Monday, 21 December 2015

PHASE DIAGRAM PART B

DATE : 3 / 11 / 2015

TITLE
PART B: 
Mutual Solubility Curve for Phenol and Water

OBJECTIVE
The objectives of the experiment are to determine the critical solution temperature for the phenol-water system and to construct the mutual solubility curve of phenol-water system.

INTRODUCTION
Ethanol and water are liquids that miscible with each other in all proportions while phenol and water have miscibility in limited proportions in other liquids. Basically, both liquids become more soluble with rising the temperature until achieve the critical solution temperature. Above this point, the liquids become completely miscible. The phenol-water system is a suitable example to illustrate the variation of solubility with temperature. At low and high percentages of phenol, water and phenol mix completely forming a single liquid. However, at the intermediate compositions and below the critical solution temperature, mixtures of phenol and water separate into two liquid phases. At any temperature below the critical solution temperature, the composition for two layers of liquids in equilibrium state is constant and does not depend on the relative amount of these two phases. The mutual solubility for the pair of partially miscible liquids in general is extremely influenced by the presence of a third component.

MATERIAL
Phenol, water

APPARATUS          
Test tubes, test tube rack, thermometer, parafilm, aluminium foil, water bath, beaker, measuring cylinder

PROCEDURE








  1. 1.      Mixtures of phenol and water in test tubes was prepared where the phenol was added in water in various percentages from 8%, 20%, 40%, 60% and 80%.
  2. 2.      The total amount of both liquids in the test tubes were fixed to be 20 mL and labelled with A, B, C, D, and E.
  3. 3.      The test tube A containing 1.6 mL of phenol and 18.4 mL of water were heated in water bath and stirred the mixtures.  
  4. 4.      The temperature at which the turbid liquid became clear was observed and recorded.
  5. 5.      The test tube then was removed from the water bath and cooled gradually.
  6. 6.      Temperature at which the liquids became turbid again and forming two separated layers was observed and recorded. The test tube was heated again and the average temperature for heating and cooling was recorded. 
  7. 7.      Steps 3 until 6 were repeated for test tubes B, C, D and E.
  8. 8.  A graph of phenol composition in the different mixtures against temperature at complete miscibility was plotted. The critical solution temperature was determined.



RESULT
Percentage of phenol
(%)
Volume of phenol
(ml)
Volume of
water
(ml)
Temperature (oC)
Average temperature
(oC)
During Heating
After Cooling
8
1.6
18.4
60
10
35
20
4
16
71
65
68
40
8
12
76
64
70
60
12
8
69
57
63
80
16
4
60
50
55





DISCUSSION
Phase rule is a useful device for relating the effect of the least number of independent variables like temperature, pressure and concentration upon the various phases (solid, liquid and gaseous) that can exist in an equilibrium system containing a given number of components.
 Phase rule can be expressed as F=C-P+2, where
F = the number of degrees of freedom in the system
C = the number of component
 P =the number of phases present

Ethyl alcohol and water are completely miscible both as vapours and liquids. A system consists of phenol and water exhibit partial miscibility, which lies between two extremes (the systems of miscible and completely immiscible).
In this experiment, two components which is the phenol and water and phases depend on the conditions in which the experiment was conducted. When phenol and water are miscible with each other at a particular condition, the degree of freedom, F = 2 − 1 + 2 = 3. Since the pressure is fixed for this system, F is reduced to 2. Both temperature and concentration need to be fixed to define this system. When phenol and water are immiscible with each other, the degree of freedom, F = 2 − 2 + 2 = 2.Pressure of the system is fixed, thus the F is reduced to 1. This means that we need to fix the temperature only to completely define the system.
From the experiment that carried out, we plotted the graph of average temperature versus percentage of phenol. After graph has been plotted, we get a incomplete n-shaped-liked graph. The curve shows the limits of temperature and concentration within which the two liquid phases (phenol and water) exist in equilibrium. Region outside the curve contains system having one liquid phase. This means that the phenol and water becomes miscible and exists as one liquid phase at the region outside the curve. The region under the of the curve, there will be existence of two liquid phases.  The quantity of phenol is gradually increased, the amount of phenol-rich phase continually increases and the amount of water-rich phase continually decreases. At the last test test tube, a single phenol-rich liquid phase is formed. The maximum temperature at which the two phase region exists is called the critical solution temperature. The critical solution temperature in this experiment is 72.0˚C. During this experiment, we are measuring the temperature of the phenol-water system at miscible and temperature at which two phases separated.
From the results that we obtained, some of the points in the graph are slightly deviated from the graph. Parallax error during reading the scale of the thermometer is one of the possible error which causes the deviation. Then, covering the mouth of the test tube with aluminium foil is one of the precaution as phenol is a carcinogenic chemical. The boiling tube should be shaken gently while it is in the water bath to produce a uniform mixture of solution.

CONCLUSION
The critical temperature of the solution peaks at  72 oC. Water and phenol are two component system. Phenol is soluble in water at certain temperature as it form clear solution and become immiscible when it is cooled down as the solution showing two layer in the test tube.




PHASE DIAGRAM PART A

PHASE DIAGRAM 
DATE : 3 / 11 / 2015

PART A :
Determination of Phase Diagram of Toluene/ Ethanol / Water System Theory

OBJECTIVES :
  1. Determination of the solubility limits in a ternary system of water and two other liquids (ethanol and toluene), one of which is completely miscible (ethanol) and the other is partly miscible with water (toluene).
  2. Construction of the solubility curve of the system being studied on triangular diagram.
INTRODUCTION :

Phase diagram is a graphical representation of the physical states of a substance under different conditions of temperature and pressure . Ternary phase diagram are 3 components system . For three-component system at constant temperature and pressure , the composition may be stated in the form of coordinated for a triangular diagram .





              In the diagram shown , each corner of the triangular diagram represent a pure component which is 100% ( A, B , C )  . Mean while ,each side represent two-component mixture and within triangular diagram itself represent ternary components . Any line parallel to side of the triangular diagram shows constant percentage value for a component , for example DE shows 20% of A varying amounts of B and C . So , does line FG , showing all mixture containing 50% of B . These lines intercept with each other at K , which definitely contain 20% A , 50% B as well as 30% C . Measurement can be made this way because in a triangular diagram , the sum of all distance from K which is drawn parallel to the three sides of diagram is same and equal to length of any one side of the triangular diagram .

              The addition of third component to a pair of miscible liquids can change their mutual solubility . If this third component is more soluble in one of the two different components of mutual solubility of the liquid pair is decreased .However , when ethanol is added to a mixture of benzene and water , the mutual solubility is increased . Thus , 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 become homogenous .

             The benefits of preparing an oily substance as homogenous water in liquid are already clear .
However what will happen to a system like this when it is diluted should also be known as and this can be explained through the understanding of triangular phase diagram . Figure 1 is also for the system containing components peppermint oilpolysorbate 20-water . A concentration of 7.5% oil , 42.5 % polysorbate20 and 50% of water ( point A in diagram ) can be diluted for 10 times with the water giving a solution that is still clear ( now containing 0.75 % of oil , 4.25% polysorbate 20 and 95% water ) .
            However , when 1 ml of water is added to 10 ml of clear solution B ( 49% oil , 5% polysorbate 20 and 1% water ) the solution become cloudy , point B’ ( 44.5% oil , 45.45 % polysorbate 20 and 10% water ). If 1 ml of water is further added , the solution become clear , point B’’ ( 40.5% oil , 41.3% polysorbate 20 , 18.2% water ) but if the original solution is diluted 3 times 
( 16 1/3 % water , 16 2/3% polysorbate 20 and 67% water ) the solution become cloudy .

APPARATUS :

8 Conical Flasks
Burette

MATERIALS :

Toluene
Distilled Water
Ethanol

PROCEDURE :


Used a burette to measure and do the titration process 
swirl the mixture until cloudiness formed





1.Mixture of ethanol and toluene was prepared in sealed container measuring 20 cm3 of the following percentage ethanol in percent  : 10 , 25 , 35 , 50 , 65 , 75 , 90 and 95% .
2. 20 ml of each mixture is prepared by filling a certain volume using a burette accurately .
3.  A burette was filled with distilled water .
4. Each mixture is titrated with water until cloudiness is observed due to existence of a second phase .
5. The volume of distilled water used was recorded .
6.Step 1 -5 were repeated for a second titration . The volume of water required for complete titration of each mixture was recorded .
7.Average volume of water used was recorded .
8. The percentage based on the volume of each component  when the second phases start to separate was calculated .
9. The points were plotted onto a triangular paper with triangular axis to give a triple phase diagram.

RESULT

Percentage of Ethanol (%)
Volume of ethanol (mL)
Volume of toluene (mL)
Volume of water titrated (mL)
Average volume of water (mL)
Titration I
Titration II
10
2
18
0.6
0.4
0.50
25
5
15
1.1
0.9
1.00
35
7
13
1.7
1.9
1.80
50
10
10
2.9
2.8
2.85
65
13
7
3.3
3.3
3.30
75
15
5
5.0
5.1
5.05
90
18
2
11.7
11.0
11.35

Percentage of Ethanol (%)
Ethanol
Toluene
Water
Total volume
Volume (mL)
Percentage (%)
Volume (mL)
Percentage (%)
Volume (mL)
Percentage (%)
10
2
9.76
18
87.80
0.50
2.40
20.50
25
5
23.81
15
71.43
1.00
4.76
21.00
35
7
32.11
13
59.63
1.80
8.26
21.80
50
10
43.76
10
43.76
2.85
12.47
22.85
65
13
55.79
7
30.04
3.30
14.16
23.30
75
15
59.88
5
19.96
5.05
20.16
25.05
90
18
57.42
2
6.38
11.35
36.20
31.35





DISCUSSION:

In this experiment , A represents ethanol, B represents toluene and C represents water. On each side of the triangle, directly opposite the apex represents 0% of the apex component. 100% of the component is represents by each apex of the triangle. Three lines joining at the corner represent the component mixture of possible combination of A and B, B and C, C and A respectively.
The system has only one phase but 3 component which in this experiment, the components are ethanol, toluene, and water. According to Gibbs phase rule,
F = C – P + 2
where, F = number of degrees of freedom in the system
           C = number of component
           P = number of phases present
In this experiment , the number of degrees of freedom in the system is ;
F = C – P + 2
F = 3 – 1 + 2
                                                                             F = 4 

The 4 degrees of freedom in this experiment including temperature, pressure, and concentration 2 out of 3 component. The third component concentration can be obtained by calculation. Throughout the experiment, the temperature which is measured to be at 26˚C and the pressure are kept constant. This will decrease the degree of freedom to 2 and allow us to use  a planar diagram to illustrate the phase equilibria.

            The experiment is first carried by preparing solution containing 10% ethanol and 90% toluene. At this point, the two components is miscible and exists in one phase. An average of 0.5 mL of water is added until cloudiness is observed which indicated that the second phase is formed. The percentage of the components is changed to 9.76% ethanol, 87.8  % toluene,  2.4% water. The experiment is repeated by increasing the percentage of ethanol to 25%,35%,50%,65%,75%,90% and the average volume of water for the second phase to appear is also increasing. This is because toluene and water are immiscible. thus, the higher the percentage of ethanol, will increased the mutual solubility ,more water is needed for second phase to occur.

From the data obtained, graph was plotted inside a triangular diagram forming a binomial curve. Bounded region by the binomial curve representing the two liquid phase so the mixture is cloudy. Phase separation is indicated by the cloudy solution. Cloudy solution is formed because there is not enough ethanol to produce homogenous mixture. High amount of ethanol will act as surfactant allowing the two liquid phases become single liquid phase. Regionabove the curve shows single liquid phase.
Few errors occur when doing this experiment. One of the error that has affect percentage by volume and binomial curve is degree of cloudiness of the liquid. No specific range of cloudiness is fixed in each experiment causing the volume of water added to the solution affected. This error can be overcome by fixing the degree of cloudiness in each experiment. Ethanol and toluene are volatile liquid. It vapourise quickly causing the actual volume of toluene and ethanol  used in this experiment is less than the measured. To avoid  this from happening, we must quickly titrate the toluene and ethanol after transferring it in the conical flask.

CONCLUSION:

Three-component system is important in preparing the formulation of solution. The three components of ethanol, toluene, and water in this system which is in one phase gives the degree of freedom value of 4. However, the degree of freedom is reduced to 2 as the temperature and pressure is kept constant. From the data, the higher the percentage of ethanol, the higher the volume of water needed for the second phase to appear. This is because toluene and water are immiscible. thus, the higher the percentage of ethanol, will increased the mutual solubility ,more water is needed for second phase to occur. Ternary phase diagrams represent the phase behaviour of mixtures containing three components in a triangular diagram. The ternary phase diagram is plotted and a binomial curve is obtained.


REFERENCES :

  1. Martin's Physical Pharmacy and Pharmaceutical Science, Sixth Edition, Patrick J. Sinko, Wolters Kluwer, Lippincott Williams & Wilkins.