Percentage of Ethanol in Vodka Using Fractional Distillation

Earl Christian *Mantes, Vicente Martires III, Jaira Lyn Mauhay, Marlon Mejia, & GRalz Olasiman Abstract Vodka is an alcoholic beverage having a percentage of ethanol of 40% (80 proof) theoretically. The experiment aimed to separate its components in order to find out if the theoretical value is factual. This was accomplished by performing a fractional distillation in which a 30 mL sample of vodka was introduced into a quick-fit fractional distillation set-up. The process was stopped when a temperature of 98oC was reached. A total of 11 mL of distillate was collected in the entire duration of the process. The effectiveness of the distillation process was checked by performing a flammability test on the first and last distillates wherein the first distillate rendered positive whereas the last distillate rendered negative. After performing the necessary calculations, an experimental percentage of ethanol was obtained which was 25.67%. Furthermore, the process has a percentage loss of 13.33% and a percentage of error of 33.33%.

Introduction
Vodka is a distilled liquor composed primarily of water and ethanol. It ranges in alcoholic content from about 40 to 55%[1]. In the United States, the fairly preferred alcoholic content of vodka is 40% or 80 proof. The alcoholic content of vodka, or any other liquor, is expressed as alcohol by volume (ABV) which is the strength of an alcohol measured as the percentage of alcohol (ethanol) contained in the liquid[2].This value can be computed by using the formula:

In fractional distillation, or distillation per se, the difference in boiling points of the substances in a mixture is the principle involved. In vodka, the substances under focus are ethanol and water. Ethanol is expected to boil at 79oC while water is expected to boil at 100oC. The experiment aims to separate these components (ethanol and water) of vodka through fractional distillation. It also aims to calculate the percentage of ethanol present in the vodka after performing the distillation process.

Methodology
Before performing the experiment, the required materials were completely gathered. These were the quick-fit apparatus, alcohol lamp, boiling stones and vodka. 40 test tubes were also calibrated down to the 0.5 mL mark. After the preparations, the quick-fit apparatus was carefully set up. A typical fractional distillation set-up is shown in Fig. No. 1. Instead of a round-bottom distilling flask as seen in Fig. No. 1, a quick-fit pear-shaped distilling flask was used. 30 mL of vodka was introduced into the flask together with 3 pieces of boiling stones. The flask was then secured to an iron stand through an iron clamp. This was connected to the fractionating column which was also held in place by an iron clamp. The stillhead was put on top of the fractionating column and the thermometer was inserted into it. Afterwards, the condenser was connected to one end of the stillhead, and was secured in another iron stand through a third iron clamp. A rubber tubing was

Alcohol proof is another measure of how much ethanol is contained in an alcoholic beverage. In the United States, the following formula is used to determine alcoholic proof: In the experiment, the factuality of a sample of vodkas alcoholic content printed in its label was tested by performing a process called fractional distillation. Fractional distillation is explained as the process of separating a mixture of two or more volatile substances into its components by causing the mixture to vaporize by suitable application of heat, condensing the vapors in such a way that fractions of varying boiling points are obtained, re-vaporizing these fractions and separating their vapors into similar fractions, combining fractions of similar boiling points, and repeating until the desired degree of separation is finally obtained[3].

connected from the water tap to the water inlet of the condenser in order to provide water for the cooling down of the vapors coming from the fractionating column. Another rubber tubing was also connected to the water outlet which allowed water coming from the inlet to flow towards the sink. A 0.5 mL calibrated test tube was used as a receiver instead of an Erlenmeyer flask as shown in Fig. No. 1. Furthermore, no adapter was utilized in the experiment. Once the set-up was ready, the temperature was read. Then, the alcohol lamp was lighted and placed beneath the distilling flask instead of an electric heater as seen in Fig. No. 1.
Thermometer stillhead Water outlet Iron stand Iron clamp condenser Water inlet adapter Fractionating column Distilling flask Source of heat receiver

After doing so, the percentage of ethanol, percentage loss, percentage of error and proof were calculated.

Results

Graph No. 1. Relationship between the volumes of distillate collected to the temperatures recorded It is shown in Graph No. 1 that in the entire duration of the distillation process, a total of 11 mL of distillate was collected through 22 0.5 mL calibrated test tubes. Moreover, the first temperature reading (at 0 mL mark) was recorded at 33oC and the last temperature reading (at the 11 mL mark) was 98oC. The value within the shaded rectangle represents the volume of ethanol (boiling point = 79oC) which is 8 mL (from 9 mL 1 mL). Table No. 1. Flammability test on the first and last distillate and their components based on the flammability test
Flammability Test Components First Distillate Flammable Ethanol Last Distillate Non-flammable Water

Fig. No. 1. Typical Fractional Distillation Set-up When the first drop of distillate was collected, the temperature was again recorded. After being able to collect 0.5 mL of distillate, the test tube was labeled as first distillate and was stored. Another 0.5 mL calibrated test tube was then used to replace the previous one in its purpose of distillate collection. Every time a test tube was filled to the 0.5 mL mark, the temperature was read and the test tube was replaced with another one. After reaching 98oC, the distillation process was stopped. The last test tube used was labeled as last distillate and was stored again. 3-5 drops of distillate were taken from the first and last test tubes used and were expelled on two separate watch glasses. A flammability test was performed by lighting each distillate.

It is expressed in Table No. 1 that the first distillate rendered positive in the flammability test while the last distillate rendered negative. Hence, it was deduced that the first distillate was composed of ethanol while the last distillate was composed of water. Calculations:

with a lighted match. This is the reason behind the flammability of the first distillate (Table No. 1). The first distillate was composed of ethanol. However, the second distillate rendered negative in the flammability test because it was only composed of water which is non-flammable. After computing for the percentage of ethanol in the vodka sample, it was found out that the sample had an alcoholic content of 26.67% or 53.34 proof. This is very far from the theoretical alcoholic content of vodka which is 40% or 80 proof. Also, the experiment had a percentage loss of 13.33%. This might have contributed to the 33.33% error of the experiment.

Conclusion
If performed correctly, fractional distillation is very effective in separating the components of a mixture, especially if their difference in boiling point is very close. In the experiment, the difference between the boiling points of ethanol and water is 21oC [from 100oC (b.p. of water) 79oC (b.p. of ethanol)]. However, the performed experiment resulted in a lower value of alcoholic content and a high percentage of error. This may be due to certain errors in the distillation set-up and process. To elaborate, too much vapors may have escaped the fractionating column, thus resulting in a lower turn out of distillate because those vapors did not condense. Moreover, some distillate may not have been collected during the act of replacing the test tube used in the collection. Some may not have flowed out of the condenser. These also result to a lower turn out of distillate collected. Hence, upon computation, the percentage of ethanol was greatly reduced. The experiment had a percentage loss of 13.33%.which means that about 4 mL of sample was lost in the experiment due to certain errors and evaporation. If this value is added to the volume of ethanol which is 8 mL and then used to calculate for the percentage of ethanol, the value would be 40% which is equal to the theoretical alcoholic content of the vodka sample. Thus, it is recommended that the experimenters be careful next time in performing the distillation process again so that the errors will be minimized.

Based on the calculations, the sample of vodka has an alcoholic content of 26.67% ethanol; the percentage loss of the experiment was 13.33%; the percentage of error was 33.33%; and the alcoholic proof was 53.34.

Discussion
Separation of components from a liquid mixture via distillation depends on the differences in boiling points of the individual components[4]. This was proven by the data recorded from the experiment (Graph No. 1) wherein the temperature reading appeared almost flat and constant at 79oC until 83oC. This was due to the fact that during this period in the distillation process, the ethanol component was being vaporized. After all the ethanol was distilled, the temperature began to rise a little rapidly until it reached 98oC which is close to the boiling point of water. During this point in the process, water was already starting to vaporize. Ethanol is highly flammable and has a flash point of 9-11oC[5]. Flash point is the lowest temperature where enough fluid can evaporate to form a combustible concentration of gas. It is an indication of how easy a chemical can burn[6]. Hence, ethanol can easily combust upon contact

References
[1] Lotha, G.; & Editors of Encyclopdia
Britannica. Vodka. http://www.britannica.com/EBchecked/to pic/631781/vodka 07/21/12. [2] Glossary of Whisky and Distillation. http://www.celticwhisky.com/glossary.htm 07/21/12. [3] Clark, S.R.; & Edwin, R.G. (1950). Elements of Fractional Distillation. 4th

Edition. USA: McGraw-Hill Book Company. Inc. [4] Tham, M.T. Distillation Principles. http://lorien.ncl.ac.uk/ming/distil/distilpri.h tm 07/21/12. [5] National Pollutant Inventory. Ethanol (ethyl alcohol): Overview. http://www.npi.gov.au/substances/ethano l/index.html 07/21/12. [6] Flash Point Fuels. http://www.engineeringtoolbox.com/flashpoint-fuels-d_937.html 07/21/12.