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Experiment 1

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Camille Alimento
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16 views

Experiment 1

Uploaded by

Camille Alimento
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Experiment 1

DETERMINATION OF MELTING POINT


The normal melting point of a solid is defined as the temperature at which the solid and liquid are
in equilibrium at a total pressure of 1 atmosphere. In contrast to the volume change that accompanies the
vaporization of a liquid, the change in volume that takes place upon the melting of a solid is very small.
This makes the melting point of a solid, unlike the boiling point of a liquid, practically independent of any
ordinary pressure change. Since the melting point of a solid can be easily and accurately determined with
small amounts of material, it is the physical property that has most often been used for the identification
and characterization of solids.

Objectives:
1. To determine the melting points of a pure and impure compounds.
2. To describe how the structure affects the melting point of the compounds.

Materials: Glass tubing (1 foot), mortar and pestle, microspatula, capillary tubes, Bunsen burner,
thermometer, rubber bands, beakers (250mL), iron stand, tripod, butterfly clamp, copper stirrer, wire
gauze

Reagents: Glycerol or cooking oil, Salicylic acid, benzoic acid, oxalic acid, and impure benzoic acid

Samples to be tested: Salicylic acid, benzoic acid, oxalic acid, and impure benzoic acid

Note! Make sure all materials are clean and dry. Each sample must have individual container and testing
of samples must be done separately to avoid contamination.

Procedure:
Filling a Capillary Tube

Usually, the melting point capillary can be filled by pressing the open end into a small heap of the crystals
of the substance, turning the capillary open end up, and vibrating it by drawing a file across the side to
rattle the crystals down into the bottom. If filing does not work, drop the tube, open length of glass tubing
about 1 foot onto a hard surface such as stone desk top, or the iron base of a ring stand. The solid should
be tightly packed to a depth of 2-3mm.

Total of eight, 8, melting capillaries will be prepared for this experiment. Four
capillaries will be subjected for rough method and the other 4 will be subjected
for accurate method.

Melting Point:
Attach the capillary tube to the thermometer with a rubber band. Adjust the
capillary so that the sample is directly adjacent to the bulb of the thermometer.
Refer to figure.1. Place the thermometer with the capillary tube into the oil bath,
not touching the bottom of the beaker.
A. Rough Method
1. Apply heat to the oil bath. Note the temperature at which the sample starts melting, T1, and the
temperature when the sample is completely melted, T2.
2. Compute the difference between the two temperature readings which represents the melting
point range, MPR.
Equation: MPR = T2 – T1.

B. Accurate Method
1. Heat the oil rapidly until the temperature is 10 – 15 degrees lower than the temperature
obtained in the rough method.
2. Then gently raise the temperature at the rate of 1 – 2 degree per minute.
3. Note the temperature when a sign of melting appears, T1, and the temperature when the sample
is completely melted, T2.
4. Solve for the MPR

Result and Observation:

Questions:
1. What is melting point?
2. What is the melting point range of the pure samples?
3. How does the melting point range of a pure sample differ that of an impure sample?
4. How does the melting point range of rough method and accurate method differ?
5. Which of the samples has the highest melting point? Discuss basing on the structures of the
compounds?

Conclusions:

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