Wednesday, December 16, 2015

PRACTICAL 3 (Part B): Mutual solubility curve for phenol and water

Title : Phase diagram (Part B): Mutual solubility curve for phenol and water 
Date of experiment : 2 November 2015
Objectives :
1) To study the relationship between solubility of mixture of water with difference percentage of phenol composition and temperature.
2) To determine and construct the mutual solubility curve for phenol and water.
3) To obtain the Critical Solution Temperature (CST) from the mutual solubility curve.

Introduction :
            Some liquids are miscible with each other in all proportions to form homogenous solution. However, some other liquids have miscibility in limited proportions in other liquids. For example, ethanol and water are miscible with each other in all proportions while etherwater and phenol-water are liquids that partially miscible yielding either one or two liquid phase, depending on the condition.
            Generally, the temperature of the system can influence the miscibility of liquids. When the temperature increases, the mutual solubility of partially miscible liquid will also increases until it reaches the consolute point which also known as critical solution temperature. This temperature is the critical temperature above which the components of a mixture are completely miscible in all proportions which can be obtain from the mutual solubility curve. It is difficult to determine the upper and lower critical solution temperature except for nicotine and water.
            The mutual solubility curve for phenol and water can be determined by analytical and synthetic method. 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 a pair of partially miscible liquids in general is extremely influenced by the presence of third component. The mutual solubility curve for phenol and water can be determined by analytical method and synthetic method.
Apparatus :
Test tube
Test tube rack
Thermometer
Beaker 20mL
Parafilm
Aluminiun fold
Water bath
Measuring cylinder 10mL or 20mL

Chemical :
Phenol
Distilled water

Experimental procedure :
1) 5 set of the phenol with concentration scale 8% to 80% are determined. The volume of phenol and distilled water used are calculated by using the total volume of 20mL.
2)  5 test tubes are prepared and placed on the test tube rack.
3) The phenol and distilled water are mixed with different concentrations and they are stirred by using the thermometer. Then, the opener of test tubes are quickly sealed with parafilm and aluminium fold.
4) The test tube are placed in the water bath and the temperature at which the liquid become 2 clear layers are recorded.
5) The test tubes are removed and cooled down. The temperature at which the liquid become cloudy are recorded.
6) The average temperature for each test tubes is calculated.
7) The graph of average temperature against percentage of phenol is plotted. The critical solution temperature is determined from the graph.

Result :
Set
Percentage of phenol (%)
Percentage of water (%)
Temperature single-phase (0C)
Temperature double-phase (0C)
Average temperature (0C)
1
8
92
29.0
24.0
26.5
2
20
80
60.0
56.0
58.0
3
40
60
68.0
56.0
62.0
4
60
40
45.0
39.0
42.0
5
80
20
26.0
24.0
25.0










Discussion :
            Phase rule is the principle that in any system in equilibrium the number of degree of freedom is equal to the number of components less than the number of phases plus two. It is a useful device for relating the effect of the least number of independent variables, for instance ,concentration, pressure and temperature upon the solid, liquid and gases that can exist in equilibrium system containing a given number of components. The phase rule can be express as F=C-P+2 where F is the number of degree of freedom, C is the number of component and P is the number of phases present. F, the number of degree of freedom is the least number of intensive variables that must be fixed to describe the system completely. C, the number of component is the smallest number of constituents by which the composition of each phase in the system at equilibrium can be expressed in the form of a chemical formula or equation .P, the number of phases present is number of homogenous, physically distinct portion of a system that is separated from other portions of the system by bounding surface.
In this experiment, we used two component which is water and phenol .The miscibility of phenol and water depends on the condition of temperature and also the percentage of the composition of phenol within the mixture of phenol and water. When phenol and water are miscible with each other, the degree of freedom, F= 2-1+2=3. As the pressure is fixed as 1 atp, the degree of Freedom will change to 2, which the variable is temperature and percentage of composition of phenol within the mixture of water and phenol. 
After the experiment was carried out, graph of average temperature against percentage of phenol composition is plotted. The ‘n’ shaped like curve graph is obtained which is mutual solubility curve. When the percentage of phenol composition less than 8%, the phenol and water and are completely miscible with each other to form water. When the percentage of phenol composition more than 80 %, the phenol and water will also completely miscible with each other to form phenol. Both situation exist as only 1 phase system. As the percentage of phenol composition  beyond 8%, the mixture exist as a two phase , at first , it exist as a water-rich phase , however , as the percentage of  phenol composition increase , the water- rich phase decreased gradually and changed to phenol-phase until beyond 80% . Both phenol and water is completely miscible with each other, exist as only 1 phase. Besides, the ‘n’ shaped curved shows the limit of the temperature and concentration within which the two liquid phase of phenol and water exist in equilibrium. The region outside the cure exist as a 1 liquid phase region while the region within the curve containing the system exist as a 2 liquid phase. The critical solution temperature is obtained by the maximum point of the ‘n’ shaped curve. This is known as the temperature of the maximum temperature at which two phase region exists and separated.
            From the result that obtained from the experiment, some of the points in the graph are slightly deviated from the actual mutual solubility curve. Moreover, the critical solution temperature obtained from the experiment is 64 0C, while the actual reading is 66.8 0C.This is due to some errors are occurred during the experiment was carried out .First and foremost, the opener of the test tube is not seal tightly by parafilm. This will lead to the evaporation of phenol once phenol is mixed with the water. The evaporated phenol can affect the actual composition of phenol within the mixture, consequently, the accuracy of the result is also affected. Moreover, the actual reading of the temperature changed of the mixture right after out of the water bath and cooling down is not recorded correctly due to the temperature increase and drop rapidly. Hence, to avoid this error, faster reaction to take record the temperature at which solution turn clearly .Moreover, the reading of the temperature after cooling down must be recorded immediately. This two precaution step can help to get the more accurate average temperature.  The desired volume of the solution of the mixture between water and phenol is inaccurate due to the use of wrong apparatus which is measuring cylinder.  Burette is the apparatus that supposed to use to get the actual desired volume of the both solutions in the mixture. 

Question :
 Explain the effect of adding foreign substances and show the importance of this effect in pharmacy.
            
The addition of foreign substances can change the binary system to produce ternary system. Binary system is the closed system that contains two components while ternary system is the closed system that contains three components. The addition of the foreign substances can give effect toward the critical solution temperature and the phase separation of the mixture. If the foreign substance is soluble in only one of the two components or the solubility of foreign substance is very different from the two components, the mutual solubility of the mixture will decrease and causes the critical solution temperature become lower. For example, the addition of foreign substances like salts can reduce the miscibility of water and phenol. This will cause the water molecules to hydrate the salt ions, reducing the tendency of water molecules to solvate the phenol. On the other hand, if the foreign substance is soluble in both components, the mutual solubility of mixture will increase and the critical solution temperature will become higher. For instance, when succinic acid is added to phenol-water mixture, this will cause the mixture become one phase. The addition of foreign substances is important in preparation of pharmaceutical solution. By knowing the properties of the drug and the mutual solubility between foreign substances with drug, the best solvent of the drug can be determined.

Conclusion :
The critical solution temperature in the experiment is 640C. The increase of temperature can increase the miscibility of the mixture. When the phenol-water mixture reached the critical solution temperature, all combination of phenol and water above this temperature are completely miscible and yield one-phase liquid system.

References :
1) Physicochemical Principles of Pharmacy (4th) edition by Alexander T Florence and David    Attwood
2)  Sinko, Patrick J., Martin’s Physical Pharmacy and Pharmaceutical Sciences, 5th ed., Lippincott Williams & Wilkins, 2005. page 51.
3)https://www.google.com/webhp?sourceid=chrome-instant&ion=1&espv=2&ie=UTF-8#q=number%20of%20degree%20of%20freedom%20definition

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