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Simple Distillation of Vodka (Cossack)

Katrina Marie Taracatac, Camile Vargas, Deric Vengua, Camille Rose Villegas, Howard William Wong Group 9, 2D-Pharmacy, Faculty of Pharmacy, University of Santo Tomas

Abstract
Distillation is the process by which components of a mixture are separated by boiling away the more volatile liquid. There are four types of distillation, namely vacuum distillation, steam distillation, fractional distillation and simple distillation. Fractional distillation involves the separation of two different substances based on the difference of boiling points which are closer to each other compared to simple distillation which involves substances with a more significant difference in their boiling points. The objective of this experiment was to separate the components of Cossack Vodka using simple distillation. The mixture was allowed to boil until an estimated temperature of 100 degrees Celsius was obtained. The distillate was collected in 0.5mL calibrated test tubes and used for the determination of the percentage of ethanol in the mixture and the percent of vodka lost. As a result, the group obtained 26.67% ethanol from the mixture, and a percentage loss of 5% from the experiment.

Introduction Distillation is one of the most common techniques for purifying and separating organic liquids. It was first discovered by the Greek alchemists and has been used since the olden times. Since then, the process has evolved greatly. Different apparatuses have now been made in order to make the process of distillation easier and faster. Distillation involves a few processes. The liquid mixture is first vaporized by boiling, then condensed back to a liquid which is called the distillate. This is collected in a separate flask or container. The liquid substance that is left in the original distillation flask after the whole process of distillation is called the residue. The boiling point of a liquid is defined as the temperature at which its vapour pressure equals the external pressure acting in the surface of the liquid. Boiling point plays an important factor when it comes to the process of distillation. A mixture having two different substances with different boiling points can be separated properly into their individual components using distillation. In this case, the substances to be separated were the ethanol and water mixture present in Cossack Vodka. The objective of this experiment was to perform the distillation process. Vodka was decided to be the mixture to be distilled. This experiment also aimed to separate the components of the alcoholic beverage properly, calculate the percentage of ethanol and the percentage of ethanol lost in the mixture, and lastly to differentiate the process of simple distillation from fractional distillation in terms of their efficiency. In order to do so, each group in class was tasked to perform either simple or fractional distillation. Simple distillation works well for most routine separation and purification procedures for organic liquids. It is best used when the boiling point difference of the two components to be separated is large. It can be effectively used if the substances to be separated have at least fifty degrees difference in their boiling points. Generally, this process was designed to evaporate a volatile liquid from a solution of non-volatile substance. In situations when the difference is lesser, it is advised to use fractional distillation. Fractional distillation is performed with the use of a fractionating column which is not present during simple distillation.

This report will be tackling the results obtained from simple distillation as it was the type of distillation process assigned to the group. Materials and Methods Materials The experiment required a microscale distillation set-up in order to be performed properly. This set-up consisted of a pear-shaped distilling flask containing boiling chips, a still head that was connected to a mercurial thermometer and a water condenser, and an adaptor. Other materials used in the experiment were iron stands, clamps, graduated cylinders, alcohol lamp which served as the source of heat, and a continuous water source. A sample of a simple distillation set-up can be seen below in Figure 1.0.

prepared. They were numbered accrodingly and each testtube was given a callibration of 0.5 mL. Thirty milliliters (30 mL) of Cossack Vodka was then placed into the pear-shaped distilling flask. An alcohol lamp was held beneath and continuosly rotated under the flask until the vodka started to boil. The temperature of the vodka during the first drop of distillate was recorded. The distillate on the first testtube, on the other hand, was kept for the future flammability test. There was a rapid drop of distillate succeeding the first one. The drops were all kept in the 0.5 mL callibrated test tubes, also, their temperatures were recorded. This was done in order to keep track of the total distillate collected, and to note the change in temperature in accordance to the volume of the mixture. The group was able to use all fifty test tubes but did not reach the maximum temperature of 100 C. The temperature ceased to increase when it reached the temperature of 94 C starting from the 44th test tube until the last. The distillate from the last test tube was kept for the flammability test. The remaining residue in the pear shaped distilling flask was also kept and measured for the future computations. Results and Discussion The group was not able to reach the maximum allowed temperature of 100 C. The temperature stopped increasing at a temperature of 94 C. Graph 1.0, below, will be a summary of the temperature versus the volume of the distillate collected during the duration of the whole of the experiment.

FIGURE 1.0 Simple Distillation Set-up

Method Prior to performing the distillation experiment, fifty test tubes were

GRAPH 1.0 Summary of Temperature (C) vs. Volume (mL)

Dalton's Law of Partial Pressure. This states that a mixture will only boil if the sum of the two partial pressures is equal to the atmospheric pressure. Second is the Raoult's Law, which states that the partial vapour pressure of a mixture in an ideal solution is equal to the vapour pressure of that pure mixture times its mole fraction in the liquid. A mixture must not have a mole fraction of water which is 0.7 because it will not boil at 100 C, which is water's boiling point. The notion behind these two laws is that the vapour composition above a mixture is dependent both on the vapour pressures of the pure compound and on their mole fraction in the mixture. A flammability test was performed on the first and last distillate collected. The first sample collected was tested to be flammable. This proves that ethanol was still present in the first drops of distillate in the experiment. The last drops of distillate were also tested, and no flame appeared. This proves that the last few drops were absent of ethanol. The last distillate was water. Both the percent of ethanol in the mixture and the percent of ethanol lost in the mixture were also computed using the following formulas

As seen in Graph 1.0 there was a constant increase of temperature as the volume of distillate increased. The relationship of the temperature and the volume of the distillate in the experiment was directly proportional to each other except for a few points in the beginnning of the experiment. When the temperature reached close to 100 C, the temperature stopped increasing and remained constant as seen through the straight lines in the graph. As seen in the graph there was a constant temperature of 78 C from volumes 6 mL up to 8 mL. This part is the azeotrope, which is a mixture that is distilled at a constant boiling point, with constant composition. The boiling point of an azeotrope is lower than that of both components to be separated. Because the boiling point is lower, the azeotrope will be distilled first before the components present in excess. As a result, the excess component will not be distilled as a pure substance until the azeotrope has first been completely distilled. There are two principles behind the process of distillation. First is

, and -

Using the formula above, the percentage of ethanol was computed

And the percentage of vodka lost

References Books: Ault, A., (1998). Techniques and Experiments for Organic Chemistry (6th Ed.). (pp. 70-83)

Therefore, the percentage of ethanol in the experiment was 26.67% which is quite far from the true value of 40% of ethanol present in Cossack Vodka. This though, may be explained because some of the ethanol might have been lost been lost during the constant heating of the flask. The percentage of vodka lost during the experiment was 5%. The percent loss shows that there was an excessive heating of the flask that caused the rapid evaporation of the sample or that this loss might have been caused by the mishandling of the test tubes that lead to the careless collection of the distillate. In conclusion, fractional distillation is more preferred to be used in the separation of water and ethanol. The boiling point of ethanol is 78.1 C, while water's boiling point is 100 C. The difference of their boiling points is 21.9 C, which is, as stated above, should be distilled by the process of fractional distillation since simple distillation needs a difference of at least 50 C in order to be done properly. Furthermore, fractional distillation is more accurate compared to simple distillation because fractional distillation uses a fractional column which provides an efficient exchange of heat and material between the condensate flowing down the column and vapours flowing up. By the use of a fractional column, there is a repeated cycle of condensing and vaporizing in the substance. This produces a more pure distillate compared to the ones given off by simple distillation.

Fessenden, R., Fessenden, J, & Feist, P. (2001). Organic Lab Techniques (3rd Ed.). (pp. 77-91) Landgrebe, J. (1993). Theory and Practice in the Organic Laboratory with Microscale and Standard Scale Experiments (4th Ed). (pp. 142-160) Pavia, D., Lampman, G., Kriz, G., & Engel, R. (2005). Introduction to Organic Laboratory Techniques: A Small Scale Approach (2nd Ed.). (pp. 733-746) Whitten, K., Davis, R., Peck, M., & Stanley, G. (2010) Chemistry (9th Ed.). (p. 463)

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