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Bienn Paulo A. Laforteza, Michael James O. Lazatin, Gell Marvi C. Lee Mary Therese S.D. Leoncio and Denise T. Magdamit Group 6 2G Medical Technology Organic Chemistry Laboratory

Distillation is the extraction of volatile component of a mixture through a two way process, evaporation and condensation. The experiment aimed to differentiate simple from fractional distillation, to separate its components, alcohol and water, and to determine its percent concentration of ethanol by using the fractional distillation method. Vodka was the alcoholic beverage that was purified. A certain volume (30 mL) of vodka was placed on the pearshaped flask with boiling chips on a fractional distillation set-up and was heated constantly with an alcohol lamp. A 0.50 mL of distillate was collected in every test tube until the temperature reached close to 100 oC. The first and last distillates were kept and its flammability was tested. The first distillate was flammable meaning it has the component, ethanol, while the last distillate inflammable thus, having the water component after being purified. The volume of distillate collected by the end of the distillation was 15.5 mL at 99 oC, giving a percent ethanol of 15%

Distillation is a process of converting a liquid to a vapour, condensing the vapour and then collecting the distillate in another container.1 Distillation is a widely used method for separating mixtures based on differences in the conditions required to change the phase of components of the mixture.2 Distillation is an important commercial process that is used in the purification of a large variety of materials.3 Distillation can be used in purifying water or other substances and removing or separating the components of mixture such as an alcoholic beverage like vodka. Vodka is a clear liquor manufactured from ethyl alcohol. It lacks color, and normally has very little taste or aroma. It is said to have been originally created from potatoes in Russia for medicinal purposes. Nowadays, Vodka is distilled from barley, wheat or rye. Most flavored vodka contains 30-35% alcohol, whereas clear vodka is normally 40%, with a few brands offering a 50% product on top. 4 There are four distillation methods namely simple distillation, fractional distillation, vacuum distillation and steam distillation.1 The objectives of the experiment are (1) Differentiate simple and fractional distillation, (2) Separate the components of an alcoholic beverage (vodka) and (3) Calculate the percentage of ethanol in the beverage.

tubes. The instruments were tightly secured and sturdy. The quick-fit distilling flask contains few pieces of boiling stones and 30mL of the sample beverage which is the vodka. After which, the flask was heated with an alcohol lamp constantly being rotated under the flask. In every test tube, a certain volume (0.5mL) of distillate was collected and recorded until it reached 98-100o C. The first distillate and the last distillate were kept to test its flammability. The set-up was cooled and the volume of the residue was recorded. The first and the last distillate were tested for flammability test in a watch glass. The temperature readings versus the volume of the distillate collected were plotted in a graph. The percentage of ethanol and the percentage loss were also computed.


Table 1 (see next pages) shows that as the volume of distillate increases, the temperature also increases until it comes to a point wherein the temperature closes to 99oC. When the temperature become constant and shows a constant slope in the graph, it confirms the presence of ethanol in the sample wherein it is most concentrated. Table 2 (see next pages) shows the graphed type of the table of values of the temperature and volume of the distillate. The constant values which signifies a steady slope is the volume of the ethanol (5.0mL to 0.50mL). All in all, the volume of the distillate is 15.5 mL and the volume of the residue is 11.4 mL. In the flammability test, the first distillate produced a blue flame with an orange tip which makes it flammable. The last distillate didnt produce any flame at all which makes it not flammable. Thus, the component of the first distillate is ethyl alcohol and the component of the last distillate is water. It shows that as the distillation of the sample continues, there is a decreasing amount of alcohol being gathered in the separate test tubes. The first test tube contains more

EXPERIMENTAL A.Compound tested or samples used

The sample used was clear unflavored vodka. (Cossack Vodka)

B. Procedure
The set-up used was a fractional distillation set-up (See Figure 1). The apparatus used were the following: iron stand, iron rings, iron clamps, alcohol lamp, pear shaped flask (with 30 mL vodka), still head, thermometer, fractionating column (with boiling stones) , condenser, rubber tubing, adapter and test

alcohol compared to the last test tubes used which contain the last few drops of distillate. After performing the flammability test, the percent alcohol, percent loss and percentage error were computed:

% EtOH=5.0mL -0.50 mL 30mL =15 % EtOH


Simple distillation is used in separating components of liquid mixtures, which have significantly different boiling point while fractional distillation is used in separating mixtures with boiling points close to each other. Fractional distillation separates liquid much better than simple distillation because of the boiling chips in the fractionating column. Simple distillation gives poorer separation than fractional distillation for it provides theoretical plates on which the refluxing liquid can condense, re-evaporate and condense again, essentially distilling the compound over and over again. Simple distillation has one distillation cycle while the fractional distillation has two.

From book: [1] Bayquen, A.V., Cruz, C.T., De Guia, R.M., Lampa, F.F., Pena, G.T., Sarile, A.S. & Torres, P.C. (2009). Laboratory Manual in Organic Chemistry. Manila: C&E Publishing, Inc. p.13-14

% loss= 30mL (11.4mL + 15.5 mL) 30mL = 10.33% loss


% error= | 15 40 | 40 =62.5%


From Internet: [2] Helmenstine, A.M. What is Distillation? http://chemistry.about.com/cs/5/f/bldistillation.htm 7/22/12 [3] [No author mentioned] Distillation. http://www.umsl.edu/~orglab/documents/distillation/d ist.htm 7/22/12 [4] Drinks Mixer. Vodka. http://www.drinksmixer.com/desc28.html 7/22/12 [5] [No author mentioned] Distillation. http://www.pharmpedia. com/Distillation. 7/22/12 [6] [No author mentioned] Simple and Fractional Distillation. http://www.scribd.com/doc/17717405/Simple-andFractional-Distillation-2EMT-Group-1-2009 7/22/12

Therefore, the percent ethanol content is 15%. The percent loss is 10.33%. This explains that there was some part of the sample that was lost which was caused by evaporation due to the constant heating of the flask. The percent loss also shows that there was an excessive heating of the flask that caused the rapid evaporation of the sample or it can be caused by them was handling of the test tube that caused to the careless collection of distillate.5 Listed below are the following possible sources of error: (1) Parallax reading of temperature, (2) 0.5ml calibration is not accurate and precise during the experiment (3) Few drops of distillate were missed while replacing new test tube for the distillate were not accounted (4) Accurate measurement of residue was skipped, resulting to 0% error (5) Distillate might have vaporize during the experiment before it was tested to flammability test (6) Not all test tubes were tested for flammability test. 6

Table 2. Graph of the Temperature versus Volume

Figure 1. Fractional Distillation Set-up Table 1. Temperature and Volume of the Distillate
Test tube no. 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 Volume (mL) 0.00 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 10.50 11.00 11.50 12.00 12.50 13.00 13.50 14.00 14.50 15.00 15.5 Temp.oC 34 76 76 76 76 76 76 76 76 76 76 80 81 83 84 85 86 87 90 92 93 95 96 96 96 97 97 97 97 98 98 99

150 100 50 0

Table 3. Graph of the Temperature versus Volume

0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15