Department of Pure and Applied Chemistry College of Arts and Sciences Visayas State University Visca, Baybay City,

Leyte Chemistry 152 Physical Chemistry II Aprilyn R. Daas Performed: November 23, 2011 Group No. 1 Submitted: December 5, 2011 Experiment No. 1 Date Date

BINARY MIXTURES
Objectives To determine the refractive index of the mixture To determine the composition of the binary mixture Procedure 1. 2. 3. 4. 5. Assemble the distillation apparatus. Add 40 mL of the water-ethanol mixture into the RBF and add a few boiling chips. One mixture is 99% ethanol and another mixture is 80% ethanol. Label 10 sample vials with these temperatures and whether it comes from the boiling flask or the end of the condenser Cautiously begin heating. Adjust the heating rate so that the mixture distills slowly, approximately one drop every 2 - 3 seconds. Be careful not to burn yourself. As the temperature approaches the first collection point, obtain the first pair of sample vials and prepare them for sample collection. When the temperature reaches the first collection point, one lab partner will quickly withdraw a sample of approximately 0.5 mL from the boiling flask and one will replace the volumetric cylinder with the appropriate sample vial and collect 0.5 mL. of sample from the condenser. When the samples have been collected, immediately replace the caps to prevent selective evaporation of the ethanol. While one lab partner analyzes the samples for its refractive index, the other lab partner will continues to record the temperature and volume. Terminate the distillation by turning off the power when only 2-3 mL of liquid remains in the flask - never allow the flask to boil dry.

6.

Results and Discussion Binary mixtures of two volatile liquids exhibit a range of boiling behavior from ideal, with a simple continuous change in boiling point with composition, to nonideal, showing the presence of an azeotrope and either a maximum or minimum boiling point. The goal of this experiment is to carry out a simple distillation of a liquid binary mixture of two organic substances, ethanol and water, analyze the contents

of samples collected from both the liquid and vapor phase during the distillation, and create a liquid - vapor composition diagram. To a reasonable degree such hydrocarbons behave as ideal binary mixtures for three reasons: (1) their gas - liquid equilibria can be described by Raoult's law; (2) they obey Dalton's law of partial pressures; and (3) their vapor pressures as a function of temperature can be approximated by the Clausius - Clapeyron equation. A mixture of ethanol and water, at different concentrations, were distilled and sample and distillate are collected to obtain the refractive index of the mixture. First different mixtures were done and their refractive indexes were obtained. Table 1. Refractive index for the water-ethanol mixture standards % ethanol Refractive index 0 -1 20 6 40 12 60 16 80 18 100 19 After obtaining the refractive index of the binary mixture, it was plotted to obtain the calibration curve. It has a slope of 0.2 and an r2 of 0.917.

Figure 1. Calibration curve for the water-ethanol mixture In the case of mixtures of ethanol and water, minimum occurs with 95.6% by mass of ethanol in the mixture. The boiling point of this mixture is 78.2C, compared with the boiling point of pure ethanol at 78.5C, and water at 100C.

Figure 2. Phase diagram for water-ethanol mixture For the distillation of 99% ethanol and 1% water, samples were collected from the vapor and liquid phase and their refractive indexes are obtained using a handheld refractometer. Table 2. Refractive indexes of the distillate and sample of 99% ethanol-1%water mixture 99% ethanol Refractive index Temp distillate sample (C) A 65 13 14 B 68 14 15 C 70 15 17 D 73 16 18 E 75 17 19 F 78 18 19 Since the mixture of ethanol and water that was distilled is richer in ethanol than the azeotrope, the distillate will be poorer in ethanol than the original but slightly richer than the azeotrope. This means the solution left behind will be richer in ethanol. As seen in the graph, refractive index increases. It coincides with the graph in Fig.2.

Figure 3. Phase diagram of the 99% ethanol-1%water mixture For the 80% ethanol-20% water mixture, distillation will not be able to completely separate the two components. Either the distillate or the residue will eventually reach the azeotropic composition and no further separation will occur. Table 3. Refractive indexes of the distillate and sample of 80% ethanol-20%water mixture 80% ethanol Refractive index Temp( distillate sample C) A 79 14 8 B 79 12 9 C 79 9 10 D 79 8 11 E 79 7 12

Figure 4. Phase diagram of the 80% ethanol-20%water mixture Distilling the 80/20% mixture produces a distillate that is 87% ethanol and 13% water. Further repeated distillations will produce mixtures that are progressively closer to the azeotropic ratio of 95.5/4.5%.

However, Fig. 3 and Fig. 4graphs does not coincide perfectly with the graph in Fig. 2 because of the variations that occurred during the experiment. Temperature also is not stable so the vapor also changes in response to the change in temperature. And also the calibration curve does not have an r2 of 0.9999. Conclusion It can be concluded that in order to obtain the refractive index of a binary mixture, first one must set up a calibration curve and be able to draw the phase diagram of the mixture. Then the mixture can be distilled and samples and distillate be collected and its refractive indexes obtained to be able to construct binary phase diagram. References www.winegrowers.info www.chemicalforums.com Kister, Henry Z. (1992). Distillation Design (1st Edition ed.). McGraw-Hill.