Jordan University of Science and Technology

Civil Engineering Department

Highway laboratory

Student Name: abdallah alhassan ID: 120034

Experiment number : 9,10 and 11

Experiment Name : flash point , solubility and Specific Gravity of Bitumen

Instructor: Eng.khaled albalas TA Name:farah jawdat

Submission Date: 11/6/2019 SEC# 5

Evaluation Elements Max Grade

grade
1 Cover page 5
2 Abstract 5
3 Introduction 5
4 Material and equipment 5
5 Objectives 5
6 Test Procedure 5
7 Results and data analysis 20
8 Discussion 15
9 Conclusions 10
10 References 5
11 Presentation of data in tables and figures 5
12 Appendix 5
13 Spilling and clarity sentences 5
14 Overall appearance 5
Total 100
  Abstract

For flash point )

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 vapours when a small flame is brought in contact with the vapours of a
bituminous product, gradually heated under standardized condition. When bituminious material is
further heated to a high temperature, the material itself catches and continues to burn, the lowest
temperature causing this is the fire point. This condition is very hazardous and it is therefore
essential to qualify this temperature for each bitumen grade.

Flash point: The flash point of a material is the lowest temperature at which the vapour of
substance momentarily takes fire in the form of a flash under specified condition of test.
Fire point: The fire point is the lowest temperature at which the material gets ignited and burns
under specified condition of test.
As shown and discussed below the flash point and the firing point are 320 and 325 respectively.

For solubility test )

• In the standard test for bitumen content (ASTM D4), a small sample of about 2 g of the
asphalt is dissolved in 100 ml of carbon disulfide and the solution is filtered through a
filtering mat in a filtering crucible. The material retained on the filter is then dried and
weighed, and used to calculate the bitumen content as a percentage of the weight of the
original asphalt.
• Due to the extreme flammability of carbon disulfide, solubility in trichloroethylene, rather
than solubility in carbon disulfide, is usually used in asphalt cement specifications. The
standard solubility test using trichloroethylene is designated as ASTM D 2042.
• The solubility test is used to detect contamination in asphalt cement. Specifications for
asphalt cements normally require a minimum solubility in trichloroethylene of 99.0
percent.
• The values we get from this experiment is 98.5% for soluble and 1.5 insoluble .
For Specific Gravity of Bitumen)
The specific gravity is an important property that is required for the design of concrete
and bituminous mixes (does not influence its behavior). We will make the pycnometer
clean, dry, empty and we will weight it, then we filled it with a distill water and weight it
again, then it filled with liquid asphalt and cooled, then weighted with asphalt then filled
again with water to determinate the specific gravity of semi-solid bituminous materials,
asphalt cements, and soft tar pitches by use of a pycnometer.

In our test the value of the specific gravity was 0.955 , if we look at the standard value
which are (0.97 – 1.02) we will conclude that our sample is not accepted .

 Introduction

For flash point )

The properties of most importance in a road making aggregate are its resistance to crushing,
impact, abrasion and polishing, it s specific gravity and water absorption and its grading and
particle shape. As aggregate obtained from different sources differ considerably in their
constitution and properties, inevitably they differ also with their engineering properties. It is
necessary therefore, to carry out various tests on aggregates to ensure not only that undesirable
materials are excluded from highway pavements but also that the best available aggregates are
included. Also for bitumen and tars, the most careful specifications with regard to the design and
construction of a bituminous road surfacing are of little value if the properties of the bituminous
binder used in the design are not adequately controlled. To ensure that the material obtained has
the desired qualities, a number of tests have been devised which attempts to measure various
binder properties for particular reasons.
For solubility test )

This test method covers the determination of the degree of solubility in trichloroethylene of
asphalt materials having little or no mineral matter.

The portion that is soluble in trichloroethylene represents the active cementing constituents.

For Specific Gravity of Bitumen)

The specific gravity of semi-solid bituminous material, asphalt cements, and soft
tar pitches shall be expressed as the ratio of the mass of a given volume of the
material at 25 °C to that of an equal volume of water at the same temperature.
This test is done to determine the specific gravity of semi-solid bitumen road tars,
creosote and anthracene oil as per IS: 1202 – 1978.
  Material and equipment

For flash point )

a.
Cleveland Open Cup Apparatus:
- This apparatus consist of the cup, heating plate, test flame applicator,
heater and support.

Figure 3.a: Cleveland Open Cup Apparatus

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

c. Thermometer:
- A thermometer having a range – 6 to + 400ºC and conforming to the
requirements prescribed in specification.

Figure 3.c: Thermometer

For solubility test )

The following apparatus are required (Figure 1).

1) Gooch Crucible – glazed inside and outside with the exception of outside bottom surface.
The approximate dimensions shall be a diameter of 44 mm at the top, tapering to 36 mm at
the bottom, and a depth of 24 – 28 mm.

2) Glass Fiber Pad – 3.2 cm.

3) Filter Flask – heavy wall, with side tube, 250 or 500 ml capacity.

4) Filter Tube – 40 to 42 mm inside diameter.

5) Rubber Tubing or Adapter – for holding the Gooch crucible on the filter tube.

6) Erlenmeyer flask – 125 ml.

7) Oven – capable of maintaining a temperature of 110 ± 50 C.

For Specific Gravity of Bitumen)
• Pycnometer — glass, consisting of a cylindrical or conical vessel carefully ground to
receive an accurately fitting glass stopper 22 to 26 mm in diameter. The stopper shall be
provided with a hole 1.0 to 2.0 mm in diameter, centrally located in reference to the vertical
axis. The top surface of the stopper shall be smooth and substantially plane and the lower
surface shall be concave in order to allow all air to escape through the bore. The height of
the concave section shall be 4.0 to 18.0 mm at the center. The stopper Pycnometer shall
have a capacity of 24 to 30 ml, and shall weigh not more than 40 gram.
• •Water bath, constant-temperature, capable of maintaining the temperature within 0.1 °C
of the test temperature.
• •Thermometers — calibrated liquid-in-glass, total immersion type, of suitable range.
• •Balance — a balance conforming to the requirements of AASHTO
• •Distilled water — freshly boiled and cooled distilled water shall he used to fill the
Pycnometer and the beaker
  Objective

For flash point )

This experiment is to obtain the temperature level of the asphalt materials for flash
and fire point. This is to know its optimum temperature level. The flash point of cutback
asphalt is generally determined by use of a Tagliabue Open Cup apparatus, whereas the
Cleveland Open Cup is used for flash point determination on other asphaltic materials.

For solubility test )

Objective of this test is to determine the degree of solubility in trichloroethylene of asphalt

materials having little or no mineral matter.

For Specific Gravity of Bitumen)

To determine the specific gravity of many materials like semi solid bituminous materials,
asphalt cements, and soft tar pitches by use of a pycnometer.

Specific gravity of the asphalt cement changes when the asphalt cement expands on
heating, therefore specific gravity determination are useful in:

Making temperature, volume correction.

Determining the weight per unit volume of asphalt cement heated to its application
temperature.
  Test Procedure

For flash point )

1. Cleaned up and dried thoroughly all part of cup

2. The material is filled in the cup up to a filling mark. The lid is placed to close the cup in a
closed system.

3. All accessories including thermometer of the specified range are suitably fixed.
4. The bitumen sample is then heated.

5. The test flame is lit and adjusted in such a way that the size of a bleed is of 4mm diameter.
 6. Stirring is done at regular intervals

7. The test flame is lit and applied at intervals depending upon the expected flash and fire
points. First application is made at least 170C below the actual flash point and then at every
10C to 30C. The stirring is discontinued during the application of the test flame.

Test Procedure for solubility test )

1) Approximately 2 g of the sample was transferred into a tarred 125 ml Erlenmeyer flask or
other suitable container.

2) The sample was allowed to cool to ambient temperature and then determined the mass to
the nearest 1 mg. This mass was designated as “B”.

3) 100 ml of the trichloroethylene was added to the container in small portions with
continuous agitation until all lumps disappeared and no un-dissolved sample adhered to the
container.

4) The flask was stopper or otherwise the container was covered and set aside for at least 15
min.

5) The previously prepared and weighed Gooch crucible was placed in the filtering tube.

6) The glass fiber pad was wetted with a small portion of trichloroethylene and the solution
was decanted through the glass fiber pad of the crucible with or without light suction as
may be necessary.
7) When the insoluble matter was appreciable, retained as much of it as possible in the
container until the solution had drained through the mat.

8) The container was washed with a small amount of solvent and, using a stream of solvent
from a wash bottle, all insoluble matter was transferred to the crucible.

9) The insoluble matter in the crucible was washed with solvent until the filtrate was
substantially colorless, then strong suction was applied to remove the remaining solvent.

10) The crucible was removed from the tube, the bottom was washed free of any dissolved
matter, and the crucible was placed on top of an oven or on a steam bath until all odor of
the trichloroethylene was removed.

11) The crucible was placed in an oven at 110 ± 50 C for at least 20 min.

12) The crucible was cooled in a desiccator for 30 ± 5 min and its mass was determined to the
nearest 0.1 mg.

13) The drying and weighing was repeated until constant mass (± 0.3 mg) was obtained. This
mass was designated as “C”.
 For Specific Gravity of Bitumen)

1. The specific gravity bottle is cleaned, dried and weighed along with the stopper.

2. It is filled with fresh distilled water, stopper placed and the same is kept in water container for at
least half an hour at temperature 270C.
3. The bottle is then removed and cleaned from outside. The specific gravity bottle containing
distilled water is now weighed.

4. The bituminous material is heated to a pouring temperature and is poured in the above empty
bottle taking all the precautions that it is clean and dry before filling sample materials. The
material is filled up to the half taking care to prevent entry of air bubbles.

5. To permit an escape of air bubbles, the sample bottle is allowed to stand for half an hour at
suitable temperature cooled to 270C and then weighed.
6. The remaining space in the specific gravity bottle is filled with distilled water at 270C , stopper
placed and is placed in water container at 270C.
7. The bottle containing bituminous material and containing water is removed, cleaned from
outside and is again weighed.
From the weights taken, the specific gravity of bitumen can be found out.

Specific gravity of Bituminous Material

  results and data analysis

For flash point )

Flash point of bitumen (ºC) 320º

Fire point of bitumen (ºC) 325º

For solubility test )

A = mass of crucible and filter = 26.10 g

B = mass of sample = 2.00 g

C = mass of crucible, filter and insoluble material = 26.13 g

Calculations and result:

% Insoluble = C – A x 100
B

% Soluble = B – (C – A) x 100
B
Where;
A = mass of crucible and filter

B = mass of sample

C = mass of crucible, filter and insoluble material

(For percentages of insoluble less than 1.0, report to the nearest 0.01 %. For percentages of
insoluble 1.0 or more, report to the nearest 0.1 %)

Specimen Calculation:

% Insoluble = 26.13 – 26.10 x 100

2.00

= 1.5 %

% Soluble = 2.00 – (26.13 – 26.10) x 100

2.00

= 98.5 %
For Specific Gravity of Bitumen)

group Weight Specific gravity

Pycnometer Pycnometer Pycnometer Pycnometer
(A) + water (B) + asphalt + water +
(C) asphalt (D)
32.85 57.06 47.32 56.39

0.955

• Where,
• A = mass of Pycnometer = 32.85 g
• B = mass of Pycnometer filled with water = 57.06 g
• C = mass of Pycnometer partially filled with asphalt = 47.32 g
• D = mass of Pycnometer + asphalt + water = 56.39g

Result
Specific Gravity of bitumen = 0.955
  Discussion

For flash point )

From the laboratory test we did on the bitumen in Flash and Fire Point, the result we
obtained is, Flash temperature is 320oC, and the Fire Point temperature is 325oC. And comparing
to the recommended values is that the minimum value of flash point is 175oC for all grades of
bitumen. So, we can conclude that the bitumen we tested is suitable to be use for road
construction, because the Flash Point for our laboratory test is higher by 145 oC, not lower than
the recommended value by JRK Specification Value.

For solubility test )

Asphalt cements which use for HMA paving, should consist of almost pure bitumen.
Impurities are not actively cementing constituents and may be detrimental to asphalt
cement performance. Mineral impurities can be quantified by the solubility test.

Minimum solubility of 99% is specified in highway specifications. Knowing solubility

values, one can determine the purity of the asphalt cement which is being used relative to
the specification values ensuring undesirable materials are not blended into the product.

 Solubility in carbon disulfide

Asphalt consists primarily of bitumens which are high-molecular- weight hydrocarbons

soluble in CS2. The bitumen material is measured by means of its solubility in CS2, ASTM
D4.

 Solubility in trichloroethylene

Due to extreme flammability of CS2, solubility in trichloroethylene is specify in asphalt

cement specifications. ASTM D 2042.
  Solubility in n-Propyl Bromide

As the trichloroethylene has identified as a carcinogen and contribute to the depletion of

the earth’s ozone layer, solubility in n-Propyl Bromide has introduced by ASTM. ASTM
D 7553.

The purpose of the doing a solubility test is to detect contaminations in asphault cement
to complied with specifications.

It is better to use different solution since the trichloroethylene has identified as a

carcinogen and contribute to the depletion of the earth’s ozone layer

For Specific Gravity of Bitumen)

• The experiment has been performed successfully and the specific gravity
determined is 0.955 which isn’t in the range of 0.97 to 1.02. So it is not
acceptable. There were no bubbles in the pycnometer so chance of error was
eliminated and thus the value is correct.
  Conclusions

For flash point )

The sample is heated at a slow, constant rate. A small flame is directed into the cup.
The flash point has endured the test of time. In many applications of used oil analysis the
flash point test remains the method of choice in detecting certain contaminants and non-
conforming lubricant conditions. In other cases the flash point serves as a dependable
diagnostic tool or confirming test when a suspect condition has already been flagged.
And, like most everything in the world of oil analysis, success in using the flash point
depends on the careful adherence to such things as sample handling and test protocol.

For solubility test )

After we calculated the solubility in our specimen which turned out to be 98.5% we can
conclude that the specimen is not accepted by the standard values of the solubility test which as
mentioned above cannot be less than 99%.

For Specific Gravity of Bitumen)

 We must be careful to get at the beginning a dry pycnometer and try not to have
any water on the inside face of the pycnometer.

 Since the specific gravity varies with the temperature, test results are expressed in
terms of specific gravity at a given temperature for both the asphalt cement and
the water used in the test. And If we want to use the calibration at a different
temperature we need to set up the again calibration at that temperature.
 We should have a lower surface of the pycnometer stopper concave, because
when it be concave we can make sure that there is no air void (air bubbles ) in the
pycnometer.

 If we have bubbles at the surface or within the test sample we will get an error in
the results, especially in the weight of water were it will increase and that lead to
decrease the specific gravity.

 References

 Course slides
 Pavement Interactive web site
 ASTM
  appendix

 For flash point ) none

 For solubility test )

 For Specific Gravity of Bitumen)