SIMPLE AND FRACTIONAL DISTILLATION Maria Janine B. Abarientos, Kuia B. Allarde, Aliana Keshia P. Andino Mary Viadelle E.

Andrada and Nina Marian Robelea G. Ang Group 1 2C Pharmacy Organic Chemistry Laboratory ABSTRACT
This test was carried out in order to differentiate simple distillation from fractional distillation, to separate the components of an alcoholic beverage, and to calculate the percentage of ethanol in a certain beverage. The group was assigned to perform simple distillation. The first and last test tubes were kept in order to test for flammability which may happen due to the ethanol that may be present in the distillate, wherein the computations performed for this experiment: percent alcohol and percent loss are based.

Distillation is a method of separating mixtures based on differences in their boiling points. It is a unit operation, or a physical separation process, and not a chemical reaction. This is also one of the methods used to purify liquids. There are four methods of distillation: simple distillation, fractional distillation, vacuum distillation, and steam distillation. Focusing on the two distillation processes in the experiment used by random groups of the class, Simple distillation and Fractional Distillation. Simple Distillation refers to the "simple" separation of compounds by evaporating the liquid and collecting it after it passes through a condenser to be changed into a liquid state. It is usually used only to separate liquids whose boiling points differ greatly or to separate liquids from non-volatile solids or oils. In this case, the distillate may be sufficiently pure for its intended purpose. Fractional distillation separates the different components in a chemical mixture according to their different boiling points. The liquid is raised to boiling and vapors pass through a tubular column where temperature is gradually lowered along its length. Components (fractions) with a higher boiling point condense on the column and return to the solution. Fractions with a lower boiling point pass through the column and are collected.

Figure 1. Simple Distillation Set-up Two members were assigned in doing the first step of the experiment, which was to prepare several test tubes calibrated down to the 0.5mL mark and number them accordingly. Three pieces of boiling stones were then put in the quick-fit distilling flask and then introduced 30mL of vodka. The flask was heated using the alcohol lamp with rotating motion, after the vodka started to boil the first drop of the distillate was the first mark to record the temperature. The assigned member to read and record the temperature with its corresponding distillate should keep it noted. The distillate was collected using the calibrated test tubes. The collection of distillate stopped after reaching its second plateau of constant temperature, 98 oC.

Sample: Vodka Brand Name: The Bar Apple Vodka %v/v alcohol(ethanol)= 25.3% Manufacturer: Emperador Distilleries

B. Procedure 1. Simple Distillation
Simple distillation was the kind of distillation assigned to the group. The experiment is composed of a distillation apparatus, vodka, alcohol lamp and boiling stones.

2. Flammability Test The last member was tasked to conduct a flammability test. 3-5 drops was both

collected from the first and last test tube into two separate watch glasses. In both watch glasses the member applied a lighted match. RESULTS AND DISCUSSION
Simple distillation will only have one distillation (vaporization-condensation) cycle in the whole process, while the fractional cycle will have at least two cycles. The only difference in the structure of the set-up is that the fractional distillation will use an additional equipment called the ‘fractionating column’, while the simple distillation will not need that equipment.   Before gathering data, the temperature should begin at 35 oC (room temperature).

After doing the experiment from 30mL of Vodka sample, 17mL was the remaining volume. The total volume of the vodka sample recovered was 28.5mL. Here is a graph that will summarize the temperature vs. volume of the distillates collected in the experiment:

Temperture vs. Volume
100 98 96 Temperature 94 92 90 88 86 84 82 80 1 3 5 7 9 11 13 15 17 19 21 23 Fractions (0.5mL portion)

Table 1. Data Recorded For Simple Distillation
Fraction Collected (0.5 mL portion) F1 F2 F3 F4 F5 F6 F7 F8 F9 F10 F11 F12 F13 F14 F15 F16 F17 F18 F19 F20 F21 F22 F23 Temperature (oC) 81 oC 83 oC 83 oC 84 oC 88 oC 90 oC 91 oC 96 oC 96 oC 97 oC 97 oC 97 oC 97 oC 97 oC 97 oC 97 oC 97 oC 97 oC 98 oC 98 oC 98 oC 98 oC 98 oC

Graph 1. The line graph of the Temperature vs. Volume of the Distillate The Percentage of ethanol can be computed by the following formula: %ethanol= (total volume of the distillate of the first plateau / volume of the sample) x 100 %ethanol= (4.5mL/ 30mL) x 100 = 15% ethanol The group was able to compute 15%ethanol. The percentage loss of the Vodka sample can be computed by the following formula: %loss= {[volume of sample- (total volume of vodka sample recovered)]/ volume of the sample} x 100 %loss= {[30mL-(28.5mL)]/ 30mL} x 100 = 5%loss The percentage loss shows the amount of liquid spilled during the experiment. The percentage loss may also indicate errors that have been committed in the experiment. Since the percentage loss computed was 5%, it is

As shown in the table 23 distillates were collected with each having a 0.5mL portion. By multiplying the number of fractions to 0.5mL calibration per test tube, the total volume of fractions collected is 11.5mL. The first fraction collected has a temperature of 81oC. At the tenth fraction a temperature of 97oC was recorded until the eighteenth fraction and this is considered as the first plateau. Then at the nineteenth fraction a temperature of 98oC until the twenty-third fraction, the last distillate collected and this is considered as the second plateau or the second constant. The group did not reach the 100oC limit because the temperature stopped increasing when it reached 98oC.

reasonable that some errors occurred. For example wrong temperature reading, spillage when getting distillate for each fraction, lack of heat needed, etc. The percentage loss that the group computed was compared to the computed percentage loss of the group who used fractional distillation. The other group computed 10%loss. So it can be noted that, when using fractional distillation, more errors can occur or more liquid spillage occur during the experiment. The first and last fraction was tested for its flammability. Table 2 shows the observation and the interference of each of the fraction. Table 2. Flammability Test of F1 and F23
Distillate F1 F23 Observation Flammable (appearance of a blue flame) Non-flammable (no appearance of flame) Interference Presence of alcohol Absence of alcohol

The first fraction produced a blue flame when a lighted match was applied. This shows that the first fraction still contains alcohol. When a lighted match was applied to the last fraction, there was no appearance of flame, meaning there is no alcohol in it.

[1] [2] _distillation [3] Bayquen A. Manual in Organic Chemistry.Quezon City: C&E Publishing Inc. [4] [5] [6] erence-between-fractional-and-simpledistillation/ 2009


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