Determination of Alcohol in Antonov Through Simple Distillation

*Lee, Sharmine Margaret Cruz

Abstract

Vodka is composed principally of two ingredients, water and ethanol, with traces of few impurities and additives giving it 80 as its proof and 40 as its percent ethanol. The experimentation aimed to separate its major constituents, and to determine the percent concentration of ethanol by using simple distillation method. A calibrated volume of 20 mL vodka was placed in the distillation set-up and was heated constantly. A calibrated volume (0.5 mL or 10 gtt) of distillate was collected in every test tube pending the temperature until it reached close to 100 oC. The volume of distillate collected by the end of the distillation was 11.0mL at 98 oC, giving a percent alcohol of 55%.

Introduction Distillation is a method where in a mixture of liquids with sufficiently different boiling points can often be separated into its components. This is a purifying technique where it can be simply explained as a process of converting liquid to a vapour, condensing the vapour, and then collecting the distillate into a separate container. Vodka is colourless liquid, usually distilled from fermented grains such as sorghum, corn, rye or wheat. Water on the other hand is known to us as the universal solvent. The objective of the experiment is to (1) Separate the components of an alcoholic beverage (vodka) by using simple distillation, (2) Calculate the percentage of ethanol and percentage loss in vodka, and (3) Examine and observe simple carefully and at a better perspective. Methodology All the needed materials were equipped and cautiously set-up for the simple distillation procedures. The joints on each end were securely wrapped with masking tape to inhibit vapour loss and for the safety of these glass apparatus. Boiling stones were placed in the quick-fit distilling flask (3 pieces of boiling stones). A certain volume (20mL) of the sample beverage (vodka) was also added here. Subsequently, the flask was heated with an alcohol lamp which was continuously being rotated underneath the flask. A certain volume (0.5mL) of distillate was collected in calibrated test tubes until the set-up reached an approximate temperature of 98oC. Afterwards, the set-up was cooled and the volume of the residue was recorded. The first and the last distillate were collected for a flammability test. The temperature readings and the volume of the distillate gathered were plotted in a graph. The percent alcohol and percent loss were also considered in the experiment. distillation

Results & Discussion The quick-fit apparatus was used. The components of a quick-fit apparatus are (1) a pear-shaped flask, where the residue is placed, (2) a distilling head, which holds the thermometer to allow the temperature of vapours to be observed during the distillation process, (3) a liebig condenser which is a tube surrounded by a water jacket to cool and condense vapours, (4) a mercurial thermometer to measure the temperature, and (5) a receiver adapter that connects the condenser and receiver.

Fig.1. Simple Distillation Set-Up with a test tube as its receiving flask.

In the pear-shaped flask contained the 20mL sample of vodka and 3 pieces of boiling stones. The boiling stones were irregularly shaped. They are added to liquid samples to make them boil more smoothly. They provide nucleation sites so that the liquid boils easily without becoming superheated. The heating of the flask should gradually be rotated. However, if heating is too rapid and the condensate is pushed too rapidly, equilibrium between liquid and vapour will not occur and separation of the components will be substandard. If the flask is heated too strongly before the distilling head has been warmed by hot vapours and condensate, the still head may overflow, or show an unnecessary amount of liquid in one or more portions. The following table shows the result from the simple distillation: Test Tube 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 Volume (mL) 0.50 1.00 1.50 2.00 2.50 3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 8.50 9.00 9.50 10.00 10.50 11 Flame Test Blue

Table 1 illustrates that as the volume of distillate increases, the temperature also increases until the temperature closes to 100 oC. It is observed that they are directly proportional to each other. In this experiment, two distinct conclusions are obtained. The first corresponds to the component with the least boiling point which is separated first, and the second corresponds with the highest boiling point that is drawn off last. The component with the highest boiling point can be distilled and redistilled until it becomes pure. Daltons Law of Partial Pressure proves this theory stating that a mixture will only boil if the sum of the two partial pressures is equal to the atmospheric pressure. According to Raoults Law, 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. The theory of Daltons and Raoults law 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. The first test tube produced a blue flame which means that ethanol is present in the first distillate, while the drops collected in the final distillate did not produce any flame because alcohol has already been separated. It shows that as the distillation of the sample continues, there is a decreasing amount of alcohol being gathered in the separate test tubes. The first test tube contains the most alcohol compared to the succeeding test tubes used which contain a decreasing amount of ethanol. Figure 2 (found on the next page) shows that as the volume of temperature increases, the amount of distillate also increases. When the temperature reached close to 100oC, at about 98oC, the temperature stopped escalating and is constant as depicted by the straight lines in the graph.

Temperature oC 78 79 80 81 82 82 82 82 82 83 84 84 84 84 89 91 92 93 96 96 97 98

Negative

Table 1. Volume, Temperature and Flammability Test of the distillate

[1] Mayo, D.W., Pike, R.M. & Trumper, P. K. (2000).Microscale Organic Laboratory. 4 th ed. New York: John Wiley & Sons, Inc. pp. 617-651. [2] Whitten,K.W.,(2010). Chemistry. 9th ed. CA: Mary Finch. P.493 [3] Vodka.http://www.associatepublisher .com/e/v/vo/vodka.htm. June 29,2012 Using the formulas above, we will obtain the results:

Therefore, the percent alcohol of the sample is 55%. The percent loss of 10%, on the other hand, is the percentage loss. Simple distillation is used in separating components of liquid mixtures, which have boiling point more than 25C from each other at one atmospheric pressure. Fractional distillation separates liquid much better than simple distillation because of the glass beads present in the fractionating column. Simple distillation gives inferior separation than fractional distillation for it provides theoretical plates on which the refluxing liquid can condense, re-evaporate and condense again, essentially distilling the compound all over again.

References