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Lara Melissa V. Ferrer Section 3 ChE A Group No.

Date Performed: January 4, 2013 Date Submitted: February 15, 2013

Experiment No. 2 PARTIALLY MISCIBLE LIQUIDS: DETERMINATION OF MUTUAL SOLUBILITY

Introduction A mixture of liquids is a homogeneous distribution of two or more substances, whereby all components have a definite vapour pressure. Two liquids may either be completely miscible or only partly miscible. When the van der Waal forces between the two components are smaller than those between molecules of the same type, then an increase in the vapour pressure occurs. The molecules can leave their arrangement more easily than with equally large attractive forces. 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. On the other hand, liquids tend to be immiscible when attractions between like molecules are much stronger than attractions between mixed pairs. The experiment is simply about the determination of mutual solubility of two liquids like water and phenol that are partially miscible. Thus, helps in the construction of mutual solubility curve of the liquids and in the determination of their critical solution temperature.

Methodology Preliminary procedures were done before the actual experiment. The density of phenol was obtained from literature and the amount of water required to prepare 5% to 95% phenol at 5% increment, starting with 10 mL phenol in each proportion, was calculated. 95% phenol-5% water by weight mixture was prepared based on 10 mL phenol. The mixture was heated with mild stirring until the cloudiness disappeared, the temperature of which was recorded. The mixture was then cooled with mild stirring until the cloudiness reappeared, the temperature of which was recorded. The process was repeated until fairly constant readings were observed. Water was added to make 90% phenol and 10% water. The procedure was repeated until 55% phenol. For 5% to 50%, 5 mL phenol was initially used. Below is a sample figure of the setup of the experiment.

Water Bath

Hot Plate

Fig. 1 95% sample-5%water mixture in a water bath

Results and Discussion The data presented below were the results of the experiment Phenol-water mixtures ranging from 5% to 95% at 5% increment of water using 10mL phenol sample were subjected to heat until cloudiness disappears. Subsequently, the mixtures were cooled down and the temperatures were recorded at which turbidity, as a result of separation, becomes visible. Table 1. The Analysis of the Solubility of Phenol-Water Mixtures at Increasing and Decreasing Temperatures % phenol 95 90 85 80 75 70 65 60 55 50 45 40 35 30 25 20 15 10 5 T (cooling) No change No change 30 35 42 46 50 54 59 63 60 55 49 44 40 38 37 No change No change T (heating) No change No change 31 42 56 63 68 70 86 66 64 60 57 55 46 42 41 No change No change

Table 1 shows the temperature readings during heating and cooling of the mixtures. The ones recorded during heating were the temperatures when cloudiness in the

mixtures was seen disappearing. On the other hand, those noted during cooling were the readings obtained at such a time when turbidity in the solutions was observed to be reappearing. When turbidity was observable, phenol and water were forming layers, and could be seen to be partially miscible. However, during heating, turbidity was gradually disappearing. Phenol and water then became one. Such increase and decrease in temperature greatly affected the solubility of the two liquids. Figure 1 shows the construction of mutual solubility curve of phenol-water mixture. A range of concentrations in which the two liquids form two phases is also shown below. This is important in the determination of critical solution temperature at which a mixture of two liquids, immiscible at ordinary temperatures, cease to separate into two distinct phases. The red dashed line symbolizes the temperature reading of phenol in the hot water bath while the blue dashed line represents the temperature reading of phenol in the cold water bath.

Mutual Solubility Curve


100 90 80 70 60 50 40 30 20 10 0 0 20 40 60 80 100 % weight of Phenol

Temperature

T (cooling) T (heating) Poly. (T (cooling)) Poly. (T (heating))

Fig. 2 Analysis of the Mutual Solubility Curve of Phenol-Water Mixture

The left side of the curve shows solutions of phenol in water, and the right side of water in phenol. Unmixing means transition to a lower energy condition. It occurs within the area of the miscibility gap under the formation of two phases, the compositions of which correspond to the abscissa values at the temperature concerned. If we mix phenol and water at 50C in a ratio of 1:1, then unmixing occurs. In these separation curves, the compositions of the two coexisting liquid phases, which form from the homogeneous mixture when a certain temperature has been reached, are plotted. The coexisting liquid phases are described as conjugated solutions. They are saturated solutions of the one component in the other. The line connecting the coexisting liquids is designated as the tie line. Normally the mutual solubility of liquid components increases with increasing temperature. The coexisting solutions are identical at a critical dissolving temperature. Above the critical dissolving temperature the components are miscible with one another in any ratio. The compositions of the coexisting solutions at certain temperature are constant and independent of the mass ratios or the two components. Answers to Questions

1. Based on the plot, is there a maximum and /or minimum critical solution temperature? What is the critical temperature? Compare this with the literature value.

Two types of liquid-liquid critical points are the upper critical solution temperature, or, which denotes the warmest point at which cooling will induce phase separation, and the lower critical solution temperature, which denotes the coolest point at which heating will

induce phase separation. Based on Figure 2, the maximum temperature is 72C and the minimum critical solution temperature is 58C.

2. Are the different temperature readings constant for cooling and heating of the same weight percent phenol-water mixture? If not, explain these differences. The different temperature readings have almost small differences. Thus, the temperature readings were constant. 3. Explain why at high sample concentrations the solution solidifies during the cooling process. The high phenol concentration of percentage of phenol-water mixture solidifies during cooling process mainly because of phenols freezing point. Phenol forms into a solid that can be liquefied by a very small amount of water. Thus, a high concentration solution of phenol with water would solidify on lower temperatures.

4. Suggest a procedure by which the composition of a layer can be determined experimentally. Given an unknown solution of the components, its concentration will be known by the use of the mutual solubility plot/graph. The composition of a layer can be determined by getting the critical solution temperature experimentally and plotting the point on the graph. The weight percentage could be obtained at the point where in the temperature intersects the curve.

Conclusion Based on the results of the experiment, it is concluded that phenol and water are two partially miscible liquids. They become more soluble in each other with increasing or decreasing temperature until such time that the critical solution temperature is attained. It is the point when a mixture of two immiscible liquids at ordinary temperature ceases to separate into two distinct phases. Also, solubility of mixtures is greatly affected by factors like temperature, nature of solute and solvent, as well as pressure. If the solution process absorbs energy, then solubility increases as the temperature is increased. If the solution releases energy, then solubility decreases with increasing temperature. Another important feature is the turbidity or cloudiness. It is the indicator of whether the mixture is mixed or unmixed.

References

1. Ayiralam, Subhash C. and Dandina N. Rao. Solubility, miscibility and their relation to interfacial tension in ternary liquid systems. Fluid Phase Equilibria 249.1 (2006): 82-91. 2. Dai, Ming and Jian-Ping Chao. Heats of mixing of the partially miscible liquid system cyclohexane + methanol. Fluid Phase Equilibria 23.2 (1985): 315-319. 3. Davarnejad, R, K.M Kassim and A Zainal. Mutual solubility study for 94.2:5.8 of ethanol to octane with supercritical carbon dioxide solvent. Journal of the Chinese Institute of Chemical Engineers 39.4 (2008): 343-352.

4. Gerbaud, Vincent;Liaw,Horng-Jang.Flash point prediction for binary partially miscible aqueousorganic mixtures. Chemical Engineering

Science.Vol63,Issue18(September2008) 5. Gramajo, Monica;Marigliano, Ana; Influence of temperature on the liquidliquid equilibria containing two pairs of partially miscible liquids. Fluid Phase Equilibria256.2(1998):78-83 6. Logan, R.S. The Behaviour of a Pair of Partially Miscible Liquids. Chemical Education 75.339 (1998): 206-208. 7. Sadus, Richard J and Ya Song Wei. Equations of state for the calculation of fluid-phase equilibria. AIChE 46.1 (2000): 169-296. 8. Slonimski, G.L. Mutual solubility of polymers and properties of their mixtures. Journal of Polymer Science 30.121 (1958): 625 637.

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