Monday, 12 December 2016

Practical 3a : Mutual Solubility Curve for Phenol and Water


Title: Mutual Solubility Curve for Phenol and Water

Date: 7th November 2016

Objectives:

1.      To determine the solubility of two partially liquids (phenol – water solution)

2.      To construct the mutual solubility curve and determine the relationship between the temperature and solubility of the liquids

3.      To determine the critical solution temperature

Introduction

Some liquid are completely immiscible (eg. Oil and water) while some are completely miscible in all proportions (eg. Ethanol and water) . However, many liquid mixtures fall between these two extremes. If you shake equal volumes of two of these liquids together, you often get two layers with unequal volumes. These liquids are “partially miscible”.



As the temperature rises, both liquids become more soluble in each other. They reach a mutual solubility temperature or critical solution temperature. Above that point, the mixture becomes homogeneous, where one layer will be formed. Below that point, the mixture separates into two layers.



Phenol is also soluble in water to some extent due to its ability to form hydrogen bonding with water molecules. Nevertheless, the large part of phenol molecule is phenyl group that is non-polar. Hence its solubility is limited in water. However the polarity of this part increases in phenoxide ion when the temperature is raised, and hence the liquids will be more soluble. 



At any temperature below the critical solution temperature, the composition for two layers of liquid in equilibrium state is constant and does not depend on the relative amount of these two phases. The mutual solubility for a pair of partially miscible liquid in general is extremely influenced by the presence of third component.



Apparatus

Boiling tube, Test tube, Measuring cylinder, 5ml pipette, 1ml pipette, Water bath, Thermometer

Materials

Distilled water, Phenol

Procedure

1.      Five boiling tube is prepared and labelled as A, B, C, D and E

2.      The boiling tubes are filled with different amount of water and phenol with the respective percentage.

a.       Boiling tube A with 8% of phenol

b.      Boiling tube B with 30% of phenol

c.       Boiling tube C with 50 % of phenol

d.      Boiling tube D with 70% of phenol

e.       Boiling tube E with 80% of phenol



          

3.      Heat the boiling tubes with water bath. The boiling tubes were swirled and shaken well.

4.      The tubes were observed and temperatures were recorded when the turbid becomes clear.

5.      The tubes were removed from the hot water and the temperature was allowed to reduce. As soon as the liquid becomes turbid and two separate layers were form, the temperature is recorded.

6.      Steps 1 – 4 are repeated.

7.      By using the temperature obtained, the average temperature for each tubes at which the two phases were no longer seen or at which two phases were exist were determined.

Result

SET
PERCENTAGE OF PHENOL (%)
PERCENTAGE OF WATER (%)
TEMPERATURE WHEN MIXTURE BECOME ONE LAYER (°C)
TEMPERATURE WHEN MIXTURE BECOME TWO LAYER (°C)
AVERAGE TEMPERATURE (°C)
1
8
92
65
X
65.0
2
30
70
74
72
73.0
3
50
50
77
75
76.0
4
70
30
71
68
69.5
5
80
20
X
X
X

  

GRAPH



Discussion

            Phase rule is a device that is used to relate the effect of the least number of independent variables upon various phases that can exist in an equilibrium system which have a given number of components. The phase rule can be expressed as F= C-P+2 where F is the number of degrees of freedom in the system, C is the number of components and P is the number of phases present. In this experiment, phenol and water is used as the components where phenol is partial miscible with water. When phenol is miscible with water at certain condition, the number of degrees of freedom in the system, F=2-1+2=3 . Since the pressure is fixed for this system which is the atmospheric pressure, F is reduced to 2. This means that we need to fix both temperature and concentration to define this system. When phenol is immiscible with water at certain condition, the number of degrees of freedom in the system ,F =2-2+2=2 . Since the pressure is also fixed for this system which is the atmospheric pressure,F is reduced to 1. This means that we only need to fix the temperature to define the system.

            After the experiment , a graph of temperature at complete miscibility versus phenol composition in different mixture is plotted. A n-shaped graph is obtained. This curve shows the limits of temperature and concentration within which phenol and water exist in equilibrium. The region outside the curve shows that phenol is miscible with water(1 liquid phase) while the region within the curve shows that phenol is immiscible with water(2 liquid phase).The maximum temperature at which the 2 liquid phase exist is called critical solution temperature. The critical solution temperature in this experiment is 76.2°c.

            The curve that is obtained from the experiment have some slight deviation compared to the actual mutual solubility curve. This occur because there are some error that have been done when conducting the experiment. Firstly, the tube are not tightly sealed. The tube together with the thermometer should be tightly sealed to prevent heat loss to the surrounding that will affect the reading of the temperature of the mixture. This can also prevent the evaporation of the phenol when it is heated. Besides that, the reading of the temperature should be taken immediately after the mixture become miscible or immiscible because the temperature of the mixture increase and drop rapidly. Lastly, parallax error might occur when taking the reading of the thermometer. The eyes of the observer should be perpendicular to the scale of the thermometer to prevent parallax error.

Questions

Explain the effect of adding foreign substances and show the importance of this effect in pharmacy.

ANS: The addition of foreign substances may affect the critical solution temperature. When the substances added dissolve in only one of the two liquid, the mutual solubility will decreased. The temperature at which the system become 1 liquid phase will increased if the system has upper critical solution temperature and temperature lowered  for system that has lower critical solution temperature. This concept is important in pharmacy as its help the pharmacist to select suitable solvent for a drug and help overcome problem arise during preparation of drugs.

Conclusion

Phenol and water are immiscible unless it meets certain temperature at particular concentration. As the concentration of phenol in the mixture increase, the temperature for the phenol to become miscible with water increase until it reach the critical solution temperature which is 76.2°c. After the critical solution temperature, the temperature of the mixture drops even though the concentration of the phenol increase.

References

1)Lecture note (Phase diagram 1)

2) College Practical Chemistry, by V K Ahluwalia, Sunita Dhingra (2005)

3) https://socratic.org/questions/what-is-mutual-solubility-temperature

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