University of Santo Tomas Faculty of Pharmacy Organic Chemistry Laboratory

Determination of Alcohol in Cossack Vodka Sample Using Simple Distillation Method

Abstract Vodka is a distilled beverage and one of the world's most popular liquors. It is composed primarily of water and ethanol with traces of impurities and flavorings. Its alcoholic content usually ranges between 35-50% by volume. The experiment was conducted for the purpose of separating the components of Cossack Vodka, which are ethanol and water. In order to determine the percentage ethanol that it contains, distillation process was performed, specifically simple distillation. Distillation is the process wherein components are separated from one another based on their boiling points. A volume of 20 mL was heated in the distillation set-up. At the end of the experiment, 11 mL of distillate was collected at 98 oC. The percentage of ethanol in the Cossack Vodka sample was found out to be 55%. Introduction Distillation is a process of converting liquid to a vapor, condensing the vapor, and then collecting the distillate in another container. This purifying technique is used to separate components in a liquid mixture which have different boiling points, or to separate a component that is not volatile. Among the various types of distillation are simple distillation, fractional distillation, vacuum distillation, and steam distillation. In this experiment, simple distillation was used to separate the components of Cossack Vodka. The experiment aims to (1) separate the components of an alcoholic beverage (vodka) by distillation process, (2) construct a distillation curve, (3) calculate the percent

ethanol in the alcoholic beverage (vodka), and (3) compare the efficiency of simple and fractional distillation in separating the liquid mixture. The method of distillation performed by the group is simple distillation. Thus, this report would focus mainly on the said method of distillation. Methodology To start with, e 20 13x100 test tubes were calibrated to 0.5mL. These were used to receive the distillate. Then, distillation set-up was prepared and assembled. In this experiment, quick-fit apparatus was used. The components of the quick-fit apparatus are (1) pear-shaped flask, where the residue was placed, (2) still head (distilling head), which held the thermometer to allow the temperature of vapors to be monitored during the distillation, (3) Liebig condenser, a tube surrounded by a water jacket which cooled and condensed vapors, (4) thermometer, which measured the temperature, (5) adapter, which connected the condenser and receiver, and (6) round bottom flask, where the distillate was placed. The joints were tightly sealed with a masking tape in order to prevent vapor loss. Moreover, 2 iron stands, were also usedone for the support of the condenser and the other is to hold the distilling flask in place. The distilling flask was placed on top of a tripod or an iron ring supported by a wire gauze above to prevent the breakage of the glassware due to direct heat. [Refer to Figure 1]

Figure 1: Distillation Set-up After the preparation of the set-up, 20mL of vodka was placed in the distilling flask and 3 boiling chips were added. These are small, irregularly shaped stones added to liquids

to make them boil more smoothly. Then, the water was gently turned on. The alcohol lamp was lit up and placed directly below the distilling flask. Rotation of the alcohol lamp is important in order to control the distribution of heat. The temperature was recorded on the first drop, and after every 0.5mL of the distillate collected. The temperature and the corresponding volume of distillate were recorded during the entire distillation process. The collection of the distillate was stopped as soon as the temperature reached 98 oC. After the distillation process, flammability test was performed. This required the use of a watch glass, a source of flame (preferably a match), and the 1st and last distillate collected. An amount of 3-5 drops of the 1st distillate was placed on the watch glass and was lighted with a match. The same process was repeated to the last distillate from the last test tube.

Results and Discussions The set up required the addition of boiling stones because they provide a nucleus on which gas bubbles grow, therefore avoiding the sudden production of large gas bubbles which can lead to 'bumping'. This is called succession; it can cause liquid to splash over into the condenser and therefore produce an impure product. Severe bumping can even lead to loss of material through vents or can blow a distillation apparatus apart.

Table 1: Volume and Temperature of the Distillate

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 Temperature (oC) (mL) 0.50 78 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 11.00 79 80 81 82 82 82 82 83 83 84 84 84 84 89 91 92 93 96 96 97 98

Table 1 shows the progress in temperature of the sample in relation to the increasing volume. It could be seen that as the volume of distillate increase, the temperature also increases until it comes to a point wherein the temperature is close to 100oC. In this experiment, two distinct fractions 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 at the last. Ethanol has a lower boiling point than water. It is more volatile so it is expected that ethanol will be the first distillate. The first distillate was collected at 78oC. The collection was stopped when 98 oC was reached, totaling an amount of 11 mL distillate.

100 95 90 85 80 75 70 65 60 55 50 45 40 35 30 25 20 15 10 5 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 6 6.5 7 7.5 8 8.5 9 9.5 10 10.5 11
Volume (mL)

Temperature (oC)

Figure 2: Graphical Representation of the Volume and Temperature of the Distillate Figure 2 shows the relationship between the volume and the temperature during the collection of the distillate. As the volume of the distillate collected increases, the temperature also increases. Table 2: Results of Flammability Test Distillate First Distillate Last Distillate Result Flammable Inflammable Component Ethanol Water

In the flammability test, the first test tube produced a yellowish-orange flame with only the tip being blue in color, which means that ethanol is present in the first distillate. On the other hand, in the last test tube, it did not produce flame because alcohol was removed. It shows that as the distillation of the vodka continues, there is a decreasing amount of alcohol being gathered in the separate test tubes. The first test tube contains more alcohol compared to the last test tubes used which contain the last few drops of distillate. After performing the flammability test, the percent alcohol and percent loss were computed: Percentage Ethanol

Percentage Loss

The total percentage alcohol of the sample is 55%. The percent loss, however, is 10%. This loss could be caused by various factors including the excessive heating of the flask which may have caused the sample to evaporate rapidly, the wrong calibration of the 0.5 mL test tubes, the collection of the distillate, the incorrect reading of the residue, or the room temperature which may have affected the temperature while heating.

Based on the results obtained, it can, therefore, be concluded that simple distillation is efficient to use only when the components of a compound or a mixture has very far boiling points. Fractional distillation, as compared to other groups experiments, produce more accurate results. Thus. it is more efficient to use since the boiling points of the chemical in the mixture are near to each other. References Bayquen, A., Cruz, C., et al. (2009). Laboratory Manual in Organic Chemistry. Quezon City, Philippines: C & E Publishing, Inc. Davis, R., Peck, L., Stanley, G. & Whitten, K. (2010). Chemistry. 8th ed. Belmont, CA: Thomson Corporation. http://en.wikipedia.org/wiki/Boiling_chip http://en.wikipedia.org/wiki/Quickfit_apparatus http://scribd.com/doc/36247410/ Distillation-of-Alcohol-in-Vodka http://yourchemistryonline.blogspot.com/2012/01/separation-techniques.html