Monday 8 December 2014

 

PRACTICAL 3:PHASE DIAGRAM


PART B

TITLE:

Mutual solubility curve for phenol and water



DATE OF EXPERIMENT:


3rd   November 2014


OBJECTIVES:

                              *            To measure the miscibility temperatures of several water-phenol mixtures of known   composition
                              *            To construct and understand the
                              *            To determine upper consolute/critical temperature of water-phenol mixtures


INTRODUCTION:

       A phenol – water solution was used to determine the solubility of two partially miscible liquids.  The group calculated the volume of water required to prepare the following mixtures with volume percentage ranging from 5% to 95% sample at 5% increment using 10mL phenol sample.  The different volume ratios of mixtures prepared were subjected to constant heating and cooling in order to gather the needed temperature necessary for the construction of the mutual solubility curve of Phenol- Water solution.

        Mutual solubility of the components in a liquid-liquid system may results complete miscibility or partial miscibility. Complete miscibility can be defined as particles involves are well distributed or fully mixed (mix in all proportions; “like dissolve like”). Meanwhile, partial miscibility is the formation of two layers when certain amounts of liquids are mixed. Two liquids are “partially miscible” if shaking equal volumes of the liquids together results in a meniscus visible between two layers of liquid, but the volumes of the layers are not identical to the volumes of the liquids originally mixed. In the experiment, we used water and phenol to discuss the idea of this mutual solubility. Phenol-water binary system is a system that shows the nature of the mutual solubility between phenol and water at a certain temperature and fixed pressure. According to the theory, water and phenol have the property of partial miscibility when it is initially mixed. As we learnt, mutual solubility of partially miscible mixture is influenced by temperature.
   As the temperature of the water-phenol mixture is increased, it will reach a critical point or we called it as upper consolute temperature where the homogenous mixture will form. Thus, under or beyond this critical point temperature, it will become heterogeneous or 2 layers of mixture will form back. In this phase, the compositions for two liquid phases in equilibrium are constant and are not affected by the relative amount of these two phases. These phases are termed conjugate phases. The relative amounts of the two phases vary. The miscibility between two partial miscible liquids is normally affected by the existence of third component. For more understanding of this mutual solubility of phenol-water mixture, the plot of mutual solubility curve for phenol and water(temperature measured versus phenol composition) is needed. By doing so, we can easily know the critical point temperature, temperature for each phenol composition for the mixture to change to the phase required and many more.

APPARATUS:

                                                                    Thermometer


                                                                       Test tubes


                                                                         Parafilm



                                                                   Measuring cylinder




                                                                       Test tube holder




                                                                         Water bath


MATERIALS:

Phenol,Water



EXPERIMENTAL PROCEDURES:



1)  Students were given tightly sealed tubes containing amounts of phenol concentration scaled between 8% to 80%.
2)    In order to increase the temperature through heating, students were about to heat the tubes in the beaker containing water.
3)  The water was stirred and the tubes were shaken as well. The temperature for each of the tube at which the turbid liquid becomes clear were observed and recorded.
4)  The tubes were removed from the hot water and the temperature was allowed to reduce gradually, the temperature at which the liquid becomes turbid and two layers were separated.
5)  The average temperature for each tube at which two phases were no longer seen or at which two phases exists were determined.
6)  Part of the tubes was to be cooled besides being heated as instructed above.



RESULTS:

Tabulation of data

PERCENTAGE OF PHENOL (%)
VOLUME OF PHENOL (mL)
VOLUME OF DISTILLED WATER (mL)
AVERAGE TEMPERATURE AT WHICH THE TURBID LIQUID BECOMES CLEAR (°C)
AVERAGE TEMPERATURE AT WHICH THE LIQUID BECOME TURBID (°C)
8
1.6
18.4
35
33
11
2.2
17.8
50
45
20
4.0
16.0
68
65
35
7.0
13.0
69
64
50
10.0
10.0
65
60
63
12.6
7.4
60
58
70
14.0
6.0
55
51
80
16.0
4.0
44
39

Graph

A graph of Composition of Phenol in water (% by volume) against Temperature at complete miscibility (°C )




                             Temperature at
                         complete miscibility
                                     ( °C )
                                                                  Composition of Phenol 
                                                                              in water  (% by volume)




 DISCUSSION:

Phase rule is a useful and may be used to determine the variance of any system at equilibrium. It is used to relate the effect of the least number of independent variables like pressure, temperature and concentration upon the various phases (solid, liquid and gaseous) that can exist in an equilibrium system containing a given number of components. There are some factors to be considered in order for the system to be in equilibrium. Those are the degree of freedom (F), the number of component making up the phases (C) and the number of phases that can coexist or the number of phases in thermodynamic equilibrium with each other (P). The number of degrees of freedom is the number of independent intensive variables.
The rule is the equality:  
 F = C – P + 2
In this experiment, the phenol and water are partially miscible. We plotted the graph of average temperature against percentage of phenol based on the data we obtained in the experiment. We get an n-shaped graph after it is been plotted. The peak of the graph showed the critical temperature for the solution where critical solution temperature is the temperature at which a mixture of two liquids (Phenol and Water for this experiment), immiscible at ordinary temperatures, cease to separate into two distinct phases. The region outside the curve will have one liquid phase and the region within the curve will have two liquid phases. The first boiling tube containing 8 % of phenol and the last boiling tube containing 80% will have their mixtures exist as one liquid phase. As the percentage of phenol increases, the amount of phenol-rich phase will continuously increase and forming two phases system. Finally, the critical solution temperature for this experiment is 69 °C. In this experiment, we are measuring the temperature of the phenol-water system at miscible and temperature at which two phases separated.
There are some precautionary steps that should be taken during this experiment. Firstly, after inserting the thermometer into the test tube, the tube must be sealed immediately and tightly to prevent evaporation of phenol once it is mixed with water. This is to ensure the accuracy of the result obtained as evaporation of phenol may affect the result. Besides, this step also ensures that there will be no heat lost to the surrounding when the test tube is heated in water bath and when the temperature is measured. Parallax error also may occur when we measure the volume of phenol and water and recording of the temperature of the thermometer. The desired volume of phenol may not be obtained due to this error and thus causes deviation the result of the experiment. Lastly, we must be very careful in taking the reading of the temperature when heating and cooling the mixtures. This is to avoid the inaccuracy in the result of the experiment as the temperature will increase or decrease rapidly.
  

CONCLUSION:

The critical solution temperature peaks at 69°C. A two-component system is formed between phenol and water. In this experiment, both water and phenol are partially miscible.

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

 The foreign substances will affect the critical solution temperature. If the foreign substance is soluble in one of the two liquids, the mutual solubility of the latter is destroyed, and the temperature at which the system becomes homogeneous is raised.This increase in temperature is due to the salting out of water. When the added substance dissolves in both the liquids, the critical solution temperature is lowered due to negative salting out effect. This effect is important to the industrial production of highly concentrated solutions of tar acids (phenols and cresols) used as disinfectants. 


REFERENCE:

3  3)     http://www.scribd.com/doc/116082090/The-Binary-System-Phenol‎















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