Tuesday, 28 May 2013

PRACTICAL 1: PHASE DIAGRAM

Objective
To determine the phase diagram for ethanol/toluene/water system.

Introduction:
Ternary phase diagrams are 3 component systems. To construct a ternary diagram it is necessary to know the three binary systems for the three components. Ternary diagrams have a vertical temperature axis.
The actual ternary diagram may be represented as a three dimensional form or more commonly as a two dimensional projection of the liquids surface onto the base of the triangle created when the three binary diagrams are joined together. This irregular triangle is often transformed into an equilateral triangle to facilitate presentation and interpretation.

For experimental studies on ternary systems the liquids surface may be contoured with the temperature interval representing the contour interval. The fields indicated on the ternary diagram represent the primary phase fields, of solid phases in equilibrium with liquid, present on the liquids surface.
Straight lines which join the composition points of two phases whose primary phase fields share a common boundary curve are called Alkemade Lines. Thus the edges of the triangle are Alkemade Lines as they join the individual phases AB, AC and BC, which share a boundary curve. Alkemade lines are a specific type of tie line.

The phase relates the number of phases present in the system, the number of components which define the system and the degrees of freedom displayed the by the system at equilibrium.

Phase Rule:
P + F = C + 1

All compositions, e.g., bulk compositions, liquid compositions and compositions of solid phases on ternary diagrams are expressed in terms of the three end member components which define the system. These three components are located at apex of the triangle.

Each apex on the triangle of the ternary system represents 100% of the component at that apex. The side of the triangle, directly opposite the apex, represents 0% of the apex component. Compositions of points which lie along the outside edge of the triangle are simply a mixture of the two components at each end of the tie line, with 0% of the third component.

The composition of points which lie inside the area of the triangle can be determined using the Triangular Grid or Two Lines method. In this experiment, we will  focus on Triangular Grid method.
Triangular Grid method:

In this method a grid is constructed on the diagram. This grid is most commonly set up representing a 10% incremental increase in the components. To determine the composition of a point within the triangular area of the diagram a series of three lines are drawn through the point of intersect, with each line parallel to a side of the triangle. With these lines in place the percentage of each component in the composition of the point can readily be determined.




Figure 1: Example of a Triangular Grid


Chemicals:

Toluene
Distilled water
Ethanol
          




Apparatus:
Measuring Cylinder

Retort Stand

Burette


Conical Flask




Procedures:

 100cm3 mixtures of ethanol and toluene were prepared in sealed containers containing the following percentages (%) of ethanol :10, 25, 35, 50, 65, 75, 90 and 95. 20m1 of each mixture is prepared using a burette. Each mixture is titrated with water until    cloudiness   is observed due to existence of second phase

A little water was added and shaken well after each addition. The percentage was calculated based on the volume of each component when the second phase started to appear/separate.  A triple phase diagram is plotted based on the percentage of the components at the recorded temperature. The experiment is repeated for more accurate reading.

Results
Table 1:
Component/
Volume(cm3)








Ethanol
2.0
5.0
7.0
10.0
13.0
15.0
18.0
19.0
Toluene
18.0
15.0
13.0
10.0
7.0
5.0
2.0
1.0
Water (first experiment)
0.2
0.5
0.9
1.7
2.5
4.6
12.0
18.6
       (second experiment)
0.1
0.8
0.7
1.4
2.7
4.2
9.7
16.1
                         (average)
0.2
0.7
0.8
1.6
2.6
4.4
10.9
17.4

Table 2:
Component/ Percentage (%)








Ethanol
9.90
24.15
33.65
46.3
57.52
61.48
58.25
50.80
Toluene
89.11
72.46
62.5
46.3
30.97
20.49
6.47
2.67
Water
0.99
3.38
3.85
7.41
11.50
18.03
35.28
46.52



Discussion
Ternary phase diagram contains three components which are water, ethanol and toluene. In this experiment, the mixture of ethanol and toluene once sealed in measuring container containing various percentages of ethanol and toluene. The mixture is prepared into 20mL of each containing various percentages of ethanol such as (%) 5,50,60,75,90. The mixture is  titrated with water until cloudiness appear due to existence of second phase. This means two phases present in this experiment is detected and the volume of water used until the cloudiness is appears is recorded.

 Based on the graph, each three corners or apexes of triangle represent 100% by volume of one component (water, ethanol and toluene). As a result, that same apex will represent 0% of another two components. When the percentages of ethanol increases in the mixture, the volume of water need to be titrated until the mixture turn cloudiness is increases. The addition of water as the third component to a pair of miscible liquids of toluene and ethanol can change their mutual solubility. If the third component is more soluble in one of the two different component mixtures the mutual solubility of the liquid pair is decreased and thus two phases liquids will be appears.

 Toluene and ethanol are miscible liquids while toluene is water insoluble liquid while ethanol contains OH group that will completely react with water as water is a polar substance that will attract OH group. Hence water and ethanol will be miscible in any amount. Hence, two phases diagram is appears due to decrease the solubility of the three components mixture.

During the experiment there are some errors that may happen. While taking the measurements of the liquids, the eyes does not perpendicularly on the scale of the measuring cylinder. Hence the eyes must be perpendicular to the scale of the to prevent the false measurement of the liquids. Other than that, when undergo shaking process during titrating to make the mixture completely miscible, the shaking process does not undergo gently and it may affect the person to take the actual amount of water needed to make the mixture cloudiness hence while titrating , the shaking process must undergo gently and the actual volume of water can be recorded.

Other than that, the errors is the degree of cloudiness. We do not have a specific range of degree of cloudiness in each of the experiment. This might affect the volume of water added to the solution. It may be less or more than the actual one. This has greatly affected the percentage by volume and the curve too.

Besides, room temperature in the laboratory that is not constant during the experiment is one of the errors too. Room temperature is one of the significant factors that will change the graph or curve pattern and this might be the cause of incomplete binomial curve.

Moreover, volatility of the liquids that we used for the experiment. We use ethanol and toluene which are volatile liquids and they will vapourise if left longer. If this happened, the measured volume may be less than the actual one as some of them already evaporates and thus affected the volume of water needed for titration. Thus we should not leave the measured toluene and ethanol too long and conduct the experiment quickly.

Questions

 1.    Does the mixture containing 70% ethanol, 20% water and 10% toluene (volume) appear clear
  or does it form two layers?

 Based on the diagram that has been plotted, it can be examined that the mixture containing 70% ethanol,  
 20% water and 10% toluene will be appeared as a clear solution.

 2.    What will happen if you dilute 1 part of the mixture with 4 parts of

        (a)    Water

         The solution appeared in two layers as there are two phases formed.

        (b)    Toluene

         The solution appeared in two layers as there are two phases formed.

        (c)    Ethanol

        The solution appeared in one layer as there is only single phase formed.

Conclusions

The reaction of water, ethanol and toluene will appears as two phase’s system due to the decreasing in solubility of the mixture.

References:
5 Davell D. Ebbing. 2009. General Chemistry. 9th edition. Page 311-319. Boston: Cengage Learning.
















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