Experiment 1: Simple and Fractional Distillation Marc Delvin Quero, Ryan Querubin, Rafaelle Raspado, Aimee Ravelo and

Ma. Lourdes Roble Group 8 2G Medical Technology Organic Chemistry Laboratory

ABSTRACT
The group extracted ethanol from the Vodka sample by fractional distillation. We observed that the sample started to boil at 78C and the first 0.5 mL distillate was collected when the temperature reading was 87C. Collection of distillate was stopped when 100C was reached. A total of 16.5 mL of distillate was collected and the first and the last test tubes containing 0.5 mL of distillate each were tested for flammability. After computing for the percentage ethanol and the percentage loss, the group arrived at 8.33% and 15% respectively.

INTRODUCTION EXPERIMENTAL
Distillation deals with a mixture, a solution composed of two or more elements, that when boiled, will cause each element to vaporized at different temperatures. Distillation involves the conversion of a liquid into its vapours (evaporation) upon heating and then cooling the vapours back into the liquid (condensation). Due to the small difference in the boiling points, both liquids form vapours simultaneously. Vapours of the boiling liquid mixture are made to pass through a glass fractionating column. The fractionating column is a simple packed column, packed with glass beads, or it is a specially designed column called the bubble plate column. The vapours of the low volatile liquid (the liquid having a higher boiling point) get condensed in this column and return to the distillation flask. The condensate consisting of the pure, more-volatile component (the compound having lower boiling point) leaves the column from the exit near the top and enters the condenser and gets collected in the receiver. The experiment was conducted to differentiate simple distillation from fractional distillation; to know the efficiency of both kinds of distillation; to extract the ethanol component of Vodka, a kind of alcoholic beverage from the other components of the beverage and to calculate the ethanol content of the said beverage. A. Compound/s Sample Tested 30 mL Vodka B. Procedure For the Fractional Distillation In this experiment, a fractional distillation set-up was prepared as shown in Figure 1. After preparing the set up, 33 test tubes were calibrated down to 0.5 mL and numbered them accordingly. Then the group placed three (3) pieces of boiling stones inside the quick-fit distilling flask and introduced 30 mL of Vodka. Afterwards, the distilling flask containing the vodka was heated using an alcohol lamp until the solution started to boil. Temperature was recorded when the first drop of distillate was collected. 0.5 mL of distillate were placed in each test tube and the collection of distillate was stopped when the temperature reading was 100C . For Flammability Test The group placed 3-5 drops of distillate from the first test tube in a watch glass and another 3-5 drops of distillate from the last test tube were placed in another watch glass for flammability test.

RESULTS AND DISCUSSION

11.5 96 12.0 96 12.5 97 13.0 97 13.5 98 14.0 98 14.5 98 15.0 99 15.5 99 16.0 99 16.5 100 Table 1. The Volume and Temperature Table 1 shows the progress in temperature of the sample in relation to the increasing volume. From 3.5 mL to 5.5 mL, there was a constant temperature of 89C which is considered the plateau. The plateau is 2.5 mL. Ethanol has a lower boiling point that water. It is more volatile than water so we expect that ethanol will be the first distillate since ethanol will evaporate first. The first distillate was collected with 87C temperature reading. And collection was stopped when 100C was reached totalling the number of distillate to 16.5 mL.

Figure 1. The Fractional Distillation Set-Up

Ethanol (ethyl alcohol) from the Vodka sample was extracted using fractional distillation. The figure above shows the proper and correct fractional distillation set up. The set up is different from that of simple distillation because of the presence of a fractionating column with packing. Volume 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 5.5 6.0 6.5 7.0 7.5 8.0 8.5 9.0 10.0 10.5 11.0 Temperature 87 87 87 88 88 88 89 89 89 89 89 90 91 92 92 93 93 94 94 95 95

Tem perature(C) vs Volum (m ) e L

Figure 2. Temperature vs. Volume Figure 2 shows the relationship between the volume and the temperature during the collection of distillate. Distillate First Distillate Last Distillate Result Flammable Non-flammable

Table 2. Observations during Flammability Test Since ethanol is more volatile than water, the first distillate is ethanol. When subjected to flammability test, the first

distillate is flammable while the last distillate is non-flammable. This is because the last distillate was collected when 100C hence it is water. Distillate First Distillate Last Distillate Component Vodka Water

http://orgchem.colorado.edu/hndbksupport/dist /html University of Santo Tomas Department of Chemistry (2006). Organic Chemistry Laboratory Manual. Manila Tutor Vista http://www.tutorvista.com/content/chemistry/c hemistry-iii/organic-compounds/distillation.php

Table 3. Component/s of the distillate based on flammability test. Percentage of Ethanol % Ethanol = 2.5 mL x 100 30 mL = 8.33 %

Based on Table 1, the plateau is from 3.5 mL to 5.5 mL which is 2.5 mL. Dividing it to the total number of sample and then multiplying the quotient to 100 the resulting percent is 8.33 Percentage Loss % Loss 100 100 = 15 % = = 30 mL (Distillate + Residue) x 30 mL 30 mL (16.5 mL + 9 mL) x 30 mL

After performing the experiment, we measured the residue and it is 9 mL. Percentage loss is the result from dividing the difference of the total number of sample used to the sum of the distillate (which is 16.5 mL based on the given date in Table 1) and the residue by the total number of sample again then the quotient is multiplied to 100 to get the %. REFERENCES
Pavia, D.L., Lampman, G.M. & Kriz, G.S. (2005). Introduction to Organic Chemistry techniques: A small-scale approach (2nd Ed). Pacific Groove, CA. Thomson Brooks/ Cole Seader, J. D., (1998). Separation York: Wiley and Henley, Ernest J. Process Principles. New

University of Colorado Boulder Department of Chemistry and Biochemistry (2003). CU Boulder Organic Chemistry Undergraduate Courses Lab Techniques. Retrieved May 30, 2007 from the University of Colorado website