UNKOWN: R

Ali Hussein Sabr | Pharmaceutical Chemistry | 21/2/2024

Supervised by: Assist. Prof. Dr. Karima Fadhil Ali
The melting point of a substance is a fundamental characteristic used for identification,
quality control, and purity assessment. It provides valuable insights into the molecular
structure and intermolecular forces present within the material.

The melting point (m.p)0C of a compound is the temperature at which it changes

from a solid to a liquid. Since this requires that the intermolecular forces that hold the
solid together have to be overcome . The melting point is a physical property (melting
point, boiling point, density, solubility ,etc.) often used to identify compounds .
Usually, chemists can only obtain a melting range of a 2 - 3oC accuracy.
A pure, nonionic, crystalline organic compound usually has a sharp and characteristic
melting point (usually 0.5-1.0 0C range). A mixture of very small amounts of miscible
impurities will produce a depression of the melting point and an increase in the
melting point range .
Melting point range: The interval between the temperature at which a solid sample
just begins to turn to liquid and the temperature at which the entire sample becomes
liquid. or range of temperatures in which the first crystal starts to melt until the
temperature at which the last crystal just disappears.
What are the factors that affect the melting point?
1- Molecular weight
Melting points are higher for higher molecular weight compounds. The reason the
melting point increases with the weight is that it takes more energy to separate larger
molecules from a crystalline structure than it takes to separate smaller ones.
2- The nature of the organic compound s
Ionic compounds, often form crystal lattices in which each ion is surrounded by ions
of the opposite charge ,because of the strength of this electrostatic attraction,. Breaking
up an ionic crystal lattice requires considerable energy as a result, ionic compounds
have high melting points, While the Covalent compounds consist of molecules
rather than ions. Since the attraction between molecules is weaker than is the
attraction between ions, covalent compounds usually have a lower melting point than
ionic compounds. Moreover, some covalent compounds have polar molecules in which
one end is more electronegative than the other, such polar compounds have a higher
melting point than nonpolar molecules .
3-Impurities
Impurities decrease the melting point. ice-salt mixtures. contaminants normally lower
the melting point and broaden the melting point range Pure samples usually have
sharp melting points, for example( 149.5-150)0C, impure samples of the same
compounds melt at lower temperatures and over a wider range, for example 145-1480C
.

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 4-Shape of Molecules
Molecular shape influences the melting point of a substance. If the shape of the
molecules allows them to be packed together in a compact fashion, For example,
symmetrical molecules give compound ( 4- n –propyl benzoic acid ) a higher melting
point than that of ( 4- iso –propyl benzoic acid ) , the molecules of which do not pack
well,

What is a Melting Point Apparatus?

A melting point apparatus is a specialized scientific instrument designed to measure
the temperature at which a solid substance transforms into a liquid state. This tool
plays a crucial role in various research and industrial applications where knowing the
melting point is essential.

Working Principle of Melting Point Apparatus

The apparatus functions on the principle that a pure compound transitions from a solid
to liquid state over a narrow temperature range. The temperature at which this
transition occurs is recorded as the melting point.

Importance of Accurate Melting Point Determination

Accurate melting point determination is crucial for ensuring the quality and purity of
substances. It aids in identifying potential impurities or deviations from expected
molecular structures.

Applications in Various Industries

Pharmaceutical Industry
In drug development, the melting point helps assess the purity of active pharmaceutical
ingredients, ensuring the safety and efficacy of medications.
Chemistry Research
Chemists utilize melting point data to characterize and synthesize compounds,
enabling advancements in various chemical applications.
Material Science
Melting point analysis aids in understanding material properties, assisting in the
development of new materials for diverse industries.

Factors Affecting Melting Point Measurements

Various factors, including pressure, impurities, and sample size, can influence melting
point measurements, underscoring the need for controlled conditions.

Advantages of Automated Melting Point Apparatus

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 Automated apparatus offer increased accuracy, reproducibility, and efficiency
compared to manual methods, enhancing research and industrial processes.

How does a melting point apparatus determine the melting point of a substance?
The basic principle behind a melting point apparatus involves carefully heating a small
amount of the substance at a controlled rate while monitoring its temperature. Here's
how the process works:
1. Sample Preparation: A small amount of the substance whose melting point
needs to be determined is placed in a small capillary tube. The substance is
usually finely powdered or crystalline in nature.
2. Insertion of Capillary Tube: The capillary tube with the sample is placed
inside the melting point apparatus. The tube is usually positioned in such a way
that the sample is observed through a magnifying lens or a digital camera.
3. Heating: The apparatus is equipped with a heating element, often an electrical
coil or a hot plate. The heating rate can be controlled, ensuring a gradual increase
in temperature. This slow heating allows for precise determination of the melting
point.
4. Observation: As the temperature of the apparatus increases, the substance in
the capillary tube starts to heat up. At a certain temperature, the substance
begins to melt, transitioning from a solid to a liquid state. This is observed
through changes in the appearance of the substance, such as the formation of a
liquid phase, changes in color, or the disappearance of distinct crystalline
structures.
5. Recording the Melting Point: The temperature at which the substance
completely transforms from solid to liquid is noted as the melting point. It's
important to note that pure substances have a specific and sharp melting point,
meaning they transition from solid to liquid over a narrow temperature range.
Impurities or mixtures tend to lower and broaden the melting point range.
6. Cooling and Cleaning: After the melting point has been recorded, the
apparatus is allowed to cool down. Any remaining substance in the capillary tube
can be removed and cleaned for the next measurement.
7. Repetition: To ensure accuracy, the process may be repeated multiple times
using fresh samples of the substance.

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 Stuart SMP30 Melting Point
Apparatus.

Using the STUART SMP30

Melting point apparatus

Prepare you melting point tubes as per instructions and

insert into the sample holder. Ensure that you can see the
sample(s) clearly. Turn the machine on at the socket if
required. Once this screen is shown select ‘NEW
MEASUREMENT’ by pressing the button indicated.

Select the ‘NO’ option indicated to set

the plateau and ramp values you require

Adjusted the temperature you want the machine

to plateau at using the ‘UP’ and ‘DOWN’ buttons
indicated. When ready press the indicated
‘NEXT’ button to continue.

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 Adjust the ramp rate, this is a measure of how
rapidly the temperature will increase, by
pressing the ‘UP’ and ‘DOWN’ buttons as
indicated. When satisfied with the rate press
the ‘NEXT’ button as indicated.

Confirm that the plateau and ramp rate values are

correct and press the ‘START’ button as indicated.
At this point the machine will heat up to the
plateau temperature, the time taken to reach this
temperature will be indicated by a count.

Once the plateau temperature is stabilised a

countdown from 120 to 0 will begin followed by an
audible bleep. When this screen is shown press the
‘START RAMP’ button indicated to proceed.

During this ramping phase you should be observing

your sample, through the viewer, until it begins to
melt. Pressing the numbered buttons will record the
temperature at that point; each button corresponds
to one of the 3 sample holders. Each button can
record up to 7 values, with an audible bleep
following each successful recording.

To view the results recorded by pressing the buttons

in the previous step, press the ‘VIEW RESULTS’
button indicated.

The results are shown on screen. You can view more results
by pressing the ‘UP’ and ‘DOWN’ buttons, or view the
results recorded for the different tubes by pressing the
buttons numbered in the picture. Once finished press the
‘DONE’ button indicated.

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Aim of experiment
Identify an unknown compound using its melting point.

Procedure
A. Preparing the Sample
1. Take a capillary tube and close its one end by heating the end in the flame for 2-3
minutes while continuously rotating it.
2. Take naphthalene on a tile and crush it into a fine powder.
3. As shown in the figure below, firmly hold the closed end of the capillary tube
between your finger and thumb.
4. Dip the open end of the capillary tube in the finely powdered naphthalene.
5. Gently tap the capillary tube on the table to fill the compound in the capillary
tube to about a length of 1–2 cm.

B. Taking a Melting Point

To record the melting point range of a compound fill two capillary tubes each to a depth
of 2-4 millimeters with the compound of interest. First, get a rough idea of the
approximate melting point range. Place one of the tubes in the Melting point apparatus
and raise the temperature to 150 c (near the range of expected unknown organic
compound). Record the range of temperature from the first visible evidence of liquid
(the sample appears moist, or a tiny drop of liquid is observed) to the complete
liquefaction of the sample. Note the temperature at which the compound first begins to
melt. Allow the melting point apparatus to cool to about 20 °C below that temperature,
and then insert the second tube. Raise the temperature again. Note the temperatures at
which:
1- The first crystals melt, and;
2- At which the sample has completely melted. This is the melting point range.

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Result
Melting point of unknown organic
compound is
1- 110 -112 c.
2- 110 – 111.5 c.

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