sample that is free from water.
• Place 50.0 ±0.5 gm of the sample of the water free material in a
container, cool the sample to room temperature and weigh to
the nearest 0.01 gm. Bring the oven to a temperature of
163°C(325°F) and place the container with the weighed sample
on recesses if the recommended shelf is used. Close the oven
and rotate the shelf during the entire test at a rate of 5 to 6
rpm. Maintain the temperature at 163 ± 1°C (325±1.8°F) for 5
hrs, start counting the time when the temperature reaches
162°C, and in no case shall the total time that a sample is in the
oven be more than 5h and 15 min. At the conclusion of the
heating period, remove the sample from the oven, cool to room
temperature, and weigh to the nearest 0.01 gm.
 CALCULATIONS:
Calculate the percentage loss to the nearest second
decimal as follows:
%loss= [(A-B)/A']*100

where,
A = initial weight of the container plus sample
B = final weight of the container plus sample
after heating.
A'= initial weight of the sample
 Reproducibility of Results
Up to 5 percent loss in mass the results obtained may be
considered as correct within 0.5. Above 5 percent loss in mass,
the numerical limit of error increases 0.01 for every 0.5 percent
increase in loss by volatilization as follows:

Volatilization Loss Numerical True Volatilization

(%) Correction Loss; (%)
5.0 ±0.50 4.50 to 5.55
5.5 ±0.51 4.99 to 6.01
6.0 ±0.52 5.48 to 6.52
10.0 ±0.60 9.40 to 10.60
15.0 ±0.70 14.30 to 15.70
25.0 ±0.90 24.10 to 25.90
40.0 ±1.20 38.80 to 41.20
 Experiment No. 4
SOFTENING POINT OF BITUMINOUS MATERIALS
(RING-AND-BALL METHOD)
AASHTO DESIGNATION: T 53-92
(ASTM DESIGNATION: D 36-89)
• Scope
• The ring and ball softening point is extensively used to evaluate the
consistency of bituminous binders. It is a very simple one, consisting of
placing a 3/8 in. diameter steel ball on a binder sample placed in a steel
ring and immersed in a water bath. Heat is applied to the water and its
temperature is raised until a value is reached when the test sample has
become sufficiently soft to allow the ball, enveloped in binder to fall
down. The water temperature at which this occurs is called the ring
and ball softening point.
• The softening point is not a melting point, bituminous binder do not
melt but instead gradually change from semi-solids to liquids on the
application of heat. It is useful for determining the temperature
susceptibilities of bitumens which are; to be used in thick films, such as
in crack fillers. When two bitumens have the same penetration value,
the one with the higher softening point is normally less susceptible to
temperature changes.
 Apparatus and Materials
• Ring-A brass ring 15.875 mm(5/8 in.) inside diameter and 6.35 mm (1/4 in.)
depth, thickness of wall, 2.38 mm(3/32) in. this ring shall be attached in a
convenient manner to a brass with (diameter 1.85 mm = 0.072 in.)
• Ball - A steel ball 9.53 mm (3/8 in.) in diameter having a mass of 3.50 ± Q.05
g.
• Container - A glass vessel, not less than 8.5 cm (3.34 in.) in diameter and
measuring 10.5 cm (4.13 in.) in depth from the bottom of the flare (a 600
ml beaker, low form, meets this requirement).
• Thermometer - ASTM Low Softening point Thermometer having a range of -
2 to + 80°C or 30°C to 180°F, is specified.
• Reagents and Materials:
• Bath liquids
• Freshly boiled distilled water.
• USP Glycerin, or
• Ethyle Glycol, with a boiling point between 195 and 197°C (383 and 387°F).
 PREPARATION OF SAMPLE
Melt and thoroughly stir the sample avoiding incorporating air bubbles in the
mass, and then pour it into the ring. The ring, while being filled, should rest on
a brass plate which has been amalgamated to prevent the bituminous material
from adhering to it. Allow the excels material to cool for 1 hr. then cut it off
cleanly with a slightly heated knife.
PROCEDURE FOR MATERIALS HAVING SOFTENING POINTS 80°C (176°F) or
BELOW:
• Fill the glass vessel to a depth of substantially 8.25 cm (3.25 in.) with fleshly
boiled, distilled water at 5°C (41°F).
• Suspended the ring containing the sample in the water so that the lower
surface of the filled ring is exactly 2.54 cm (1'in.) above the bottom of the
glass vessel and its super surface is 5.08 (2 in), below the surface of the
water.
• Place the ball in the water but not on the specimen.
• Suspend the thermometer so that the bottom of the bulb is level with the
bottom of the ring and within 0.635 cm (3/4 in.) but not touching the ring.
Maintain the temperature of the water at 5°C(41°F) for 15 min.
• With suitable force, place the ball in the center of the upper surface of the
bitumen in the ring, this completing the assembly.
• Apply the heat in such manner that the temperature of the water is raised
5°C (9°F) each minute.
 REPORT
Report the temperature recorded by the thermometer at
the instant the bituminous material touches the bottom of
the glass vessel as the softening point. No correction shall
be made for emergent stem of the thermometer.
• PERMISSIBLE VARIATION IN RISE OF TEMPERATURE
The rate of rise of temperature shall be uniform and shall
not be averaged over the period of the test. The maximum
permissible variation for any minute period after the first
three 3 minutes shall be 0.5°C (0.9°F). All tests in which the
rate of rise in temperature exceeds these limits shall be
rejected.
 Experiment No. 7
DUCTILITY OF BITUMINOUS MATERIALS
AASHTO DESIGNATION: T 51.-93
(ASTM DESIGNTIQN: D 113-79)
SCOPE
The ductility of a bituminous material is
measured by the distance to which it will elongated
before breaking when two ends of a briquette
specimen of the material, of the for n describe in
Section 2, are pulled apart at a specified speed and
at a specified temperature. Unless otherwise
specified, the test shall be made at a temperature
of 77 ± 0.9°F (25 o ± 0.5°C) and with a speed of 5
cm/min. + 5.0 percent. At other temperatures the
speed should be specified.
 APPARATUS
Mould - the mould shall be similar in design to that shown in Fig. 1.
Dimensions shown n Fig. 1 shall be as given with the permissible
variations indicated. The mould shall be made of brass, the ends b and
b' being 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 briquet specimen having the following
dimensions:
Total length 7.45 to 7.55 cm
Distance between clips 2.97 to 3.03 era
Width at mouth of clip 1.98 to 2.02 cm
Width at minimum cross section (halfway between clips)
Thickness throughout 0.99 to 1.01cm
• Water Bath
• Testing Machine
• Thermometer
A Distance between crnters 111.5 to
113.5mm
B Total length of briquet 74.5 to 75.5 mm
D Width at minimum cross 9.9 to 10.1 mm
section
T Thickness 9. 9 to 10.1 mm

FIGURE 1 Mold for Ductility Test Specimen

 Procedure
• Moulding Test Specimen - Heat the sample with care to prevent local
overheating until it has become sufficiently fluid to pour. Strain the melted
sample through a No. 50 alive conforming to ASTM Specification E-l1, for
Wire cloth Sieves for Testing Purposes, and. after a thorough stirring pour
it into the mould. Assemble the mould on a brass, plate and, to prevent
the material under test from sticking, thoroughly amalgamate the surface
of the plate and interior surface of the sides a and a', Fig. 1, of the mould
or coat with a mixture of glycerin and dextrin, talc, or china clay. The plate
upon which the mould is placed shall be perfectly flat and level so that the
bottom surface of the mould, will touch it throughout. In filling the mould,
take care not to disarrange the parts and thus distort the briquette. In
filing, pour the material in a thin stream back and forth form end to end of
the mold until the mould is more than level full. Let the mould containing
the material cool to room temperature FOR a period of from 30 to 40 min.
and then place it in the water bath maintained at the specified
temperature of test for 30 min.; then cut off the excess bitumen with a
hot straight edged putty knife or spetula to make the mold just level full.
 Procedure
• Keeping Specimen at Standard Temperature - Place the brass plate
and mould, with briquette specimen, in the water bath and keep at
the specified temperature for a period of from 85 to 95 min. Then
remove the briquette from plate, detach the side, pieces, aid
immediately test the briquette.
• 3.3 Testing - Attach the rings at each end of the clips to the pins or
hooks in the testing machine and pull the two clips apart at a
uniform speed as specified until the briquette ruptures. A variation
of + 5 percent from the speed specified will be permissible Measure
the distance in centimeters through which the clips have been
pulled to produce rupture. While, the test is being made, the water
in the tank of the testing machine shall cover the specimen both
above and below it by a least 2.5 cm and shall be kept continuously
at the temperature specified within + 0.9°F (0.5°C).
 REPORT:
• A normal test is one in which the material between the clips pulls
out to a point or thread until rupture occurs at the point where the
thread has practically no cross-sectional area. Report the average
of three normal tests as the ductility of the sample
• 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 bath by the
addition of either methyl alcohol or sodium chloride so that the
bituminous material neither comes to the surface of the water, nor
touches the bottom of the bath at any time during the test.
• If a normal tests not obtainable on three terms, report the ductility
as being unobtainable under the conditions of the test.