Distillation Boiling Point Determination

Bicol University
College of Science
DEPARTMENT OF CHEMISTRY
Chem 12C -Organic Chemistry (BS Biology 1)

LABORATORY ACTIVITIES
2nd semester 2014-2015
Distillation and Boiling Point Determination

Activity No. _____
INTRODUCTION
Simple distillation is a process designed to evaporate a volatile liquid from a solution of
non-volatile substances. With the application of heat, the vapor is condensed and collected in a
receiving flask. The boiling point of the volatile substance must be known to be able to monitor
the temperature of the vapor rising to the top of the distilling flask.
The boiling point of a liquid refers to the temperature when its vapor pressure is equal
to the external pressure. The normal boiling point is the temperature at which the vapor
pressure of the liquid is equal to the standard atmospheric pressure, 1 atm. Since pure
substances have a distinct boiling point, boiling points are sometimes used to determine the
purity of substances.
In this activity, a sample of wine will be distilled to be able to collect ethanol. The
boiling point of the distillate will be determined and compared with that of pure ethanol. The
distillate will also be tested for the presence of ethanol using simple chemical tests.
OBJECTIVES
At the end of the experiment, the students should be able to:
1.
2.
3.
4.
Perform simple distillation.

Determine the boiling point of the distillate.
Use the boiling point of a sample as an indication of its purity.
Perform tests for the presence of alcohol in the distillate.
MATERIALS
Reagents
acidified K2Cr2O7
ethanol
wine
Apparatus
1 distilling flask
condenser
adapter
3 rubber stopper
2 burner
2 thermometer
3 Iron stand
2 Iron ring
2 wire gauze
2 rubber tubing
1 250 mL Erlenmeyer flask
1 100 mL Graduated cylinder
1 trough
1 water pump
2 small test tubes

2 dropper
1 funnel
1 capillary tubing
1 rubber band
1 100 mL beaker
3 iron clamp
35
Bicol University
College of Science

PROCEDURE
A. Simple Distillation
1. Assemble the set-up as shown in the diagram on the next page. Half-fill (~170mL) the
distilling flask with the wine sample and put boiling chips. Connect the rubber tubing to
the water inlet and water outlet of the condenser and let water flow inside the water
jacket of the condenser. Make sure that the water output rubber tubing has the
necessary receiver of the water coming from the condenser. Heat the distilling flask
and maintain the temperature at 78.3C. Collect about 10 mL of distillate or until vapor
ceases to condense.
2. Record the volume of the distillate and calculate for % yield.
B. Test for Alcohol

1. Place 10 drops of the distillate in a test tube. Add 10 drops of acidified K 2Cr2O7 or until
a color change is observed. What color change did you observe?
2. Place 1mL of the distillate to an evaporating dish and ignite. Record your observation.
C. Boiling Point Determination
1. Heat one end of a capillary tube until it closes.
2. Make a test tube assembly by using the following directions and illustration below.
a. Place about 1 mL of ethanol in a 10-12mm diameter test tube.
b. Using a small rubber band, attach a thermometer to the outside of the test tube. The
thermometer bulb should be even with the test tube's bottom.
c. Insert the capillary tube into the test tube in an inverted position.
36
Bicol University
College of Science

3. Make a water bath assembly by using the following directions and illustration.
a. Half fill a 100 mL beaker with tap water. Place the above test tube assembly in the
water bath so that the level of the alcohol in the test tube is beneath the surface of
the water bath.
b. Heat the water bath with continuous stirring to ensure even heating. There will be
an initial stream of bubbles as dissolved air is expelled. Then, a little later, a rapid
stream of bubbles emerges from the capillary tube. At this point, stop heating and
begin observing the stream of bubbles.
c. Soon the stream of bubbles will slow down and stop. When they stop, the liquid will
enter the capillary tube. This point corresponds to the boiling point of the liquid.
Record this value under trial 1.
3. Cool the water bath for a few minutes and repeat the heating process using another
capillary tube. . Record the temperature reading as trial 2 and average the values of the
two trials.
4. How does your observed boiling point compare with the accepted boiling point of
ethanol? Calculate your percentage error.
37
Bicol University
College of Science
Activity No. _____

Distillation and Boiling Point Determination
Name ____________________________________________________
Co-workers _____________________________________________
_____________________________________________
Date Started ________________________

Date Finished _______________________
Group/Section ______________________
DATA AND RESULTS
DATA TABLES
Volume of wine used (mL)
Volume of distillate (mL)
% Yield
Color of distillate with acidified K2Cr2O7
Flammability test
Boiling pt. of distillate (C) Trial 1:
Trial 2:
Average:
Boiling pt. of ethanol (C)
78.3
% error
Calculations:
38
Bicol University
College of Science

POSTLAB QUESTIONS
1. How were you able to collect ethanol in this activity? Explain the process.
2. How did the boiling point of the distillate compare with the boiling point of ethanol?
3. What is the importance of boiling point determination of organic substances?
4. What tests were performed to confirm the presence of alcohol in the distillate? Write
the chemical equations.
39

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Bicol University

Chem 12C -Organic Chemistry (BS Biology 1)

Distillation and Boiling Point Determination

Perform simple distillation.

2 small test tubes

Chem 12C -Organic Chemistry (BS Biology 1)

B. Test for Alcohol

Chem 12C -Organic Chemistry (BS Biology 1)

Activity No. _____

Chem 12C -Organic Chemistry (BS Biology 1)

Distillation and Boiling Point Determination

Date Started ________________________

DATA AND RESULTS

Chem 12C -Organic Chemistry (BS Biology 1)

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