Thursday, 17 December 2015

LAB 3 PART A DETERMINATION OF PHASE DIAGRAM FOR ETHANOL / TUOLENE / WATER SYSTEM THEORY THREE-COMPONENT SYSTEMS

TITLE
Part A: DETERMINATION OF PHASE DIAGRAM FOR ETHANOL / TUOLENE / WATER SYSTEM THEORY THREE-COMPONENT SYSTEMS

AIM
The aims of this lab are:
1.      To determine the solubility limits in a three component systems of water with ethanol and ethanol in which ethanol is completely miscible whereas toluene which is partly miscible in water.
2.      To construct the solubility curve of the system on triangular diagram.

DATE OF EXPERIMENT
2th November 2015

INTRODUCTION
       
In this experiment, there are three components of concern which were Ethanol, Toluene and Water. Water and toluene is insoluble, but as it was mixed together with ethanol, all three components can achieve homogeneous solution at equilibrium if proper proportion was used. Phase diagrams are graphical representations of the liquid, vapour, and solid phases that co-exist at various ranges of temperature and pressure within a reservoir. Ternary phase diagrams are 3 component systems and represent the phase behaviour of mixtures containing three components in a triangular diagram. The three components are usually compositions of elements, but may include temperature or pressure also. It is necessary to know the three binary systems for the three components to construct a ternary phase diagram. Ternary diagrams have a vertical temperature axis.
Figure 1 : Ternary Phase Diagram

In Figure 1, the concentration of each pure component is 100% at each corner of the triangle and 0% at the line opposite it, which is 100% or A, 100% of B and 100% of C. Each side represents two-component mixtures and within the triangular diagram itself represents ternary components. By drawing line parallel to a side of the triangular diagram shows constant percentage value for a component, for example: DE shows 20% of A component with varying amounts of B and C. So does line FG which shows all mixture containing 50% of B. These lines intercept with each other at K, which contains 20% of A, 50% of B and 30% of C. Measurements can be made this way because in a triangular diagram, the sum of all distances from K which is drawn parallel to the three sides of the diagram is same and equals to length of any side of the diagram.

            The addition of a third component to a pair of miscible liquids can change their mutual solubility and settle into 2 phases. If this third component is more soluble in one of the two different components the mutual solubility of the liquid pair is decreased. However, if it is soluble in both of the liquids, the mutual solubility is increased.  For example when ethanol is added to a mixture of benzene and water, the mutual solubility of the liquid pair increased until it reached a point whereby the mixture becomes homogenous. This approach is used in the formulation of solutions.

            In pharmaceutical formulation, multiple components need to be mixed together and be in homogeneous form. This can be achieved by knowing the exact ratio of each component to be mixed with regard of some other condition such as temperature. Examples of three-component systems that has been studied include castor oil/ alcohol/ water; peppermint oil/ propylene glycol/ water; peppermint oil/ polyethylene glycol/ water.

LIST OF MATERIALS
Toluene, ethanol, distilled water

LIST OF APPARATUS
100cm3 conical flask, burette, retort stand, measuring cylinder, test tubes

EXPERIMENTAL PROCEDURES

1. Ethanol/ toluene mixtures of different compositions were prepared and placed in sealed conical flasks.
2. Eight 20 ml solution of toluene and ethanol were prepared in eight different 100cm3  conical flasks.


3. Each flash were filled so that it contain 10%, 25%, 35%, 50%, 65%, 75%, 90% and 95% of ethanol with the rest was toluene. 

   
4. The conical flask were labelled A, B, C, D, E, F, G and H respectively.
5. A burette was filled with distilled water.


6. The mixtures were titrated with water, accompanied by vigorous shaking of the conical flask.
7. Titration was stopped when a cloudy mixture was formed.
8. The volume of the water used was recorded.
9. Steps 1-6 were repeated to do a second titration. The volume of water required for complete titration of each mixture was recorded.
10.  Average volume of water used was calculated.
11.  % volume of each component of the ternary system for when a second phase became separated was calculated.
12.  These values were plotted on a graph paper with triangular axes to produce a triple phase diagram.


RESULTS
Table of data:

Conical flask
Component
Percentage (%)
Volume (mL)
A
Ethanol
14.71
2
Toluene
82.38
8
Water
2.91
12
B
Ethanol
21.74
5
Toluene
72.82
15
Water
5.44
10
C
Ethanol
31.13
7
Toluene
61.47
13
Water
7.40
3.5
D
Ethanol
45.23
7
Toluene
46.30
13
Water
8.47
1.6
E
Ethanol
57.49
10
Toluene
30.91
10
Water
11.60
1.9
F
Ethanol
61.48
13
Toluene
20.49
7
Water
18.03
3.2
G
Ethanol
59.31
18
Toluene
6.59
2
Water
34.10
10.3
H
Ethanol
51.35
19
Toluene
2.70
1
Water
45.95
16.2



QUESTIONS
1.) Does the mixture containing 70% ethanol, 20% water and toluene appear clear or does it form two layer?
The solution appear clear.
2.) What will happen if you dilute 1 part of the mixture with 4 parts of
(a)        Water
Two phases will be observed.
(b)        Toluene
Two phases will be observed.
(c)        Ethanol
One phase will be observed.

DISCUSSION

            Phase diagrams are graphical representations of the liquid, vapor, and solid phases that co-exist at various ranges of temperature and pressure within a reservoir. Ternary phase diagrams represent the phase behavior of mixtures containing three components in a triangular diagram. In this experiment, the mixtures of ethanol and toluene in sealed containers containing following percentages of ethanol (%) which are 10,25,35,50,65,75,90 and 95. Each mixture is titrated with water until cloudiness is observed. This is due to the existence of second phase.


          
  There are three apex in the ternary phase diagram above. Each of them represents 100% by volume of one component which is water, ethanol and toluene. The side of the triangle, directly opposite the apex, represents 0% of the apex component. The area within the triangle represents all the possible combinations of ethanol, toluene and water to give 3 components systems. Toluene and ethanol are miscible liquids. Toluene is water insoluble liquid while ethanol completely react with water as ethanol has OH- group. Water is a polar substance that will attract OH- group. Hence water and ethanol will be miscible in any amount. Due to the decrease in solubility of the three components mixture, two phases diagram appears.

            However, based on the phase diagram plotted above, it is not accurate enough as we have done some errors during the experiment. Firstly, during titration, the eye is not perpendicular to the scale of the burette when taking the reading. The eye must be perpendicular to the reading scale to avoid parallax error and obtain a more accurate result. Besides, titration is not carried out in a proper way. We should do the titration with drop by drop method so that we can stop the titration process immediately at the first presence of two phases. Furthermore, the tendency of cloudiness of all mixtures are not the same. Some may be less and some may be more. The titration should be conducted by the same person throughout this experiment to reduce the difference in the tendency of cloudiness as this may affect the volume of water added to the solution and eventually reduce the accuracy of the result.
            Besides, room temperature in the laboratory during the experiment was not kept constant. It is one of the factor that will change the graph pattern. Lastly, ethanol and toluene should be closed in a container and not exposed to the surrounding too long time. This is because both ethanol and toluene are volatile liquids and they may evaporate rapidly.

CONCLUSION
From the experiment, the 3-component system is considered as condensed system. We need to fix only 2 number of degree of freedom, which are temperature and pressure.
REFERENCE
http://petrowiki.org/Ternary_phase_diagrams
Sinko, P. J. (n.d.). Martin's Physical Pharmacy and Pharmaceutical Science. Lippincott Williams & Wilkins.
 Chang, R. & Goldsby, K. A. 2014. Chemistry. Edisi ke-11. New York: McGraw- Hill Education.



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