Sunday, 11 December 2016

Experiment 3A - Determination Of The Phase Diagram For Ethanol/Toulene/Water System Theory (3 System Theory) UKM

TITLE: EXPERIMENT 3 (PART A) – DETERMINATION OF THE PHASE DIAGRAM FOR ETHANOL/TOLUENE/WATER SYSTEM THEORY (3 SYSTEM THEORY)
DATE OF EXPERIMENT: 10TH NOVEMBER 2016
OBJECTIVES
  1.      To determine the solubility limit in a ternary system of water and two other liquids (ethanol and toluene), one of which is completely miscible (ethanol) and the is partly miscible with water (toluene)
  2.      To construct a solubility curve on the triangular diagram or ternary diagram based on the three-system mixture that is being studied.

INTRODUCTION
A ternary plot or known as the triangle plot, simplex plot is a graph based on three variables which equals to a constant. Graphically, it depicts the ratios of the three variables as positioned in the equilateral triangle where at the vertices of each triangle represents the pure composition of the component practically in a system composed of three species or components. In the ternary plot, the proportions of the three variables a, b, and c (the vertices of the triangle) must sum to some constant, K. Usually, this constant is represented as 1.0 or 100%. Because a + b + c = K for all substances being graphed, any one variable is not independent of the others, so only two variables must be known to find a sample's point on the graph: for instance, c must be equal to K − a − b.
Because the three proportions cannot vary independently: there were only two degree of freedom and it is possible to graph the intersection of all three variables in only two dimensions. The advantage of using a ternary plot for depicting compositions is that three variables can be conveniently plotted in a two-dimensional graph as shown in this experiment and can be referred in the data presentation part. Ternary plot is used in this experiment since it can also be used to create phase diagrams by outlining the composition regions on the plot where different phases exist. The area bounded by the graph in this experiment technically represents the three-system mixture can exist in two-phase or physically when the mixture turned cloudy during the addition of distilled water.


MATERIALS AND APPARATUS
APPARATUS:
   1.      Volumetric flasks
   2.      Retort stand
   3.      Burette
   4.      Dropper
   5.      Measuring cylinder
   6.      Beaker
CHEMICALS:
   1.      Ethanol
   2.      Toluene
   3.      Distilled water

METHODOLOGY
   1.      8 conical flasks were labelled as A, B, C, D, E, F, G and H.



   2.      2mL of Ethanol is added into conical flask A, and 18mL of Toluene is added into the same volumetric flask for a total volume of the mixture is 20mL in the conical flask.
    3.      A burette is filled with distilled water and clamped to the retort stand
    4.      The initial reading of the burette is recorded.
   5.      The content in the conical flask was titrated with the distilled water in the burette and the conical flask was swirled gently until the mixture turns cloudy and the final reading of the burette is recorded.



   6.      Step 2-5 is repeated with volumetric flask B, C, D, E, F, G and H with different percentage composition of Toluene and Ethanol in each volumetric flask respectively with the reference to the table below:

ETHANOL
TOLUENE
VOLUMETRIC FLASK
PERCENTAGE
(%)
VOLUME
(mL)
VOLUME
(mL)
A
10
2
18
B
25
5
15
C
35
7
13
D
50
10
10
E
65
13
7
F
75
15
5
G
90
18
2
H
95
19
1





RESULTS:
VOLUME OF DISTILLED WATER USED

VOLUMETRIC FLASK
VOLUME OF DISTILLED WATER USED (mL)
TITRATION I
TITRATION II
AVERAGE
A
1.4
1.2
1.3
B
0.9
0.5
0.7
 C
1.2
0.5
0.9
D
2.8
1.4
2.1
E
2.9
2.5
2.7
F
3.9
3.9
3.9
G
9.8
11.0
10.4
H
17.3
16.5
16.9

FINAL VOLUME AND PERCENTAGE OF EACH COMPONENT IN THE MIXTURE


VOLUMETRIC FLASK
ETHANOL
TOLUENE
DISTILLED WATER
TOTAL
mL
%
mL
%
mL
%
mL
A
2.0
9.39
18.0
84.51
1.3
6.10
21.3
B
5.0
24.15
15.0
72.46
0.7
3.39
20.7
C
7.0
33.49
13.0
62.20
0.9
4.31
20.9
D
10.0
45.25
10.0
45.25
2.1
9.50
22.1
E
13.0
57.27
7.0
30.84
2.7
11.89
22.7
F
15.0
62.76
5.0
20.92
3.9
16.32
23.9
G
18.0
59.21
2.0
6.58
10.4
34.21
30.4
H
19.0
51.49
1.0
2.71
16.9
45.80
36.9







DATA PRESENTATION






DISCUSSION
           
Ethanol is completely miscible with Toluene and thus the mixtures of the two solutions prepared in the conical flask earlier were in one phase. However, toluene is not miscible with water and the result from the titration of the content in the conical flask with distilled water, at certain point will becomes completely immiscible. Solubility of a component in a system can differs or changes when another foreign component is added into the system since it can affect the mutual solubility of the system. In the case of our system, since different percentage composition of Toluene and Ethanol is prepared, we will discuss more on the effect of the percentage composition of toluene with the volume of water needed to form a two-phase system. Generally, we can say that as the percentage composition of Ethanol in the conical flask is higher, the volume of water needed to turn the system into a two-phase system is also higher.
Based on the basis of the understanding on the solubility of a component can change when different component is added, adding water into the system when it is immiscible with toluene will cause the mutual solubility of the system to decrease. Since ethanol is miscible with the distilled water added, this explains the reason of the conical flask with higher ethanol composition needed a higher amount of distilled water for a two-phase system to be formed. As a reversal, if the third component added into the system is miscible with both toluene and ethanol then the mutual solubility of the system will increase and thus the system will remains as a one-phase system. The end point of the titration of the mixture of ethanol and toluene with water is recorded when the solution was turned into the two-phase system and physically put as the solution turned cloudy.
To prove the explanation above, we can compare the system in conical flask A and H. In conical flask A where the percentage composition of Ethanol is the lowest; which is at 10%, the volume of water needed is also the lowest of all which is only 1.3mL of distilled water is needed to turn the system into a two-phase system. In conical flask H where the percentage composition of ethanol is the highest; which is at 95%, the volume of water needed is also the highest of all which is 16.9mL is needed in order to form a two-phase system. On the ternary triangular diagram, each vertices of the triangle represents the pure percentage composition of each component involved in the three system mixture (after titration with distilled water).
With reference to the triangle in the data presentation part, the top vertices represent the percentage composition of the ethanol, the right vertices on the bottom part represent the percentage composition of distilled water and the left vertices on the bottom represents the percentage composition of Toluene. To plot the graph, the value of each point is taken from the percentage composition of each component (toluene, distilled water and ethanol) after the addition of water (the data can be referred in the result section). The area bounded below the graph is when the system turned into a three-phase system after the addition of foreign substance which changes the mutual solubility of the system.
 A phase rule is a useful device for relating the effect of the least number of independent variables (temperature, concentration, density) that might affect the result of the experiment to improve the accuracy of the data obtained. Knowing the number of the degrees of freedom for the variables mentioned above can help to minimize possible errors that might arise in this experiment since we can fix the involving variables. For a system at equilibrium based on the phase rule:
F = C – P + 2
F = number of phases that can coexist
C = number of components making up the phases
F = degree of freedom

In this experiment, the number of components that that was involved in the system is 3 and the number of phases that it owned was 2. Thus, the value of the degree of freedom is:

F = 3 – 2 + 2
   = 3
From the degree of freedom obtained, we can say that there are three factors that can affect the experimental data.
From the graph plotted, noticed that there was a single point left unconnected since the point lies a bit deviated from the rest of the points and we conclude that some errors might arise while experimenting.  The main error that can affect the overall result is due to the contaminated or unclean apparatus. Some apparatus used in the lab were practically used by another student before, and there was a high possibility of the apparatus for not being clean thoroughly and some residue from the previous experiment might be left in the apparatus. Thus, the precaution step that must be taken in overcoming this source of error is to clean and rinse the apparatus beforehand. However, second error might arise due to the precaution step by cleaning the apparatus. Since our experiment involve distilled water as the manipulated variable, presence of water from the cleaning process can greatly influenced the result obtained since the mixture in the conical flask might get cloudy even before the titration begin.
To overcome this, the apparatus used must be wiped well to remove excess water from the cleaning process. Apart from that, error might also occur from the degree of the cloudiness observed. There are variety degrees of cloudiness that can be observed and thus, the same person must observe the phase change of the system to avoid error in determining the end point of the titration. Besides, the volatile properties of ethanol and toluene were also contributing to the error in this experiment. The mixture prepared must be titrated quickly to minimize the amount of vaporization that can cause the volume of the mixture to be lower than it supposedly to be. Parallax error was also included in response to the inaccurate data obtained. This error can occur when there is some distance between the measuring scale and the indicator used to obtain a measurement and the observer eyes was not squarely aligned with the calibration, causing the reading may be too high or low. To overcome this, the observer eyes must be directly perpendicular with the calibration reading.

CONCLUSION
In a nutshell, as the percentage composition of ethanol increase, the volume of distilled water needed to titrate the mixture is also increasing. Understanding the principle of mutual solubility when a foreign substance is added into the system is the basis of doing this experiment. Before water was added into the system, both toluene and ethanol is miscible with each other and the mixture exist in one-phase. When distilled water is added, it was immiscible towards one of the mixture component which is the toluene and this causes the mutual solubility of the mixture to decrease and addition of enough water can cause the formation of a two-phase system. Since ethanol is miscible with water, conical flasks with higher percentage composition of ethanol needed more distilled water to form a two-phase system. Some errors have affected the overall result obtained and to overcome this, several precautions step have been done to minimize the inaccurate reading.

QUESTIONS
1.        Does the mixture containing 70% ethanol, 20% water and 10% toluene (volume) appear clear or does it form 2 layers?

From the graph plotted, at these concentrations, the solution will appear clear (one phase) as the plot is outside the two-phase boundary.

2.        What will happen if you dilute 1 part of the mixture with 4 parts of (a) water; (b) toluene; (c) ethanol?
1 part x 70% ethanol = 1 part x 70/100 = 0.7 part of ethanol
1 part x 20% water = 1 part x 20/100 = 0.2 part of water
1 part x 10% toluene = 1 part x 10/100 = 0.1 part of toluene
Thus, there are 0.7 part of ethanol; 0.2 part of water; 0.1 part of toluene in the mixture.
(a)      1 part of mixture + 4 parts of water:

Ethanol = (0.7 / 1 + 4) x 100% = 14%
Water = (0.2 + 4 / 1 + 4) x 100% = 84%
Toluene = (0.1 / 1 + 4) x 100% = 2%

From the phase diagram, this mixture is outside the area of the curve. Therefore, a clear single liquid phase of solution will be form.

(b)      1 part of mixture + 4 parts of toluene

Ethanol = (0.7 / 1 + 4) x 100% = 14%
Water = (0.2 / 1 + 4) x 100% = 4%
Toluene = (0.1 + 4 / 1 + 4) x 100% = 82%
From the phase diagram, this mixture is in the area of the curve. Therefore, a two liquid phase will form and the mixture is cloudy.

(c)        1 part of mixture + 4 parts of ethanol

Ethanol = (0.7 + 4 / 1 + 4) x 100% = 94%
Water = (0.2 / 1 + 4) x 100% = 4%
Toluene = (0.1 / 1 + 4) x 100% = 2%

From the phase diagram, this mixture is outside the area of the curve. Therefore, a single liquid phase of solution will be form and appear clear.


REFERENCE
    1.      Chang/Goldsby.2016.Chemistry Twelfth Edition.McGraw-Hill Education, USA:2 Penn Plaza, New York
    2.      Wikipedia,  Ternary Plot, updated on 15 November  2016 at 18:28


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