EXPERIMENT 2

MELTING POINT DETERMINATION

GROUP 6

ABSTRACT
The experiment is all about melting point determination of an unknown compound.
Melting point is the temperature at which solid melts to turn into a liquid form. This experiment
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is about to determine the melting points of different organic compounds and to use these to
identify unknowns. It is done by heating a solid until it reached a temperature where it melts. The
objectives for this experiment are: 1 Identify an unknown compound using its experimentally
determined melting point. 2.) Summarize the factors that affect the melting point of an organic
compound. 3.) Analyze the effects of impurities in the melting point range of a substance.

INTRODUCTION

The melting point or sometimes called liquefaction point, is the temperature at which the
substance changes its state from solid to liquid at atmospheric pressure. At the melting point of a
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substance the solid phase and liquid phase are in equilibrium. The melting point of a substance
depends on pressure and is usually specified at standard pressure. The best example of melting
point is the disappearance of ice rather than the formation of ice, that is, the melting point.
Melting points are often used to distinguish and differentiate organic and inorganic
compounds and to measure their purity. The melting point of a pure substance is always higher
and has a smaller range than the melting point of an impure substance or of mixtures. The higher
the quantity of other components, the lower the melting point.
The melting point is sensitive to extremely large changes in pressure, but generally this
sensitivity of magnitude is less than that for the boiling point, because the solid-liquid transition
represents only a small change in volume. A substance is denser in the solid than in the liquid
state, which is why the ice floats on water. The melting point will increase with increases in
pressure, making it directly proportional with each other.
In this second experiment, there is an unknown substance and determined its melting
point. Determining the melting point of a compound is one way to test if the substance is pure. A
pure substance generally has a melting range of one or two degrees. Melting range is the
difference between the temperature where the sample starts to melt and the temperature where
melting is complete. Impurities tend to depress and broaden the melting range so the purified
sample should have a higher and smaller melting range than the original, impure sample. In this
second experiment, there is an unknown substance and determined its melting point.
The objectives of this experiment is to identify an unknown compound using its
experimentally determined melting point and summarize the factors that affect the melting point
of an organic compound. And also to analyze the effects of impurities in the melting point range
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of a substance.

PHYSICAL DATA
LIST OF CHEMICALS
NAME OF

MELTING

COMPOUND
POINT, C
1. Benzoic Acid
121 - 123
2. Naphthalene
79 - 82
3. Salicylic Acid
157 -159
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4. Urea
5. Vanillin
6. Fumaric Acid
7. Maleic Acid

133 - 135
82
287
135

METHODOLOGY
The first part of melting point determination was to prepare a sample solid to melt. An
unknown sample was pulverize and packed inside a closed end capillary tube about a 0.5cm.drop
repeatedly until it compressed. Two capillary need to be filled. Second part was melting it using
a hot plate beside an iron stand. A half-filled 50ml beaker mineral oil will be heated and inside
there are the thermometer tied with capillary tube using rubber band. The rubber band must be
placed above the level of the oil in the beaker. Turning on the hot plate to 300C monitor the
temperature until the first sign of melting and the last sign that was when the crystals are
liquefied. After that repeated again for the second trial.

DATA AND OBSERVATIONS

Table 1.1 Melting point of an unknown solid sample
Physical State and Appearance

colorless and odorless solid

Temperature (Initial Melting)

115C

118C

Temperature (All Crystals

liquefied)

120C

132C

Table 1.2 Identity of the Unknown Compound

Identity of Unknown
Sample Based on Melting
Point (Systematic Name)

Urea

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Molecular Formula
Molar Mass

Lewis Structure
Physical State and
Appearance
Density
Dipole Moment
Boiling Point
Melting Point
Solubility in Water
Vapour Pressure, kPa at
20C
Flash Point
Auto-Ignition Temperature
Occupational Exposure
Limits (TLV)
Inhalation Risk

Literature Values of the Unknown

CH4N2O
60.06 g/mol

white solid
1.32 g/cm
4.56 D
Decomposes
133 to 135 C
107.9 g/100 ml (20 C)
0.08 kPa
non - flammable
non - flammable
15 mg/m3 total dust and 5 mg/m3 respirable dust
Over exposure may produce irritation of the mucous membranes,
nose, throat, coughing and shortness of breath.

DISCUSSION OF RESULTS
The objective of this experiment is to determine the melting point of an unknown solid
sample. It was executed by pulverizing the solid sample and putting it inside a capillary tube. It
is important that the solid sample is pressed into the tube. It is then submerged and heated into a
mineral oil until the melting point is determined. The group must be mindful and observant on
the changes and notice what temperature is the initial melting pointwhen the sample started to
liquefy, and the temperature when all the crystals liquefied. The first trial was very tricky
because the group lack prior knowledge about the experiment. The initial melting point obtained
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was 115C and the temperature in which all of the sample melted was 120C. The group was
hesitant of the results because there was still a little amount of sample that was not melted and
because the hot plate was defectivethe electric cord is loose, interrupting the heating process.
On the second trial, the group decided that it is best to wait until all of the sample was totally
melted. The initial melting point is 118C and by 132C, all the crystals liquefied. Based on the
melting point, the unknown sample is Urea.
To obtain more accurate results, be sure that the hot plate or any other instruments is not
defective. The sample size should be enough to see in the tube. Too much sample will lead to a
wide temperature range. Avoid contamination on the sample because this will give an erroneous
or lower melting point. Lastly, the sample must be firmly packed in the bottom of the capillary
tube to have an efficient heat transfer.

SUMMARY AND CONCLUSION

The objectives of this experiment is to state the factors that affect the melting point of an
organic compound, to identify the unknown compound based on its melting point, and to analyze
the effects of impurities in the melting point range of a substance. The melting point of a solid is
the temperature at which it changes state from solid to liquid at atmospheric pressure. During the
heating, we noted the temperature of the first drop of liquid forms in the sample and the point at
which the sample is completely turns to a clear liquid.
In conclusion, melting point is also used to identify the unknown compound. The factors that
affect the melting point of a sample are the impurities, the force attraction between the molecules
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and when the unknown solid sample is not pulverize well. The temperature at which all the
crystals liquefied was 132C which is closest to Urea.

REFERENCES
http://www.inchem.org/documents/sids/sids/57136.pdf
http://www.peterschemical.com/urea/msds-sheet-urea/
http://pubchem.ncbi.nlm.nih.gov/compound/urea#section=Top
https://en.wikipedia.org/wiki/Urea

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POST LAB QUESTIONS:

1. Rank the following compounds in decreasing melting point: benzoic acid, naphthalene,
salicylic acid, and urea. Justify your rank by citing the intermolecular forces of attraction
present in the particular compound.
1-salicylic acid (159C) - It is ldf and dipole-dipole and polar
2-urea (133C) - Hydrogen bonding and London Dispersion forces
3-Benzoic acid (122.41C) It is ldf and dipole-dipole and polar
4-naphtalene (80.26C) - Hydrogen bonding and London Dispersion forces

2. How does molecular geometry affect the melting point of an organic compound?
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The more symmetrical is the compound, the higher the melting point. If the
molecular shape of the molecules allows them to be packed together, the substance has a
higher melting point.

3. How do impurities affect the melting point of an organic compound?

A substance (solid) containing soluble impurities usually melts at a lower
temperature than the pure compound, and melts over a wide range of temperatures.

4. In general, what are the factors that affect the melting point of an organic compound?
What are the effects?
First factor is force of attraction between molecules because stronger
intermolecular interactions result in higher melting points. The presence of polarity, or
especially hydrogen bonding, generally leads to higher melting point. Second factor is the
molecular shape. If the shape of the molecules allows them to be packed together, the
substance has a higher melting point than compounds with oddly shaped molecules.
5. Before packing into the capillary tube, a solid substance has to be powdered. Why is this
done on a watch glass rather than on a piece of paper?
It is done on the watch glass because some of the particles stay on the filter paper
and other small amounts of paper can mixed up on the substance that can screw up the
measurement. The paper can absorb some of the particles in the powdered substance
which is important in very small reactions like a capillary tube.

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