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Experiment 2:
Partially Miscible Liquids:
Determination of Mutual Solubility
I. Introduction
The objective of the experiment is to determine the solubility of two partially miscible
liquids, construct the mutual solubility curve for the pair and determine their critical solution
temperature.
Miscibility means how completely two or more liquids dissolve in each other. It is a
qualitative rather than quantitative observation—miscible, partially miscible, not miscible.
Like any other solubility phenomenon, miscibility depends on the forces of attraction
between the molecules of the different liquids. The rule of thumb "like dissolves like" means
that liquids with similar molecular structures, in particular similar polarity, will likely dissolve
in each other. (Polarity means the extent to which partial positive and negative charges
appear on a molecule, because of the type and arrangement of its component atoms.)
However there are some substances with varying polarity like water which will play a vital
issue on how solute will dissolve in it.
Volume vs Solute
The above diagram shows the solubility trend mostly occuring in solid-liquid
solutions. The level of concentration of the dissolved solute can be classified as saturated,
supersaturated and unsaturated solution. Saturated solution is attained when the maximum
amount of solute a solvent can dissolve has already been reached. The saturation point of
a solution is represented graphically by points along the straight line. On the other hand,
unsaturated solutions are those when the maximum amount of solute dissolved is not yet
reached by the solvent. The unsaturated region is represented by the lower region of the
graph(below the line).Lastly, a supersaturated solution is attained when the maximum
amount of solute is exceeded and precipitation are evident. The supersaturated solution
takes the section above the saturation line. This however can be altered depending on the
temperature on which dissolving takes place. For solubility depends highly on temperature.
If the phase rule is applied in this two-phase mixture, two variables are needed to be
specified to describe the system completely. The phase rule calculation is shown below.
P=c–p+2
=2–2+2
=2
II. Methodology
Preliminary procedures were done before the actual experiment. The density of
phenol was obtained from literature and the amount of water required to prepare 5% to 95%
phenol at 5% increment, starting with 10 mL phenol in each proportion, was calculated.
95% phenol-5% water by weight mixture was prepared based on 10 mL phenol. The
mixture was heated with mild stirring until the cloudiness disappeared, the temperature of
which was recorded. The mixture was then cooled with mild stirring until the cloudiness
reappeared, the temperature of which was recorded. The process was repeated until fairly
constant readings were observed. Water was added to make 90% phenol and 10% water.
The procedure was repeated until 55% phenol. For 5% to 50%, 5 mL phenol was initially
used.
III.Discussion of Results
Different changes were observed and noted in the experiment. After the 95% phenol-
5% water by weight solution was prepared, the mixture was heated in a water bath with mild
stirring and recorded its constant temperature until the cloudiness of the solution
disappeared and cooled instantly until the cloudiness reappeared. It is observed that the
turbidity, which signifies the partial immiscibility of the liquids, is highly dependent on
concentration of mixture and temperature. If the mixture is highly concentrated to either
water or phenol, after the mild stirring in room temperature there would be no visible
cloudiness observed. It is seen in the 5% and 95% phenol-water solution that no cloudiness
appeared because both exhibits almost a pure compound. In the 80, 85, and 90% it is noted
that there was cloudiness before heating the mixture and required a certain heating
temperature to make the mixture miscible. In the cooling process, however, it is observed
that no cloudiness reappeared. The reason for this is that just a certain small amount of heat
can make the solute and solvent miscible but once the equilibrium is established, the
mixture is hard to separate into two components. An account to the said results is seen on
Table I.
Table I: Values of the temperature for each increment
HEATING COOLING
% by Weight
Temperat Temperat
Phenol-Water
ure ure
Solution
(ºC) (ºC)
5 No change No change
10 40 38
15 58 56
20 65 63
25 66 64
30 66 65
35 66 65
40 66 65
45 66 66
50 66 64
55 64 58
60 63 58
65 55 54
70 45 42
75 41 30
80 34 No change
85 30 No change
90 29 No change
95 No change No change
The heating and cooling temperatures gradually increase but as it reached a certain
constant high temperature, it gradually decreases. It is seen on the 45% mixture that the
heating and cooling temperature is the same. It is where, after heating the solution and
putting in the ice bath, the cloudiness immediately reappears.
The temperature versus percentage by weight phenol mixture was plotted in order to
determine the critical solution temperature of the mixture and is seen in Graph 1.
Graph 1
To clearly see the single and double-phase regions, the lines were set to polynomial
trend line forming smooth curves. The dotted lines represent the temperature at which the
cloudiness of the mixture disappeared in the heating step and said to be the state where the
mixture is single-phase. The dashed lines represent the temperature at which the cloudiness
reappeared in the cooling step and said to be the point in which the mixture began to
separate and became double-phase. It is seen in the graph that there would be a region
created in the intersection of the dotted and dashed line. This region is a single-phase
region in which the phenol and water are miscible. Beyond this region would be a double-
phase in which the mixture is said to be partially miscible or immiscible.
Critical solution temperature is the temperature which will lead to separation of the
mixture into two distinct liquid phases. This is denoted by the intersection of the polynomial
trend line of the heating and cooling temperature. The critical temperatures at which the
lines intersect are 63ºC and 66ºC.
IV.Answers to Questions
1. Two types of liquid-liquid critical points are the upper critical solution temperature, or,
which denotes the warmest point at which cooling will induce phase separation, and
the lower critical solution temperature, which denotes the coolest point at which
heating will induce phase separation. Based on Graph 1, the maximum temperature
is 66ºC and the minimum critical solution temperature is 63ºC.
2. The different temperature readings have very small differences. Thus, the
temperature readings were constant.
3. The high phenol concentration of percentage of phenol-water mixture solidifies
during cooling process mainly because of phenol’s freezing point. At 41˚C, phenol
forms into a solid that can be liquefied by a very small amount of water. Thus, a high
concentration solution of phenol with water would solidify on lower temperatures.
4. Given an unknown solution of the components, its concentration will be known by the
use of the mutual solubility plot/graph. The composition of a layer can be determined
by getting the critical solution temperature experimentally and plotting the point on
the graph. The weight percentage could be obtained at the point where in the
temperature intersects the curve.
I. Conclusions
It is also concluded that in the plot of the mutual solubility curve, a region was
enclosed and signified the single-phase stage of the mixture. Beyond that region, the
mixture is of double-phase. The intersection of the trend lines for heating and cooling would
be the critical solution temperature of the mixture and was found to be approximately 63ºC
and 66ºC.
II. References
[1] Atkins, Peter & De Paula, Julio. Atkins’ Physical Chemistry, 7th ed. (Oxford University
Press Inc., New York, 2002.)
[2] Barrow, Gordon M. Physical Chemistry, 6th ed. (The McGraw-Hill Companies Inc., USA,
1995) pp. 327-330
[3] Daniels, Farrigton and Alberty, Robert. Physical Chemistry, 2nd ed. (John Wiley & Sons,
Inc., USA, 1961) pp. 241-243
[5] http://science.jrank.org/pages/4382/Miscibility.html
[4] http://www.citycollegiate.com/chapter3d.htm
[6] http://www.sciencebyjones.com/solubility.htm