Sunday, 11 December 2016

Experiment 3B - Mutual Solubility Curve for Phenol and Water UKM

Title: Experiment 3 (Phase Diagram Part B) - Mutual Solubility Curve for Phenol and Water.
Date of experiment: 10th November 2016
Aim:
     1.      To determine the solubility of two partially liquids ( phenol- water solution)

Introduction:
A few liquids are miscible with each other in all proportions, for example: ethanol and water. Others have miscibility in limited proportions in other liquids, for example: etherwater, phenol-water. The curve gbhi shows the limits of the temperature and concentration within which two liquid phases exist in equilibrium. The region outside the curve contains systems having but one liquid phase.

Generally, both liquids become more soluble more soluble with rising temperature until the critical solution temperature or consulate point is attained and above this point the liquids become completely miscible. There is a big possibility that any pair of liquids can form a closed system, whereby both upper and lower critical solution temperature exist, however it is not easy to determine both the temperatures (before the substances freezes or evaporates).
At any temperature below the critical solution temperature, the composition for the 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 pair of partially miscible liquids in general is extremely influenced by the presence of a third component.


Apparatus/Materials:
Boiling tubes, Beaker, Thermometer, Test tube holder, Parafilm, Measuring cylinder, Dropper
Chemicals:
Distilled water, Phenol
Procedure:
1.      Prepare 5 boiling tubes with labels A, B, C, D and E
2.      Tightly seal the boiling tubes with water and different concentration of phenol – 8%, 30%, 50%, 70% and 80% respectively to the boiling tubes.


3.      The boiling tubes heated with water to increase the temperature of solution.
4.      The solution stirred and boiling tubes shake.
5.      When the turbid liquids become clear, the temperature of the boiling tubes observed and recorded.
6.      The boiling tubes removed from the heated water and allowed the boiling tubes reduce the temperature gradually.
7.      The temperature of boiling tubes when the liquid becomes turbid and two layers separated is recorded.

8.      Average temperature for each tube at which two phases are no longer seen or at which two phases exist is determined (Part of the tubes may need to be cooled besides being heated as instructed above). 

Results
Percentage of phenol %
Volume of phenol (mL)
Volume of water (mL)
Temperature (˚C)
Average temperature (˚C)
During heating
After heating
8
1.60
18.40
77.00
31.00
54.00
30
6.00
14.00
80.00
51.00
65.50
50
10.00
10.00
51.00
41.00
46.00
70
14.00
6.00
79.00
32.00
55.50
80
16.00
4.00
60.00
30.00
45.00



Critical solution temperature of phenol-water system is 65.5 oC




Discussion
           
Phase rule is a useful device for relating effect of the least number of independent variables such as 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. The 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 components
·         P = the number of phase present

In this experiment, the phases of the two components used which are phenol and water depend on the conditions the experiment was conducted. When phenol and water and water are miscible at a particular condition, having one-phase liquid system, the degree of freedom is, F=2-1+2 =3. Since this is a condensed system (the pressure of the system is fixed), F is reduced to 2. This means that only two variables are needed which are temperature and concentration to define the system. When phenol and water are immiscible with each other, the degree of freedom is, F=2-2+2 =2. Since the pressure is fixed for this system, F is reduced to 1. This means that temperature is the only variable to define the system.

            This experiment is conducted to determine the solubility of two partially liquid (phenol-water solution). Based on graph, the graph shows the temperature at complete miscibility of the solution against the percentage of phenol composition in the solution. The region inside the curve shows that the solution has two phase system while the region inside the curve shows that the solution is completely miscible and exist in one-phase liquid system. In this experiment, the maximum temperature which are the critical solution temperature of phenol-water system obtain is 65.5 oC. As the percentage of phenol increases, the amount of phenol-rich phase increases and the amount of the water-rich phase decreases. The theoretical critical solution temperature for this phenol-water system is 66.8 oC.

From the result obtained, one of the point obtained is slightly deviated from the graph and the critical solution temperature obtained also slightly different from the theoretical value. This may due to some errors that occurred during the experiment. Firstly, the parafilm is not sealed properly on the boiling tube. This parafilm is used to prevent the escaping of vapour from the boiling tube and to fixed the pressure for this experiment. If the boiling tubes are not sealed properly, the heat will escape the surrounding when the temperature is measured. To overcome this error, the parafilm should be sealed properly on the boiling tube. Next, the reading of temperature is not being recorded immediately after a particular condition is obtained. This might affect the accuracy of the results. To overcome this result, the reading of temperature should have been recorded immediately after a particular condition is obtained. Lastly, parallax error occurred when taking the reading of measuring cylinder to measure the volume of the two components (phenol and water) and also when taking the reading of the thermometer. To overcome this error, the eye of the observer should be parallel to the scale line of the apparatus.

Some precaution should be done during the experiment. Firstly, the adding of phenol into the water should be done in fume cardboard as the phenol is a carcinogenic substance. Besides, goggles and gloves should be wear throughout the experiment. The boiling tube should be shake gently while it is in the water bath to produce a uniform mixture of solution.

Conclusion
The critical solution temperature of the experiment is 65.5 oC. The solubility of two partially liquid (phenol-water solution) is determined.
Question
    1.      Explain the effect of adding foreign substances and show the importance of this effect in pharmacy.
The addition of the foreign substances such as salt can give effect toward the critical temperature and the phase separation. The addition of the salt will reduce the miscibility of the phenol and water which cause the phase separation. The water molecules will associate with the salt ions and hydrating them. So, the simple ion will lower the tendency of the water to solvate the phenol. The result of addition of the salt will be increasing the critical temperature and the phenol on phenol rich side of the coexistence of the curve. If the foreign substance are soluble in both liquid, the solution will be soluble that called as blending. An example of this is when succinic acid is added to the water-phenol mixture , succinic acid is soluble or completely miscible in each water and phenol therefore it causes a blending of the liquids making the mixture one phase. The solubility of the substance is important to determine the purity of the substance.
References
    1.      Martin's Physical Pharmacy and Pharmaceutics 6th Edition


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