Distillation

Abstract
Distillation is the process of separating and purifying compounds or mixtures through the differences of the boiling points of the mixtures to be separated. The objective of this experiment is to separate two distinct components of a mixture using their differences in boiling point. Two mixtures were distilled during the performance of the experiment. A distillation apparatus was set up with a water condenser as cooling device for the vapors. The first mixture, which was a colored aqueous solution of potassium permanganate (KMnO4), was heated to a boil. The vapors went straight to the condenser, where they went back to their liquid form. A colorless distillate was collected. The same process was repeated for the second mixture, a solution of ethanol (C2H5OH) and water. The first 3mL of distillate was collected and then exposed to a flame. The distillate readily burned. The last 3mL was also collected and exposed to a flame. No more flame was observed. At the end of the experiment, it turned out that an effective separation was attained in the first mixture, while the same was not immediately obtained by the second mixture. The observations show how the differences in boiling point and volatility of the solution can affect efficiency in distillation.

Introduction Distillation is the process of heating a liquid until it boils, and then condensing and collecting the resultant hot vapors.1 This process is useful in organic chemistry for separating and purifying compounds, and for indirectly determining the boiling point of a substance. To understand distillation further, the concept of vapor pressure must first be taken into account. At a certain temperature, some molecules of a liquid gain enough kinetic energy to escape to the vapor phase (evaporation), and these molecules can also go back to the liquid state (condensation).2 At any given temperature a liquid is in equilibrium with its vapor. This equilibrium is described by the vapor pressure of the liquid. The vapor pressure is the pressure that the molecules at the surface of the liquid exert against the external pressure, which is usually the atmospheric pressure. When the vapor pressure equals the applied pressure (in cases when boiling is open to the atmosphere, this pressure is equal to 1 atm), the liquid boils.3 However, with increasing altitude with respect to sea level comes a decrease in atmospheric pressure. For example, the boiling point of water at a high altitude is lower than 100C.

The concept of Raoults law can also be linked to the distillation process. Raoults law states that, The vapor pressure of a solvent in a solution equals the vapor pressure of the pure solvent multiplied by the mole fraction.4 Likewise, the total vapor pressure of a solution is equal to the sum of the vapor pressures of its components. This relationship, derived from Raoults law, is capable of describing the boiling point behavior of a compound in a mixture of compounds under a variety of different circumstances. The boiling point of the solution is reached when the total vapor pressure PT is equal to the pressure applied to the surface of the solution.3 Experimental Details A distillation apparatus was set up. A distilling flask was clamped above a Bunsen burner. A water condenser was attached to the tube at the side of the flask, where the water inlet is below the water outlet. Water, through a rubber tube, was continuously running through the condenser, with some of the water flowing out from another rubber tube. An adapter curve was placed at the other end of the condenser, leading to the collecting flask. The distilling flask was half-filled with the colored solution to be distilled. A thermometer, with a cork, was placed at the mouth of the distilling flask such that the bulb of the thermometer is lightly below to the tube leading to the condenser. Once everything was set, the Bunsen burner was lit up to start the distillation process. When the first drop of distillate fell into the receiving flask, the temperature was recorded. Thermometer readings were recorded every two minutes until 20mL of distillate was collected. The whole process was repeated using alcoholic solution. The first thermometer reading was recorded when the first drop of distillate fell to the receiving flask. The first 3mL of distillate was collected in a separate tube, placed in a watch glass and exposed to a flame. The distillate caught fire, but the fire eventually went off after 90 seconds. After every 5mL of collected distillate, the temperature was recorded, until 40mL of distillate was obtained. Another 3mL of distillate was collected after the previously collected 40mL. This sample was put close to a flame, but it did not burn. Results and Discussion Distillation of Colored Solution. The observations and temperature readings are recorded in Table 1.

Time (mm:ss) Temperature Color of Distillate First drop of distillate 104.0C Colorless 02:00 104.0C Colorless 04:00 104.0C Colorless 06:00 104.0C Colorless 08:00 104.0C Colorless Table 1. Temperature readings during the distillation of colored solution In this distillation process, an effective separation was attained, as shown by the colorless distillate. Water has a boiling point of 100C, while potassium permanganate does not exist as a gas, so water was the substance vaporized and collected as the distillate. As observed, the temperature did not change over time. This is an indication of a pure substance being distilled.5 Distillation of Alcoholic Solution. The observations and temperature readings for this part of the experiment are recorded in Table 2. Amount of Collected Temperature Distillate (mL) First drop 90.0C 5mL 92.0C 10mL 95.0C 15mL 96.0C 20mL 98.0C 25mL 98.0C 30mL 98.0C 35mL 98.0C 40mL 98.0C Table 2. Collected data for the distillation of alcoholic solution An effective separation was not immediately attained because the first 3mL of distillate still burned for 90 seconds. This indicates that alcohol (which is flammable and volatile) was still present in the compound. When the test was repeated using the last 3mL of distillate, the sample no longer burned. Generally, in a distillation setup, the component with a lower boiling point vaporizes first. However, azeotropes (such as the alcoholic solution) tend to mimic the boiling behavior of liquids. These cannot be separated by simple distillation. The azeotropic composition sometimes boils lower than the boiling point of its components, and sometimes higher.5 Purified compounds boil at a relatively low temperature range. As the temperature of the vapors in the flask changes, a pure compound is no longer being distilled.6 Table 2 shows that

temperature has drastically changed throughout the apparatus during the process. This means that separation was not effective, and some other kind of distillation must be used to separate the two components. Conclusion Simple distillation is a useful process in the laboratory, especially in separating and purifying compounds. It is effective when separating liquids with a large difference in boiling point, or when separating a volatile substance from a nonvolatile liquid.6 The distillation of the colored solution was effective, considering that the distillate was colorless and that the temperature of the vapors remained constant. However, in the case of the alcoholic solution, which was an azeotropic mixture, effective separation was not immediately attained, as proven in the positive result of the flammability test and drastic temperature chamges. References
1

Distillation. (2013, May 13). Retrieved July 7, 2013, from http://orgchem.colorado.edu/Technique/Procedures/Distillation/Distillation.html 2 (n.d.). Retrieved July 7, 2013, from http://www.chem.umass.edu/~samal/269/distill.pdf 3 (n.d.). Retrieved July 7, 2013, from http://swc2.hccs.edu/pahlavan/2423L7.pdf 4 (n.d.). Retrieved July 7, 2013, from http://www.knockhardy.org.uk/sci_htm_files/raoult.pdf 5 Distillation. (n.d.). Retrieved July 8, 2013, from http://www.umsl.edu/~orglab/documents/distillation/dist.htm 6 Distillation. (n.d.). Retrieved July 8, 2013, from Wired Chemist: http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/distillation

Michael C. Guinita

BS Chem-2

07-08-13