Wednesday, 7 May 2014

PRACTICAL 1

Practical 1 : Phase Diagram
PART A
Determination of Phase Diagram For Ethanol / Toluene / Water System Theory
Tree-Component System
OBJECTIVE:

To study the miscibility of ethanol / toluene / water system and to investigate the behavior of system of the three liquid which is ethanol, toluene and water.

APPARATUS:

Burette, conical flask, retort stand, measuring cylinder, test tubes

MATERIALS:

Ethanol, Toluene, Water

INTRODUCTION:
Phase diagrams for ternary systems are usually represented using a triangle shown in Fig. 2.





                                                                      Figure 1

A three-component phase diagram has four degrees of freedom: F = 3 − 1 + 2 = 4. In this case, temperature and pressure are two of the conditions and the concentrations of two of the three components make up the rest. In this diagram, each of three corners or apexes of the triangle represent 100% by weight of one component (in this experiment ethanol, toluene, water). As the result the other two apex will represent 0% of the other two components.Only two concentrations are required because the third will be the difference between 100% and the sum of the other two components.
These systems are used for determining miscibility/solubility, coacervation regions, gel-forming regions for multicomponent mixtures, etc. The lines joining the corner points forming the triangle each represent two component mixtures of the three possible combinations (AB, BC, and CA). If two of the components are known, the third is known by difference. Any combination of the three components is described by a single point on the diagram. The addition of a 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 the mutual solubility of the liquid pair is decreased. However, if it is soluble in both of liquids 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.

PROCEDURES:
  1.  Ethanol/ toluene mixtures of different compositions were prepared and placed in sealed conical flasks.
  2. Each mixture contained different % volume of ethanol in 50 ml: 10, 25, 35, 50, 65, 75, 90, 95% v/v.
  3.  A burette was filled with distilled water.
  4.   The mixtures were titrated with water, accompanied by vigorous shaking of the conical flask.
  5.  Titration was stopped when a cloudy mixture was formed.
  6.   The volume of the water used was recorded.
  7.  Steps 1-6 were repeated to do a second titration. The volume of water required for complete titration of each mixture was recorded.
  8. Average volume of water used was calculated.
  9.  % volume of each component of the ternary system for when a second phase became separated was calculated.
  10.  These values were plotted on a graph paper with triangular axes to produce a triple phase diagram.

RESULTS:

Ethanol
Toluene
Water
Volume of Ethanol /mL
% of Ethanol
Volume of Toluene/mL
% of Toluene
Volume of Water/mL
% of Water
2.0
9.9
18.0
88.7
0.3
1.5
5.0
24.0
15.0
72.1
0.8
3.9
7.0
33.3
13.0
61.8
1.1
5.0
10.0
45.6
10.0
45.6
2.0
8.9
13.0
55.6
7.0
30.0
3.4
14.5
15.0
60.0
5.0
20.0
5.0
20.0
18.0
59.0
2.0
6.6
10.6
34.5
19.0
49.0
1.0
2.6
18.8
48.5




QUESTIONS:
1.       Does the mixture containing 70% ethanol, 20% water, and 10% toluene (volume) appear clear or does it form two layers?

No. The solution appear clear and form one liquid phase.

2.       What will happen if you dilute one part of the mixture with four part of (a) water (b) toluene (c) ethanol?

The mixture contain 70% ethanol, 20% water and 10% toluene

 1 part x 70/100 = 0.7 part of ethanol
 1 part x 20/100 = 0.2 part of water
 1 part x 10/100 = 0.1 part of toluene
~There are 0.7 part of ethanol, 0.2 part of water, 0.1 part of toluene in the                                    mixture.

(a)    One part mixture + four part water
Ethanol =         0.7
                    --------- × 100%
                      1+4
               = 14%

Water =       0.2 + 4
                  ---------- × 100%
                     1+4
            = 84%

Toluene =       0.1
                 ----------× 100%
                      1+4
                = 2%
̃ based on phase diagram, the mixture is outside the curve. Thus single liquid      phase will formed.

(b)   One part of mixture + four part toluene
        Ethanol =       0.7
                         ----------- × 100%
                             1+4     
               = 14%

                           
                                 Water =    0.2
                     ---------- × 100%
                              1+4
                = 4%

            Toluene =    0.1 + 4
                              ----------× 100%
                                 1+4
                    =82%
̃ based on phase diagram, the mixture is outside the curve. Thus, single liquid       phase will formed.

(c)    One part mixture + four part ethanol

        Ethanol =     0.7 + 4
                         ----------- × 100%
                             1+4     
               = 94%

                           
                                 Water =     0.2
                     ---------- × 100%
                              1+4
                = 4%

            Toluene =        0.1
                              ----------× 100%
                                 1+4
                    =2%
̃ based on phase diagram, the mixture is outside the curve. Thus, single liquid      phase will formed.

    DISCUSSION:

For the diagram, each corner represent 100% of each component, which is 100% toluene, 100% ethanol, and 100% water while the other two component 0%. In going along the line bounding the triangle represent the concentration in two-component system, it does not matter whether we proceed in a clockwise or counterclockwise direction. But the more usual convention is clockwise. In this case, as we move along water to ethanol in the direction of ethanol, we assume the system of containing increasing concentration of ethanol and smaller amounts of water. Moving along ethanol to toluene will results in increasing amount of toluene and the closer we approach water, the more its concentration will be. For example, at the first point the amount of ethanol increases as we read it in clockwise. Ethanol is 9.9%, water 1.5% and toluene 88.7%. Result obtained in this experiment was not accurate due to some error occurred during the experiment. Some of the error occurred are parallax error during recorded and measured the scale. Furthermore, the temperature also is not constant causing the measurement become slightly deviated and some of the glassware have been contaminated causing the chemical mixed with other compound. All this error causing result to be inaccurate and slightly affect the graph obtained.

Some precaution need to be taken such as make sure our eyes are parallel with the meniscus so that measurement is more accurate. We also need to make sure the temperature is constant so that the reaction of the chemical are almost the same for all set and clean the apparatus before use to reduce contamination.





CONCLUSION:

Water and toluene form a two-phase system because they are only slightly miscible. Ethanol is completely miscible with both toluene and water. The rule that relate to the use of triangular coordinates fully explained the three-component system.

REFERENCES:



3.       Martin’s Physical Pharmacy And Pharmaceutical Sciences, 6th edition (2011). Patrick J. Sinko. Lippincott Williams and Wilkins

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