NAME: CALISA JOSEPH ID#: 2013060012

LAB TITLE: MELTING POINT DETERMINATION DATE: 25.09.14

LAB PARTNER(S):

Abstract:
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Hypothesis:
The impurity of an unknown substance will record a melting point depression compared with the
pure compound, and will cause the melting point range to widen.

Introduction:
Melting point and boiling point are known as the physical properties of a compound that
provide important information which can help in the identification of a sample, characterize new
compounds or to establish its purity. In order to determine the identity of a solid compound using
the melting point technique one needs to compare its melting point with that of the true
compound.
The temperature at which a solid melts and becomes a liquid is known as the melting
point of that substance. Normally, a solid melts over a range of temperatures rather than at one
definite temperature. For this reason it is more appropriate to refer to this as a melting point
range. If the compound melts over a very narrow range (usually 0.5-1.0oC range), it suggests that
the compound is relatively pure. However, compounds that melt over a wide range are said to be
generally impure.
 The compounds that are used in today’s experiment are:-

Naphthalene Acetanilide Urea

In this experiment, the Thiele tube method is used where the capillary is immersed in a heated oil
bath. This system can also be used for boiling point determination. Before attempting this
experiment it is important to be aware of the safety precautions that surrounds it. The instruments
in this lab would be heated to high temperatures so it is necessary to handle the apparatus with
extreme caution. In addition to this, certain chemicals in the lab are considered irritants therefore
the appropriate protective wear (gloves and eye goggles) must be worn.
While performing the experiment ensure the substance is packed well in the capillary,
otherwise air pockets will form in the capillary. This causes one to obtain a lower melting range
than the actual range.

Procedure:
Refer to: CHEM 241 Lab Manual, Lab #4 Melting Point Determination, pg. 1-3
Flow Chart:

Obtain 0.5g of
sample in test
tube

Use spatula to crush

sample to a powder
on a hard surface

Push melting point

capillary in powder

Force powder
down the tube by
tapping to a height
of 2-3 mm

Record temp. Record temp.

at which last While using Thiele of 1st
solid tube appearance of
disappears drop of water

Repeat procedure for

part1, part 2 and part 3
Pre-lab Questions:
1. Indicate which of the following statements is true (T) and which is false (F).

False (a) An impurity raises the melting point of an organic compound.

True (b) A eutectic mixture has a sharp melting point, just as does a pure
compound.
False (c) If the rate of heating of the oil bath used in a melting-point
determination is too high, the melting point that results will likely
be too low.
False (d) The sample should not be packed tightly into a capillary melting-point
tube.
True (e) A heating bath containing mineral oil should not be used to determine
the melting points of solids melting above 200 °C.

2. Six (6) physical properties of organic compounds that are often measured by organic
chemists in attempting to identify a compound are: - 1. Melting point, 2. Boiling point, 3.
Electrical conductivity, 4. Thermal Conductivity, 5. Hardness and 6. Colour

3. Melting involves the change of state from a solid to a liquid by the addition of heat. The
particles in a solid are held together by strong electrostatic forces and contain vibrational
energy. When heat is applied to the solid the molecules vibrate rapidly to overcome these
forces which causes the solid to liquefy. Dissolving on the other hand is slightly different,
the solid or solute is incorporated into the solvent to form a solution.

4. Solids do not melt at one specific temperature but rather over a range of temperatures.
Therefore a melting point range would always be observed using conventional apparatus.

5. If two substances have the same melting point, a mixed melting point can be done.
Combine the same amount of the Unknown with A and B. Determine the melting points
of (Unknown + A) and (Unknown + B). The pure sample will melt at the same melting
point as the unknown, while the mixture will express a lower melting point. If (Unknown
+ A) has lower boiling point and (Unknown + B) has the same melting point as pure A
(or pure B), then the Unknown is B. If Unknown + A is the same, and Unknown + B is
lower, then Unknown is A.

6. It is possible that the unknown compound is an amorphous solid. Amorphous solids lack
a repetitive crystalline structure and definite melting points; thus giving them the ability
to flow over a range of temperatures.
Results/Data:
Part 1- Comparison of Literature and Observed Melting Points

Naphtalene Acetanilide Urea

Literature mp

Observed mp range

Part 2- Determining the Identity of an Unknown by Melting Point

Unknown # ______________

preliminary mp range

mp range

Identity

Structure

Physical properties

Hazardous properties
 Part 3- Mixed Melting Point Determination

Unknown # ________/Identity of Unknown ________________

Mixed mp range
Identity of Unknown confirmed? (circle YES NO
answer)

If NO, continue……

Mixed mp range
Identity of Unknown confirmed? (circle YES NO
answer)
Discussion:
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Conclusion:
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References:
 University of Massachusetts. Melting Points.
http://www.chem.umass.edu/~samal/269/extract.pdf (Accessed September 9, 2014)

 Zubrick, J. The Organic Chem Lab Survival Manual, 6th ed.; John Wiley and Sons, 2004.

 Bruice, P. Organic Chemistry, 7th ed.; Pearson: Santa Barbara, 2011