Integrated Physical
Pharmacy & Pharmaceutics
I
Laboratory Manual
Experiment-Two
Three component system
Objective:
To study a three-component system: Carbon tetrachloride, Acetic acid and Water.
Background:
Pharmaceutical preparations, for a multitude of reasons, usually consist of two or more
components. Many of the preparations are combinations of immiscible materials to which a
blending agent must be added to produce a clear homogenous solution.
Blending is a term used to describe the mutual solubility of normally immiscible liquids in
the presence of an amphiphilics agent. Controlling the amount of blending agent used is an
important task. An insufficient quantity provides
Layering which can be extremely dangerous in pharmaceutical preparations and excessive
blending agent is undesirable due to side effects.
The tree component system is best described and interpreted by means of a phase rule and
phase diagram. At constant temperature and pressure, Gibb`s phase rule for a three-
component system is given by the following equation:
F= C-P
Where F is degree of Freedom, p is the number of phases at equilibrium, and C is number of
components comprising the system. The degree of freedom is defined as the least number of
variable factors (e.g., temperature, pressure and concentration, refractive index, viscosity etc.)
which must be arbitrarily fixed to have the condition of the system perfectly defined.
In order to assure a symmetrical representation of the three liquids in a ternary system an
equilateral diagram is employed. The following rules should be taken into account in
equilateral triangle diagram method.
1. In an equilateral triangle the sum of the distances from any given point to the three
sides, along the perpendicular to the sides, is equal to the height of the triangle.
2. Each apex equilateral triangle represents 100 percent by weight of one component and
zero for the others.
3. Each side is divided in to 100 equal parts and the distance from each apex to the
center of the opposite side of the equilateral triangle is divided into 100 equal parts.
4. The area within the triangle represents all the possible combinations of the three
components.
A very important feature of the phase diagram is the line which connects the compositions of
the two phases which are in equilibrium. The relative amounts of the two
Phase can be calculated by measuring the distance along the tie line from point representing
the gross composition of the mixture to the points representing the two solutions at
equilibrium. Usually, the tie lines are parallel to each other or to a side of the triangle. The
only case in which the tie lines are parallel is when the blending agent has the same degree of
solubility in either of the immiscible substances.
In carbon tetrachloride, water and acetic system, carbon tetrachloride and water are
immiscible liquids and acid is the blending agent,
Procedure:
The most accurate way to determine the three-component system of carbon tetrachloride,
glacial acetic acid and water is first to prepare nine 25 g samples of the two organic liquids
which are miscible. The following percentages of w/w are suggested 10, 20, 30, 40, 50, 60,
70, 80, and 90. A volumetric procedure could be employed with the aid of density values.
Titrate each sample while shaking with distilled water until the appearance of turbidity.
Although turbidity does not necessarily indicate a distance separation in to two phases, it
suggests an unstable state which will probably layer with time in to distance phases.
Upon completion of titration, signaled by turbidity of the system, the samples under
investigation no longer weights 25 g. The exact weight for practical consideration is 25 g plus
the volume of water added to produce turbidity (since 1 ml. weights approximately 1 g). The
quantity of each component in the samples will be calculated (% w/w) and the system will
be plotted.
Discussion:
1. Explain the pharmaceutical importance of determining the three-component system.
2. Discuss the lines of equilateral diagram and their application