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Analytical Chemistry Experiment: Simple Distillation Method

December 21, 2008

Analytical Chemistry Experiment

Simple Distillation Method

Abstract

A quick fit set-up for simple distillation was been assembled carefully. 50ml of Pineapple wine was placed in a pear shaped flask and added with boiling chips. Making sure that water was flowing in a condenser, the wine sample was heated with a burner using one inch blue flame. Four distillate with recorded temperatures were collected. These distillates were kept for boiling point experiments…

Introduction

The boiling point of a pure organic liquid is a physical property of that liquid. It is defined as the temperature at which the vapor pressure of the liquid exactly equals the pressure exerted on it. Boiling points can be determined using the technique of simple distillation. Distillation is a technique that is used to purify a mixture of liquids or to obtain a boiling point of a pure liquid (in the case of this course). Essentially, the liquid is heated to boiling and the vapors condensed above the boiling liquid.

Distillation is a very old technique which is frequently used to purify compounds and to determine their boiling points. The boiling point is a useful molecular constant for the characterization and identification of pure compounds. Furthermore, the boiling point range is usually a good indicator of the purity of a liquid.

Distillation is a physical process used to separate mixtures that contain at least one liquid. Distillation works because each substance in the mixture has its own unique boiling point. So, as a mixture is heated, the temperature of the mixture rises until it reaches the temperature of the lowest boiling substance in the mixture. The lowest boiling substance boils away. Meanwhile, the other components of the mixture remain in their original phase (either solid or liquid) until the lowest boiling component has all boiled off. Only then does the temperature of the remaining mixture rise and other components are boiled off.

I. Review of Related Literature

Distillation often follows fermentation. Fermentation is used to produce alcoholic beverages. Grain is fermented to make beer, while grape juice is fermented to make wine. Beer and wine never contain more than around 12% alcohol, because any higher concentration kills the yeast that produce the alcohol. To make stronger drink, distillation is used. Wine, beer, or fermented brews made from corn, sugar cane, or potatoes can be purified by distillation. Since ethyl alcohol boils at only 83°C while water boils at 100°C, the alcohol will boil off, leaving the water behind. The alcohol vapors are then condensed and collected. Distillation can produce liquors that range from 40-95% ethyl alcohol.

The object of distillation is the separation of the alcohol from the other ingredients in the beer, mostly water. In making fuel alcohol it is necessary to get all of the alcohol and water separated if the alcohol is going to be mixed with gasoline, and most of the alcohol and water separated if the alcohol is going to be burned in a converted engine. As will be seen, the purer the alcohol, the harder it is to make.

The separation of the alcohol and water by distillation is made possible by the fact that alcohol boils at about 173 degrees F. and water at 212 degrees F. When the mixture of water and alcohol is boiled, vapors with a greater concentration of alcohol will be formed and liquid with a lesser concentration of alcohol will remain behind. However, because water and alcohol do not form what is called an “ideal” mixture, the separation cannot be done in one clean step.

61Figure Simple Distillation

It illustrates a simple distillation apparatus using laboratory-type equipment. Note that the equipment consists basically of a container for the liquid to be distilled (still pot), a heat source, and a condenser to turn the distilled vapors back into liquid form. The thermometer is necessary to monitor the temperature of the vapors.

II. Methodology

1.)    Carefully assemble the quick-fit set-up.

2.)    Place 50ml of the liquid sample in the pear shaped flask. Add a few pieces of boiling chips.

3.)    Make sure the water is flowing through the condenser. Heat the sample with a burner, using a one-inch blue flame.

4.)    Collect the distillate in labeled test tubes, recording the temperature. Change the test tube after collecting 5 to 10 drops. Keep the distillate for the boiling point determination.

5.)    When done, cut off the heat source first, before closing the water valve.

6.)    Allow time for the set-up to cool before dismantling the glassware.

III. Discussions of Data and Interference from Results

The data below are from the collected fractions of distillates from the liquid sample. Every fraction contains 1mL of the distillate. We used a test tube containing 1mL of distilled water to compare it with our fraction to know if it contains the right amount of volume we wanted.

Volume of fraction collected

Temperature

Flame test result

Fraction 1

1mL

°C

Not Tested

Fraction 2

1mL

°C

Fraction 3

1mL

°C

Fraction 4

1mL

°C

The first fraction we collected with 1mL of the distillate was at __°C, the second at __°C  third at __°C  and the last is at __°C . We didn’t tested the first fraction if it is flammable or not to know if the distillate was an ethanol or not since our instructor not ask to do it so. But as far as the temperature values are concerned since they are closed to the accepted values boiling ethyl alcohol, I can say that the product is an ethyl alcohol.

IV. Answers to Guide Questions

1.)    Where should the thermometer bulb in the distillation setup be placed and why?

The thermometer should be placed above the liquid sample where the vapor is passing. In this case, we can determine the temperature of the vapor and not the liquid sample.

2.)    How can one know that a component of liquid mixture has been completely vaporized and distilled over?

One can know that a component of liquid mixture has been completely vaporized and distilled over if, the vapor from the liquid sample turned to pure liquid.

3.)    What is the advantage of a fractional distillation over the simple distillation type?

The advantage of fractional distillation over the the simple distillation type is that, in fractional distillation, the separation of a mixture into its component parts, or fractions, such as in separating chemical compounds by their boiling point by heating them to a temperature at which several fractions of the compound will evaporate.

While in simple distillation, all the hot vapors produced are immediately channeled into a condenser which cools and condenses the vapors. Therefore, the distillate will not be pure, its composition will be identical to the composition of the vapors at the given temperature and pressure.

V. Bibliography

  • Zubrick, James W. The Organic Chemistry Lab Survival Manual: A Student’s Guide to Techniques 6th Edition. New York: John Wiley & Sons Canada, Ltd.; 5th edition.
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