Solubility Test for Asphalt Materials

Introduction:
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.
Objectives:
Objective of this test is to determine the degree of solubility in trichloroethylene of asphalt
materials having little or no mineral matter.
Apparatus:
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.

Figure 1 Solubility Test Apparatus.

Procedure:
Sample Preparation
1) The Gooch crucible plus one thickness of the glass fiber pad was placed in an oven at 110
50 C for 15 min, was allowed to cool in a desiccator, and then the mass was determined
to the nearest 0.1 mg. This mass was designated as A. The desiccator was stored in until
ready for use.
2) If the sample was not fluid, it was heated to any convenient temperature, but in any case
not more than 1110 C above the softening point. 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 0.30 C for 1 hour before filtering.
Test Procedure
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.

Observation:
A = mass of crucible and filter = 17.38 g
B = mass of sample

= 2.15 g

C = mass of crucible, filter and insoluble material = 17.39 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 = 17.39 17.38
2.15

x 100

= 0.47 %
% Soluble = 2.15 (17.39 17.38)
2.15
= 99.53 %

x 100

Discussion:
1) What is the importance of the solubility value of a bitumen sample?
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.
2) What are the other methods available to find the solubility of bitumen?

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 earths ozone layer, solubility in n-Propyl Bromide has introduced by ASTM. ASTM
D 7553.

3) What is the purpose of doing a solubility test?

The purpose of the doing a solubility test is to detect contaminations in asphault cement
to complied with specifications.
4) What are the modifications can propose to the solubility test?
It is better to use different solution since the trichloroethylene has identified as a
carcinogen and contribute to the depletion of the earths ozone layer.