CHEM 331-Lab

Organic Chemistry

Experiment 4

Melting and Boiling Points

Department of Chemistry - Faculty of Science

Beirut Arab University
Fall 2020-2021
 Aim of the Experiment

Calibrate the thermometer by measuring the

melting point of a solid substances and detect
that of an unknown, and measure the boiling
point of a liquid substances.

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 Introduction

 There are several material constants that can be used to describe a material, for

example, its specific gravity, light refraction, adsorption capacity, or

chromatographic behavior.

 The melting point is also one of these constants. Along with the boiling point

and the solidification point, it is one of the important thermal characteristics

that describe a material.

 Melting point correspond to the melting of a solid, while boiling point

correspond to the boiling of a liquid.

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 Melting point
 Is the temperature at which it changes state from solid to
liquid.
 Is the temperature at which the solid and liquid can exist in
equilibrium at pressure 1 atmosphere.
 Pure compounds usually melt over a very sharp and narrow temperature range

(0.5°C – 1°C). While, impure compounds melt over a wide range (>2°C) and at

lower temperature, lowered and broadened temperature. Which means that

impurities decrease the m.p of a compound. (m.p decreases as impurities increases)

 Thus, impurities must be soluble in order to affect the m.p of a solid, but impurities

like charcoal and broken glass do not affect the m.p since they are insoluble.

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 Melting point-Continued
 We said that, most pure organic compounds melt over a sharp and narrow range, hence the term
“melting range” is more appropriate than “ melting point”.

 The small temperature difference observed between temperature at which compound starts to melt
and that at which the compound is liquid is caused by “heat transfer”. It will take a little time for the
heat to transfer from the heating block through the glass of the tube and into the organic compound.

 Whenever this solid structure is heated, the particles in it begin to move more strongly, until finally
the forces of attraction between them are no longer strong enough to maintain the crystalline
structure. The lattice is destroyed and the solid material melts.

 At the melting point of a material shifts from its ordered solid state to an unordered liquid state. The
stronger the forces of attraction between the particles within the lattice, the greater the amount of
energy that must be used to overcome them. The melting temperature of a crystalline solid is thus an
indicator for the stability of its lattice. The higher the temperature, the more strongly the lattice
structure in question holds together.

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 Importance of melting point

 There are various methods of chemical and physical analysis

used to differentiate, identify, and classify materials.

 Measurement of the melting point is, one of these standard

laboratory procedures. It is an experimental and easily

performed method of physical analysis used to find out the

identity, the purity, and the thermal stability of a material.

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 How to detect an unknown compound?
 The technique is called “mixed melting point”, it helps to identify
the identity of an unknown compound.
 Suppose that, we have an unknown melts at 122°C (which is
benzoic acid).
 First, we determine the m.p of this unknown, for example, it
was found 118-119°C, this is quite close to the expected value,
the compound could be benzoic acid but, there is hundreds of
organic compounds that melt in this range.

What could we do?

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 How to detect an unknown compound?

Mix an equal amount of the unknown with benzoic acid

If the m.p = 122°C, If it melts below 122°C, so, it

so it is benzoic acid. will act as impurities, and the

compound is not benzoic acid.

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 Boiling Point

 Is the temperature at which the vapor pressure of the liquid is

equal to 1 atm.
 Is the temperature at which states transfer from liquid to gas,
liquid is in equilibrium with gas.
 We should distinguish between Evaporation and Boiling.

The liquid changes to vapor Molecules are anywhere

below the b.p, the molecules the liquid escape, resulting
are located near the liquid in the formation of vapor
surface. bubbles within the liquid.

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 Boiling Point-Continued
 All elements and many inorganic and organic compounds have characteristic
boiling points. Mixed liquids do not have a precisely defined boiling point.
Instead, they boil over a fairly wide range of temperatures within clearly
defined boiling limits.
 Accordingly, observation of their boiling behavior is an easily measurable
experimental criterion for determining their purity. Whenever the boiling
temperature changes during the boiling process, the material you are
investigating cannot be a single pure material.
 However, it must be noted that impurities basically have less effect on the
boiling point than on the melting point. For that reason, the boiling point is
less as informative criterion for the purity or for the description of materials as
the melting point.
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 Safety Precautions

As in all laboratory exercises:

• Safety glasses, mask, and gloves must be worn at all
times.
• Avoid skin and eye contact with any chemical reagent.
• In case of skin contact, rinse the area with water for
several minutes.
• For eye contact, flush eyes with water and seek
immediate medical advice.

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 Procedure (Melting Point)
First, calibration of thermometer should be done due to the variation in the size of their internal base.
Laboratory thermometers differ in accuracy and need to be calibrated. So, standard known compound used
to calibrate the thermometer.

A.
Thermometer (attached by a
clamp on the stand)
B.
1. Attach the capillary by Capillary tube filled with compound,
the thermometer using a tapped well and rubbered with the
rubber. thermometer.
2. Fill 100 mL beaker with
30 mL paraffin oil. 30 mL paraffin oil

Known will be used:

1. Benzoic acid 122-121
°C
2. Salicylic acid 158.6 °C

1. Close one end of the capillary by

heating on the flame. C.
2. Fill the capillary with the solid.
3. Tap well the capillary in order Heat and record temperature
to get the solid at the closed end.

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 Procedure (Mixed melting point)
D. Similarly as for known solid compounds

Substance will be used:

1. Unknown

1. Record the temperature of your

1. Attach the capillary
by the thermometer unknown
using a rubber. 2. Mix the unknown with each known
2. Fill 100 mL beaker
with 30 mL paraffin compound done before.
oil. 3. Same steps should be applied
4. Record the correct m.p and identify
your unknown
5. Draw a calibration curve to record the
corrected m.p

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 Procedure (Boiling Point)
 Micro boiling method

Heat until a
Attach the micro boiling 1. the temperature is noted
continuous bubbles Stop
tube with the inverted when bubbles cease to
comes out of the heating,
closed capillary inside come out of the capillary
small capillary and cooling.
with the thermometer on and just enters it.
pass through the
a stand, similarly as 2. Record the temperature
liquid.
melting procedure.

Known will be used:

1. Chlorobenzene 132°C
2. Nitrobenzene 210°C

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 Calculation
Thermometer
    calibration

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