Experiment 3

Date: 11/12/2017
Experiment number: 03
Experiment: solubility relation in a three component system
INTRODUCTION
A phase diagram shows the phase existing in equilibrium at any given condition. According
to the phase rule, a maximum of four intensive variables (intensive properties) must be
specified to completely define the state of three-component system. In this system, we can
find out that the degree of freedom is 4 which are temperature, pressure, and concentrations
of the two of the three component. At constant temperature and pressure, the composition
of a ternary system can be presented in the form of triangular coordinates.
Each of three corners or apexes of the triangle represent 100% weight of one component (A,
B or C). As a result, that same apex will represent 0% of the other two components. For
example, the top corner point represents 100% B. Each side of the triangle represent a binary
mixture where two components mixed together and any line drawn parallel to one of the
side shows the percentage of a particular component. By dividing each line into 100 equal
units, the location of a point along the line can be directly related to the percent
concentration of one component in two-component system. In going along a line bounding
the triangle so as to represent the concentration in a two-component system, it does not
matter whether we proceed in a clockwise or counterclockwise direction around the triangle,
provide we are consistent. If a line is drawn through any apex to a point on the opposite side
then all systems represented by points on such a line have a constant ratio of two
components, in this case A and B.
Solubility differ when there are different components mixing together. When the third
component is added to a pair of miscible liquid, it may affect the mutual solubility, if the third
component is more soluble in one of the liquids than in the other, then the miscibility
between that pair of liquids decreases. But, if the third component is soluble in both
components, then the mutual solubility will increase.
PROCEDURE
Approximately 20 g mixture of 𝐶𝐻2 𝐶𝑙2 and acetic acid containing 10, 20, 40, 60, 80 and 90 %
was prepared by weight of𝐶𝐻2 𝐶𝑙2 . The calculated volumes were run in from a burette
(Density of 𝐶𝐻2 𝐶𝑙2 = 1.33 g/𝑐𝑚−3 , acetic acid = 1.05 g/𝑐𝑚−3 ). Solutions were titrated with
water small amounts at time with vigorous shaking until the first appearance of turbidity. The
temperature was recorded.
In separate funnels, three different mixtures of dichloromethane, acetic acid and water were
prepared from within the bimodal curve, which are known to separate into two layers.
Solutions were shake vigorously and allowed the two layers to separate out. Carefully each
layer was run off and weighted. A small aliquot was removed, 1 ml was weighted, and 50 ml
of water was added and titrated with the standard sodium hydroxide solution using
phenolphthalein as indicator.
RESULTS
Results of titration between water and mixture (𝐶𝐻2 𝐶𝑙2 and acetic acid)
Percentage Volume of Volume of Initial burette Final burette Consumed

of 𝐶𝐻2 𝐶𝑙2 𝐶𝐻2 𝐶𝑙2 / 𝑐𝑚3 acetic acid reading/ 𝑐𝑚3 reading/ 𝑐𝑚3 volume of
/ 𝑐𝑚3 water/ 𝑐𝑚 3
10% 1.50 17.14 0.00 ----------------- -----------------

20% 3.01 15.20 0.00 20.90 20.90
40% 6.03 11.42 0.00 6.50 6.50
60% 9.05 7.61 0.00 2.20 2.20
80% 12.07 3.80 0.00 0.50 0.50
90% 13.58 1.90 0.00 0.30 0.30
Results of separations and titrations
1st sample (Organic layer=6.00 𝑐𝑚3 & aqueous layer=4.00 𝑐𝑚3 )

Organic layer
Weight of Weight of Initial Final burette Consumed
beaker beaker with burette reading volume of
3 𝑁𝑎𝑂𝐻(𝑎𝑞)
without organic layer reading / 𝑐𝑚
organic /g / 𝑐𝑚3 / 𝑐𝑚3
layer/ g
101.64 110.68 0.00 54.20 54.20
Weight of 1ml organic layer = 1.76 g.
Aqueous layer
without aqueous reading / 𝑐𝑚
aqueous layer/ g / 𝑐𝑚3 / 𝑐𝑚3
layer/ g
101.67 109.56 0.00 86.60 86.60
Weight of 1ml aqueous layer = 1.52 g.
2nd sampler (Organic layer=5.00 𝑐𝑚3 & aqueous layer=5.00 𝑐𝑚3 )
Organic layer
without organic layer reading / 𝑐𝑚
organic /g / 𝑐𝑚3 / 𝑐𝑚3
layer/ g
101.67 109.56 0.00 76.20 76.20
Weight of 1ml organic layer = 1.72 g.
Aqueous layer
without aqueous reading / 𝑐𝑚
aqueous layer/ g / 𝑐𝑚3 / 𝑐𝑚3
layer/ g
104.08 109.79 0.00 136.80 136.80
Weight of 1ml aqueous layer = 1.52 g.
CALCULATIONS
Density of water = 1 g/𝑐𝑚3 .
Weight of Weight of Weight of Total Weight percentage %
𝐶𝐻2 𝐶𝑙2 / g 𝐶𝐻3 𝐶𝑂𝑂𝐻 𝐻2 𝑂/ g weight/ g 𝐶𝐻2 𝐶𝑙2 % 𝐶𝐻3 𝐶𝑂𝑂𝐻% 𝐻2 𝑂%
/g
2 18 -------------- -------------- -------------- ---------------- --------------
4 16 20.90 40.9 9.77 39.11 51.10
8 12 6.50 26.50 30.18 45.28 24.52
12 8 2.20 16.20 74.07 49.38 13.58
16 4 0.50 20.50 78.04 19.51 2.43
18 2 0.30 20.30 88.66 9.85 1.47
1st Sample
 organic layer
Concentration of 𝑁𝑎𝑂𝐻(𝑎𝑞) = 0.1 𝑚𝑜𝑙𝑑𝑚−3
Consumed volume of 𝑁𝑎𝑂𝐻(𝑎𝑞) = 54.20 𝑐𝑚3
0.1 𝑚𝑜𝑙
So, consumed moles of 𝑁𝑎𝑂𝐻(𝑎𝑞) = ⨯54.20 𝑐𝑚3
1000𝑐𝑚3
= 5.420⨯10−3 mol
𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) + 𝑁𝑎𝑂𝐻(𝑎𝑞) ⟶ 𝐶𝐻3 𝐶𝑂𝑂−+ 𝑁𝑎(𝑎𝑞) + 𝐻2 𝑂(𝑎𝑞)
According to this reaction stoichiometry
Ratio between 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) and 𝑁𝑎𝑂𝐻(𝑎𝑞) = 1 : 1
So moles of react mol𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) = 5.420⨯10−3 mol
Molar mass of 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) = 60.05 g/mol
60.05 𝑔
So, weight of react 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) = ⨯5.420⨯10−3 mol
1 𝑚𝑜𝑙
= 0.325 g
Weight of 1ml organic layer = 1.76 g
0.325 𝑔
So, weight percentage of 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) in organic layer = ⨯100
1.76 𝑔
= 18.4%
 Aqueous layer
0.1 𝑚𝑜𝑙
1000𝑐𝑚3
= 8.660⨯10−3 mol
60.05 𝑔
1 𝑚𝑜𝑙
= 0.520 g
Weight of 1ml aqueous layer = 1.52 g
0.520 𝑔
So, weight percentage of 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) in aqueous layer = ⨯100
1.52 𝑔
= 34.2%
2nd sample
 Organic layer
0.1 𝑚𝑜𝑙
1000𝑐𝑚3
= 7.620⨯10−3 mol
60.05 𝑔
1 𝑚𝑜𝑙
= 0.381 g
Weight of 1ml organic layer = 1.72 g
0.381 𝑔
So, weight percentage of 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) in organic layer = ⨯100
1.72 𝑔
= 22.1%
 aqueous layer
0.1 𝑚𝑜𝑙
1000𝑐𝑚3
= 13.68⨯10−3 mol
60.05 𝑔
1 𝑚𝑜𝑙
= 0.821 g
Weight of 1ml aqueous layer = 1.52 g
0.821 𝑔
So, weight percentage of 𝐶𝐻3 𝐶𝑂𝑂𝐻(𝑎𝑞) in aqueous layer = ⨯100
1.52 𝑔
= 54.0%
DISCUSSION
Phase diagram is a diagram representing the limits of stability of the various phase in
chemical system at equilibrium, with respect to variables of parameters such as
concentration and temperature. Therefore, to define the state of each phase, knowledge of
several variables is need and essential. Thus, regarding to this issue, phase rule is formulated.
Phase rule is used to relate the effect of the minimal number of independent variables upon
the various phases that can exist in an equilibrium system that containing a given number of
components. The phase rule is expressed as following:
F=C–P+2
Where,
F = Number of degree of freedom
C = Number of components
P = number of phases
By using phase rule equation in this experiment, the number of degree of freedom, F can be
determined. In this experiment, we use three component as each components are composed
of different elements. At the beginning of the experiment, we mixed dichloromethane and
acetic acid which eventually resulting only one liquid phase (homogenous solution). Thus the
F obtain this experiment is 4 (as F = 3 – 1 + 2) for a non-condensed system. The degree of
freedom at the beginning of the experiment is comprised of temperature, pressure and the
each of concentration of components. As water added to the system, F will be reduced to 2
(as F = 3 – 3 + 2) for a condensed system as the number of phases are increased from one
liquid phase to two liquid phase and addition of one vapour phase. As the number of
components increase, the number of degree of freedom also will be increased. However, as
F is increased, the system will become more complex, it becomes necessary to fix more
variable to define the system. Ironically, the greater the number of phases in equilibrium,
fewer the degree of freedom.
On this experiment, we are using different components, which is dichloromethane and acetic
acid and water. It is important to know the properties of dichloromethane and acetic acid
solubility in water. Both dichloromethane and acetic acid different properties in water. Acetic
acid is soluble in water while dichloromethane is not soluble in water. At the beginning of the
experiment, we mixed an amount of dichloromethane and acetic acid together. Both are
forming a clear mutual miscible solution and forming homogenous solution (one liquid
phase). But after adding an amount of water, the solubility of the clear mutual miscible
solution are disrupted. The clear solution turns cloudy which indicates the solution does not
longer miscible to each other and starts to form two layer (two liquid phase) as resulting from
the different degree of solubility of dichloromethane and acetic acid in water. The addition
of water (third component to miscible liquids, which is dichloromethane and acetic acid can
change their mutual solubility. As water is more soluble in acetic acid compare to
dichloromethane, the mutual solubility of dichloromethane and acetic acid is decreased.
However, if water is soluble in both of liquids, mutual solubility will increased. Thus, when
water is added to the mixture of dichloromethane and acetic acid, the mutual solubility will
increased until it reached a point where the mixture becomes homogenous solution. This is
proved in the experiment, as more amount of water is needed turn the clear miscible solution
into cloudy immiscible solution. In addition, all of the component in this experiment can be
a miscible solution when they are mixed together if and only if correct proportion of each
components is determined.
Parallax-this error can occur whenever there is some distance between the measuring the
scale and the indicator used to obtain a measurement. If the observer’s eye is not squarely
aligned with the pointer and scale, the reading may be too high or low.
We must ensure that there are no bubbles of the solution of inside the burette or pipette
because it can makes readings errors.

Experiment 3

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Experiment 3

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Date: 11/12/2017

Percentage Volume of Volume of Initial burette Final burette Consumed

10% 1.50 17.14 0.00 ----------------- -----------------

Results of separations and titrations

1st sample (Organic layer=6.00 𝑐𝑚3 & aqueous layer=4.00 𝑐𝑚3 )

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