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Experiment Title : PHASE DIAGRAM OF THE WATER-ETHYL ACETATE-PROPIONIC ACID TERNARY SYSTEM Name : Muhammad Zil-Ikram Bin Bahrudin

Lab Partners : 1. Ahmad Bukhari 2. Liew Yen Tze Valerie 3. Tee Rui Jing 4. Derek Goh Kah Sheng Date of Submission : 17 May 2012 Marker : Mohamad Rezuwan Shah Zakaria

Report Summary

1.0

Introduction 1.1 Abstract 1.2 Background Theory

2.0

Experiment Methods and Materials 2.1 Apparatus 2.2 2.3 Materials Procedures of Experiment

3.0 4.0 5.0 6.0

Results and Analysis Discussion Conclusion References

Abstract

This experiment was carried out purposely to determine the bimodal curve and the typical tie lines of the water-ethyl acetate-propionic acid system. The points on the bimodal curve was determined using the mass fractions of ethyl acetate, water and propionic acid of mixtures A to F after the propanoic acid was slowly added until a clear solution was obtained. The tie line was drawn using the mass fractions of ethyl acetate, water and propionic acid of mixtures S, T and U with the ratio of mass of E/mass of W using trial and error method. Three phase diagram was drawn in this experiment.

Theory

Separation process in which a solute in a feed stream is extracted by contacting the feed with a solvent is called solvent extraction. The solute has to be soluble in both the feed and solvent in order for the extraction to take place. The solvent and the feed for industrial extraction operations are normally partially soluble in one another. A ternary system will be formed consists of the feed, solvent and solute. The composition of such a system can be conveniently represented on an equilateral triangle plot with each corner of the triangle representing one of the three components. In this experiment, the three components are ethyl acetate (the solvent E), water (the feed W) and propionic acid (the solute A). The mixture of E-W-A may form a single phase or separate into two phases depending on the overall composition. The curve SEPQRSW separates the single phases from the two-phase region. It is variously referred to as the bimodal curve and E-W base line in the two-phase region and in the remaining area of the triangle plot is the single-phase region. It is essential to locate the bimodal curve in order to understand the operation of solvent extraction. A mixture, such as S, in the two-phase region will separate into two-phases an organic phase SE(rich in E) and an aqueous phase SW(rich in W). SE and SW lie on the bimodal cuve when equilibrium is obtained. Mass balance requires SE, S and SW to lie on a straight line. It is known as the tie line. The orientation of the tie line and the bimodal curve together determine the composition of phase SE and SW that are equilibrium with one another. Component balances require that Mass of SE/Mass of SW = Length of line SSW/Length of line SES. This is referred to as the Inverse Lever rule. This rule will be used to construct the tie line passing through a two-phase mixture.

EXPERIMENT METHODS AND MATERIALS

Apparatus Conical flask 100ml measuring cylinders with stopper Hanging weight of knows volume 4 decimal place balance Top loading balance Dropper

Materials Water Ethyl Acetate Propionic Acid

Methods of Experiment (A) Determination of Points M and N on the Bimodal Curve

(M) 20 g of water + 4g ethyl acetate

(N) 4g of water + 20g of ethyl acetate

Water was add to both conical flask to get clear phase

The weight of water use then recorded `

The weight of water used then recorded

(M)

(N)

(B)

Determination of point A,B,C,D,E,F on the Bimodal Curve Mixture as show in table 3.1 has been prepared

mixture of Ethyl Acetate and Water

Propionic Acid then been added slowly to each mixture and shake until the clear phase solution appeared

Then the weight of propionic acid use to obtained clear phase solution was recorded accordingly

(C)

Determination of Tie Lines

The mixture was prepared as in table 3.2

(S) 40g of Ethyl acetate 40g of Water 9g of Propionic Acid

(T) 37g of Ethyl Acetate 37g of Water 15g of Priopionic Acid

(U) 30g of Ethyl Acetate 40g of Water 20g of Priopionic Acid

The mixture was shake and allow for rest about 2 minutes to get two phase solution

The density for both aqueous and organic pahse, then determined by using the hanging weight and digital balance by using Archimedes Principle

mass of ME of the organic phase for each solution then been computed as well as the Mw of the aqueous solution. Then the ratio of ME /Mw calculated

Then, tie line of each mixture was plotted by using the inverse Lever Rule and the ratio of ME/Mw.

RESULTS AND ANALYSIS

(A)

Determination of M and N points on the Bimodal Curve

For M value Mass of H2O needed to get clear phase solution was 81.1g Mass of total solution after the existence of clear phase solution was 105.1g Mass percentage of Ethyl Acetate Mass percentage of H2O Mass percentage of Ethyl Acetate Mass percentage of H2O = = = = = 3.8 % = 3.8 %

For N value, Mass of H2O needed to get clear phase solution was Mass of total solution after the existence of clear phase solution was 300.5g Mass percentage of Ethyl Acetate Mass percentage of HsO Mass percentage of Ethyl Acetate Mass percentage of HsO = = = =

(B)

Determination of point A,B,C,D,E,F on the Bimodal Curve Ethyl Acetate ( g) Water ( g ) Prop ionic Acid ( g ) Propionic acid mass percentage (%) 23.5 29 31.3 33.7 26.1 22.8

Mixture

A B C D E F (C)

16 12 10 9 6 2

2 3 4 7 14 16

5.54 6.14 6.39 8.12 7.06 5.33

Determination of Tie Lines

Mixture

Ethyl Acetate ( g )

Water ( g )

Propionic Acid ( g )

S T U Mixture

40 37 30 V (m3) S T U 0.000003 0.000002 0.000002

40 37 40

9 15 20 Aqueous Mass (kg) 0.0026 0.0032 0.0023

Ehtyl Acetate Mass Fraction ( %) 44.94 41.57 33.33

Water Mass Fraction ( %)

Priopionic Acid Mass Fraction ( %)

Density (kg/m3) 866.67 1600 1150

44.94 10.11 41.57 16.85 44.44 22.22 Organic V (m3) Mass Density (kg) (kg/m3) 0.000002 0.0019 950 0.000002 0.0026 1300 0.000002 0.0020 1000

Mixture

S T U

Aqueous Initial Final 3 Volume(m ) Volume(m3) 0.00004 0.000043 0.000037 0.000039 0.000041 0.000043

Mass (g) 2.6 3.2 2.3

Organic Initial Final 3 Volume(m ) Volume(m3) 0.000094 0.000096 0.000094 0.000096 0.000095 0.000097

Mass (g) 1.9 2.6 2.0

Discussion

From experiment A, mass percentage of ethyl acetate and water are calculated from the M and N value. The bimodal curve was drawn using the mass fractions of ethyl acetate, water and propionic acid of mixtures A to F after the propionic acid was slowly added until a single phase clear solution is obtained. The densities for organic phase are calculated using desity=mass/volume and water phase also are calculated. The mass of SE and SW are calculated. The tie line was then drawn using the mass fractions of ethyl acetate, water and propionic acid of mixtures S, T and U with the ratio of mass of SE/mass of SW. Relationship of Mass of SE / Mass of SW = Length of line S SW / Length of line SE S also used in drawing the tie line by trial and error method.

The tie line for mixture S was unable to draw because of the errors occurred during the experiment. Some of the errors might included that the propionic acid was added in excess or insufficiently. So the amount of the solution needed for the mixture to turn clear may excesses the actual amount needed. Besides that, the solution was not confirmed 100% clear. The sensitivity of the measurement also was not good enough. Accuracy of the points draws using free hand may not accurate enough.

Conclusion As a conclusion, the orientation of the tie line and the bimodal curve together determine the composition of phase SE and SW that are equilibrium with one another. In order to get more accurate results, the experiment should be repeated several times.

References 1. Analysis of phase diagram, accessed on 16th May 2012


http://www.sciencedirect.com/science/article/pii/S0378517309008606

2. Ternary phase diagram,


http://www.sv.vt.edu/classes/MSE2094_NoteBook/96ClassProj/experimental/ternary2.html