FRACTIONAL DISTILLATION

Jan Michael V. Salcedo, Bea Marie B. Samar, Maria Ysabel O. San Juan, and Gabriel Jerome M. Sandimas Group 8 2G Pharmacy Organic Chemistry Laboratory

ABSTRACT
Distillation is a commonly used method for purifying liquids and separating mixtures of liquids into their individual components. It is used for many commercial processes, such as production of gasoline, distilled water, xylene, alcohol, paraffin, kerosene, and many other liquids. There are two types of distillation, simple and fractional. The group was assigned to perform fractional distillation. The sample used for the experiment was Vodka. It was distilled and heated continuously by alcohol lamp until the temperature reached 100C. The distillates were collected using the calibrated and numbered test tubes. The first distillate collected undergone flame test and a formation of blue flame was observed. The percentage of ethanol was computed by getting the ratio of the volume of azeotrope and the total volume of the sample multiplied by 100. The percentage of ethanol was 10%. The percentage loss was also computed by getting the ratio of the total volume of sample minus the sum of distillates and residue, and the total volume of the sample multiplied by 100. The percentage loss was 3.33%.

INTRODUCTION
Distillation separates compounds using a closed system consisting of a "still" to which heat is applied, a "condenser" in which the vaporized substance cools to a liquid and a "receiver" that captures the condensed liquid. Substances are separated and vaporized by applying heat until the still reaches the "boiling point" of the substance that is to be separated.[4] Basically, this process involves the heating of a liquid and separating the condensed vapors. Purification of a compound uses distillation by separating it from a non-volatile or a less-volatile material. Boiling point plays an important role in distillation. In a mixture, if two different compounds that have different boiling points are distilled properly, they can be separated into individual components. Such is the case with the ethanol-water mixture present in vodka.[7] There are two common processes in distillation, Simple and Fractional Distillation. Simple distillation is the method used to separate substances in mixtures with significantly different boiling points. This set-up will only have one distillation (vaporization-condensation) cycle. On the other hand, Fractional distillation is used for mixtures containing chemicals with boiling points close to each other. This set-up will have at least two (vaporization-condensation) cycles. It also uses fractionating column which acts as a minor obstruction to the rising gas and will prevent the not so pure vapor from passing through.[3] There are two principles that lie in the experiment, Raoults Law and Daltons Law. Raoults Law connotes that the vapor pressure of a solution equals the product of the vapor pressure of the pure solvent and the mole fraction of solvent while Daltons Law, which is also known as Law of Partial Pressure, implies that the pressure of a gas mixture is equal to the

sum of the partial pressures of the gases composing it.[6] In this experiment, the group should be able to attain the following objectives: (1) to be able to separate the components of an alcoholic beverage, (2) to differentiate simple from fractional distillation, and (3) to calculate the percentage of ethanol in a beverage.

EXPERIMENTAL
A. Compounds tested (or Samples used) Vodka is the sample used for distillation. B. Procedure The group used Fractional distillation to examine the presence of ethanol in the alcoholic beverage. Before starting the experiment, the set-up was prepared and tightly secured using clamps and iron stand. Several test tubes were calibrated down to 0.5mL for accurate volume of distillates. Boiling stones were put into the pear shaped flask and 30mL of vodka was introduced. By rotating the alcohol lamp, the flask was continuously heated until the vodka started to boil. The temperature was recorded at the first drop of the distillate. The remaining calibrated and numbered test tubes are still filled with 0.5mL each of the distillate and temperatures were recorded. Collection of distillates stopped when temperature reached 98C. Three to five drops of the distillate from the first test tube are placed on a watch glass then lighted match was applied. Same procedure was observed on the distillate from the last test tube.

Table 2 will indicate the summary of the color of the flame and components of the first and last distillate. Table 2. Flammability Test
Distillate First distillate (Test tube #1) Last distillate (Test tube #22) Color of the flame Blue flame Components Alcohol content is present Alcohol content is absent

The table shows the result obtained from flammability test wherein the first distillate produced a blue flame (presence of alcohol) while the last distillate did not (absence of alcohol). This means that the process of distillation was successful and that the components of vodka were separated to ethanol and water.

RESULTS AND DISCUSSION

The group was not able to reach the required temperature limit of 100C. The collection of distillates stopped at 98C because the temperature stopped increasing. Table 1 will indicate the summary of the number of the test tube used, volume of each distillate and its temperature. Table 1. Temperature of Distillates
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 of distillate per test tube 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL 0.5mL Temperature (c) 26C 79C 79C 79C 80C 80C 81C 81C 82C 82C 83C 85C 85C 88C 89C 92C 92C 92C 92C 92C 92C 95C 98C

Figure 2 will indicate the summary of temperature versus volume recorded throughout the experiment in a plotted graph. 120
Temperature (C)

100 80 60 40 20 0 1 2 3 4 5 6 7 Volume (mL) 8 9 10 11

Figure 2. Temperature versus Volume The graph shows the relationship of temperature to the volume of vapor collected from the sample. The highlighted part indicates where the concentration of alcohol is strongest. Calculations:

The table shows that 22 test tubes are used for the collection of distillates and each test tube contained 0.5mL distillate. The initial temperature was 26C. The collection of distillates started at 79C and stopped at 98C.

The given formula was used to determine the percentage of ethanol and percentage loss in the experiment. The percentage of ethanol was 10% and the percentage loss was 3.33%.

REFERENCES
WEBSITES: [1] Chem.umass.edu (n.d.) Retrieve July 19, 2012 from www.chem.umass.edu/~samal/269/distill.pdf [2] Chemistry.about.com (n.d.) Retrieve July 21, 2012 from http://chemistry.about.com/cs/5/f/bldistillation.h tm [3] Differencebetween.net (n.d.) Retrieve July 19, 2012 from www.differencebetween.net/science/differencebetween-fractional-and-simple-distillation/ [4] Ehow.com (n.d.) Retrieve July 21, 2012 from www.ehow.com/about_5401943_definitionsimple-distillation.html [5] Hugotapia.tripod.com (n.d.) Retrieve July 19, 2012 from www.hugotapia.tripod.com/simpledistillationvsfra ctionaldistillation/ [6] Scribd.com (n.d.) Retrieve July 19, 2012 from www.scribd.com/doc/17717405 [7] Scribd.com (n.d.) Retrieve July 21, 2912 from www.scribd.com/doc/38610134