University of Santo Tomas Faculty of Pharmacy Organic Chemistry Laboratory

The Percentage of Ethanol using Simple Distillation Method

*Urmaza,A.M; Valenton,J.G.; Villaceran,A.R.; Yap,K.M.; Zabala,K.; Zipagan,W.R.

Abstract
Vodka is composed primarily of water and ethanol with traces of impurities and flavorings and it has 40 percent alcohol by volume (80 proof). The experiment aimed to separate its components, alcohol and water, and to determine its percent concentration of ethanol by using the simple distillation method. A certain volume (30 mL) of vodka was placed on the distillation set-up and was heated constantly. A certain volume (0.5 mL) of distillate was collected in every test tube until the temperature reached close to 100 oC. The volume of distillate collected by the end of the distillation was 10.0mL at 99 oC, giving a percent alcohol of 33.33%.

Introduction Distillation is the process of purifying and concentrating a liquid through separating its components by heating it to the point of vaporization and collecting the cooled condensate in another container. This purifying technique is used to separate substances that have different boiling points. There are four types of distillation: simple, fractional, vacuum and steam distillation. Distillation can be use in purifying water or other substances and removing or separating the components of mixture such as the vodka. Vodka is colorless liquor, usually distilled from fermented grains such as sorghum, corn, rye or wheat. It is believe to be originated in the growing region of western Russia. It usually has an alcohol content of 40% [1-4].

The experiment aims to (1) separate the components of an alcoholic beverage (vodka) by distillation process, more specifically by simple distillation, (2) calculate the percentage alcohol and percentage loss in the alcoholic beverage (vodka) and (3) differentiate simple and fractional distillation techniques. Experimental In the experiment, all the needed materials were prepared and carefully set-up the simple distillation apparatus. The joints were tightly sealed with a masking tape in order to prevent vapor loss. The quick-fit distilling flask contains 3 pieces of boiling stones and a certain volume (30mL) of the sample beverage (vodka). After which, the flask was heated with an bunsen burner constantly being

rotated around the flask. In every test tube, a certain volume (0.05mL) of distillate was being collected and recorded until it reached 99oC. The set-up was cooled and the volume of the residue was recorded. The first and the last distillate were tested for flammability test. The temperature readings versus the volume of the distillate collected were plotted. The percent alcohol and percent loss were also calculated. Results & Discussion In the experiment, quick-fit apparatus was used. The components of quick-fit apparatus are (1)pear-shaped flask, where the residue is placed, (2) still head(distilling head), it holds the thermometer to allow the temperature of vapors to be monitored during the distillation, (3) liebig condenser, a tube surrounded by a water jacket to cool and condense vapors, (4) thermometer, measures the temperature, (5) receiver adapter, connects the condenser and receiver, (6) round bottom flask, where the distillate is placed.[1 & 2]. Refer to Fig.1. In a pear-shaped flask contains the sample and 3 pieces of boiling stones. The boiling stones are small, irregularly

shaped stones added to liquids to make them boil more smoothly.

Figure 1. Quick-fit apparatus Simple Distillation

They provide nucleation sites so the liquid boils easily without becoming superheated. The heating of the flask should be slowly rotated. When the solution boils, a ring of condensate rising up the still head can be observed. If heating is too rapid and the condensate is pushed too rapidly, equilibrium between liquid and vapor will not occur and separation of the components will not be satisfactory. If the flask is heated too strongly before the distilling head has been warmed by hot vapors and condensate, the still head may flood, or shows an excessive amount of liquid in one or more portions. [4].

The following table shows the result from the simple distillation:

the least boiling point which is separated first, and the second corresponds with the highest boiling point that is drawn off at the last. The component with the highest distilled boiling and point can until be it redistilled

Test Tube

Volume (mL)

Temperature o C

Flame Test
Positive

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
17 18 19 20

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

78 79 79 80 80 81 82 88 94 95 95 95 96 96 97 97
98 98 99 99

becomes pure [2]. According to Daltons Law of Partial Pressure, a mixture will only boil if the sum of the two partial pressures atmospheric according to is equal pressure. Raoults Law, to the And the

partial vapor pressure of a mixture in an ideal solution is equal to the vapor

Negative

pressure

of

that

pure

mixture times its mole fraction in the liquid. A mixture must not have a mole fraction of water that is 0.7 because it will not boil at 100oC and is less than atmospheric pressure. The concept of Daltons and Raoults law is that the vapor composition above a mixture is dependent both on the vapor pressures of the pure compound and on their mole fraction in the mixture [2 & 4].

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

Table 1 show that as the volume of distillate increase, the temperature also increases until it comes this to a point wherein two the temperature closes to 100oC. In experiment, distinct fractions are obtained. The first corresponds to the component with

In the flammability test, the first test tube produced a blue flame which means that ethanol is present in the first distillate, while in the 20th test tube, it did not produce flame because alcohol was removed. It shows that as the distillation of the sample continues, there is a decreasing amount of alcohol tube being contains gathered more in the separate test tubes. The first test alcohol compared to the last test tubes used which contain the last few drops of distillate.
T E M P E R A T U R E
o

temperature stopped from rising and is constant as showcased by the straight lines in the chart. The highlighted part is the azeotrope, which is a mixture that distills at a constant boiling point and with a constant composition. The boiling point of the azeotrope is lower than that of either pure component. Because boiling point is lower, the azeotrope component will distill in before a present excess.

Thus, the excess component will not distill as pure compound until the azeotrope has completely distill [2-4]. After flammability performing test, the the percent

120 100 80 60 40 20 0 0.5 1.5 2.5 3.5 4.5 5.5 6.5 7.5 8.5 9.5

alcohol and percent loss can then be computed using these formulas.

Volume (mL)
Figure 2. Temperature (oC) versus Volume (mL) of distillate

Figure 2 shows that as the volume increases, reached of the close distillate collected also the And so, using the formulas above, temperature to 100oC,

increases. When the temperature

distillation because of the glass beads in the fractionating column. Simple distillation than for it gives poorer provides separation Therefore, the percent distillation fractional

alcohol of the sample is 33.33%. The percent loss of 21.66%, on the other hand, is quite near compared to the original alcohol content of vodka. This explains that there is some part of the sample that is loss which was caused by evaporation due to the constant heating of the flask. The percent loss also shows that there is an excessive heating of the flask that caused the rapid evaporation of the sample or it can be caused by the mishandling of the test tube that caused to the careless collection of distillate [6]. Simple distillation is used in separating components of liquid mixtures, which have boiling point more than 25C from each other at one atmospheric distillation pressure. separates than simple Fractional

theoretical plates on which the refluxing liquid can condense, reevaporate and condense again, essentially distilling the compound over and over again. [2, 4 &6]. References [1] Mayo, D.W., Pike, R.M. & Trumper, P. K. (2000).Microscale Organic Laboratory. 4th ed. New York: John Wiley & Sons, Inc. pp. 617-651. [2] Pavia, D.I., et.al. (1999). Introduction to Organic Laboratory Technique: A Microscale Approach. pp 22-54. [3] Russell, C.A. Society (2000). and

Chemistry,

Environment: A New History of the British Chemical Industry. Royal Society of Chemistry. pp.69. [4] Fessenden, R.J., Fessenden, J.S. & Fiest, P. (2001) Organic Laboratory 77-96. Techniques. 3rd ed. California, USA: Brooks/Cole. pp.

liquid much better

[4]Vodka.http://www.associatepub lisher .com/e/v/vo/vodka.htm.

[6]Distillation.http://www.pharmpe dia. com/Distillation.