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Activity No. 12
Boiling Point and Melting Point Determination

I. Objectives

1. To be familiar with the principles of melting point and boiling point determinations.
2. To master the method of determination of melting point and boiling point using capillary
tube.
3. To determine the melting point and boiling point of organic solids and liquids.

II. Introduction

The determination of physical properties of organic compounds such as boiling points,

melting points, density, solubility, refractive index, etc. is important for characterizing and
identifying organic compounds. In this experiment you will be learning the techniques for
measuring the melting point of a solid and the boiling point of a liquid.

Boiling point is formally defined as the temperature at which the vapor pressure of the liquid
becomes equal to the pressure at the surface of the liquid. The boiling point of a liquid can
change if the pressure at the liquid's surface changes. Since pure substances have a distinct
boiling point, boiling points are sometimes used to determine the purity of substances.

A solid is said to melt sharply if the melting point range is 0.5 - 1.0 oC (narrow melting point
range). A pure solid will generally melt sharply because the forces of attraction between its
particles are the same. However, the presence of a foreign particle in a crystal lattice interrupts
its uniform structure and the forces of attraction are weakened. An impure solid melts at a
lower temperature and over a wider range. Thus, a solid's melting point is useful not only as an
aid in identification but also as an indication of purity.

III. Materials/ Reagents

(6) Capillary Tubes Cooking Oil

(1) Thermometer 0.5 g Urea
(1) Bunsen Burner 0.5 g Benzoic Acid
(1) Watch Glass 0.5 g Benzoic Acid-Urea Mixture
(1) Stirring Rod 0.5 mL Isopropyl Alcohol
(5) rubber band 0.5 mL Acetone
(1) Iron Ring, Iron Stand, Wire Gauze 0.5 mL Acetic Acid
 (1) Universal Clamp (2)- 5-mL test tube
(1) 50-mL Beaker

IV. Procedure

A. Melting Point Determination

1. Sealing Capillary Tubes

Put one end of a prepared capillary tube to the edge of a small hot flame and rotate the
capillary tube slowly so that the end is sealed. To ensure the capillary tube sealed compactly
and smoothly, you should operate it carefully and not make it bended or into a small ball.

2. Filling capillary tubes.

Place a small sample of the solid pulverized finely on a clean watch glass, then collect the solid
into a small mound and push the open end of the capillary tube down into the sample. The
solid may be forced down by dropping the tube (sealed end downward) through a long length
of ordinary glass tubing onto the desktop. Further increments of the sample are introduced in
the same way until the material forms a compact column 3-5 mm high at the bottom of the
tube after repeated dropping. It is essential that the material be packed firmly and densely into
the end of the tube.

Follow the method above; fill three tubes with benzoic acid, urea, and mixtures of unknown
sample.

3. Arranging assembly.

Introduce oil bath liquid into a 50-mL beaker and keep the bath level at the position of the two-
third of the beaker. The capillary tube containing the sample is attached to a thermometer by
means of a small rubber band. The rubber band must be kept well above the level of the hot
oil, or the oil could melt the rubber and break the band. For accurate reading, the sample
compound in the capillary tube is kept close to and at the level of the thermometer bulb, which
is fully submerged and centered in the oil bath, as shown in Figures 1-2.

4. Taking melting point

When the apparatus has been arranged, properly heat the bottom portion of the side arm with
burner. Convection currents carry the heated oil up through the side arm and down the main
shaft of the apparatus for uniform heating. Apply heat at a moderately rapid rate until the bath
liquid is within 15-20 oC of the melting point. Continue the heating with a very small flame
adjusted so that the temperature rises slowly and at a uniform rate (about 1 oC per minute). If
necessary, hold the burner by its base and move it back and forth under the bath. Observe
carefully the samples in the melting point tube and the thermometer reading. Record as the
observed melting point the range between the thermometer reading when sample starts to
liquefy and that when the melt is clear. After the samples have melted, extinguish the flame
and allow the bath to cool.

Figure 1. Test Tube Assembly for Melting Point Determination.

B. Boiling Point Determination

1. Make a test tube assembly by using the following directions and illustration.
Figure 2. Test Tube Assembly for Boiling Point Determination.

1. Place about 1 mL of Isopropyl alcohol in a 10-12 mm diameter test tube.

2. 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.
3. Insert an inverted closed end capillary tube into the test tube.
4. Make an oil bath assembly similar to Figure 1.
5. Place the above test tube assembly in the oil bath so that the surface level of the alcohol in
the test tube is beneath the surface level of the oil bath.
6. Heat the oil bath carefully and observe the stream of bubbles emerging from the capillary
tube.
7. Remove the heat source and when the last bubble emerges from the capillary tube, record
the temperature.
.
Clean-up:

Dispose of the used capillary tubes by putting them in your trash can. If any isopropyl alcohol is
left in your test tube, you may pour it down the drain with water.
 Activity No. 12
Boiling Point and Melting Point Determination

Name:_______________________ Date Submitted:______________

Course:______________________ Professor:__________________

A. Melting Point Determination

Sample Melting Point Range (oC) Melting Point (oC) % Error

(Expt’l) (Theoretical)
Benzoic Acid
Urea
Benzoic Acid-Urea Mixture
B. Boiling Point Determination

Sample Boiling Point (oC) Boiling Point (oC) % Error

(Expt’l) (Theoretical)
Isopropyl Alcohol
Acetone
Acetic Acid

Watch this Video on boiling point determination: https://youtu.be/8b5Ha-8QGhY

Watch this video on melting point determination: https://youtu.be/nQNaTfqXECk

V. Questions.

1. Define boiling point and melting point.

2. Which of the three liquids has the largest boiling point. Explain

3. Which of the two solids ( urea or benzoic acid) has a larger melting point. Explain.

4. Why different liquids have different boiling points.

5. What is the effect of increase in pressure on the boiling point of a substance.

6. Why do pure solids have sharp melting points.

7. What is the effect of impurity on the melting point of a substance.

8. Do you expect the benzoic acid-urea mixture to have a higher melting point than pure
benzoic acid or pure urea. Explain your answer.