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Exp 1

This document describes an experiment on determining melting points of organic compounds. The objectives are to determine melting points of various organic compounds and use them to identify unknown samples. Key steps include using a Mel-Temp apparatus or oil bath to heat samples in capillary tubes and record the melting range. Melting points can indicate purity and be used to identify unknowns by comparing to known compounds. Sample preparation is important for accurate results. Data is recorded on melting points of known compounds and any unknown samples.

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74 views11 pages

Exp 1

This document describes an experiment on determining melting points of organic compounds. The objectives are to determine melting points of various organic compounds and use them to identify unknown samples. Key steps include using a Mel-Temp apparatus or oil bath to heat samples in capillary tubes and record the melting range. Melting points can indicate purity and be used to identify unknowns by comparing to known compounds. Sample preparation is important for accurate results. Data is recorded on melting points of known compounds and any unknown samples.

Uploaded by

tamanranya234
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Organic Chemistry

MLS Department, University of Raparin


College of science

EXP: 1
Melting Point
Lecturer: Ali R.Hamad
2022 - 2023
2/28/2023 1
Introduction:

Melting Point (MP): the melting point of a compound is the


temperature at which it changes from solid to liquid form at
standard atmospheric pressure.

In practice, a solid usually melts over a range of temperatures


rather than at one specific temperature. For this reason it is
more useful to speak of a melting point range.

Melting Point Range (MPR): The difference between the


temperature where the sample starts to melt and the
temperature where melting is complete

2/28/2023 2
Generally, melting points are taken for two reasons:

1- Determination of purity.
2- Identification of unknowns.

1- Determination of purity:

➢ If the compound melts over a very narrow range, it can usually be


assumed that the compound is relatively pure. Conversely,
compounds that melt over a wide range are assumed to be
relatively impure.
➢ Also impure solids also melt at a temperature lower than that for
the pure compound.
➢ If the range of melting point is greater than 2°, usually indicates an
impure compound. For example, if an unknown solid melts at 102-
106°C, the 4° range suggests that the sample is impure.
2/28/2023 3
Range of (MP) and purity:

1. If (0.5-1)°: The substance is very pure.

2. If (1-2)°: The substance is pure.

3. If Greater than 2°: The substance is impure.

2/28/2023 4
2- Identification of unknowns:
Part One: Chemical Classification
1. Preliminary classification by physical state, color, and odor
2. Melting-point or boiling-point determination; other physical data
3. Purification, if necessary
4. Determination of solubility behavior in water and in acids and bases
5. Simple preliminary tests: Beilstein, ignition (combustion)
6. Application of relevant chemical classification tests
Part Two: Spectroscopy
7. Determination of infrared and NMR (proton and 13C, if available) spectra
8. Confirmation of structure

The type of compound and functional group should be discovered after completing
Part One. Spectroscopy (Part Two) will be used principally to confirm the structural
assignment and to provide further information toward identifying the unknown.

2/28/2023 5
Purpose of this experiment:

The purpose of this experiment is to determine the melting


points of various organic compounds and to use these to identify
unknowns.

Equipment / Materials:

Mel - Temp apparatus capillary tubes


Thermometer beaker
mortar and pestle (optional) solid organic compounds

2/28/2023 6
Melting point can be measured either by using:
A. Mel-temp apparatus.
B. Oil bath.

Oil bath Mel-temp apparatus.

2/28/2023
Procedure:
1. Obtain a capillary melting point tube and a known compound. Press the open
end of the capillary gently into the substance several times.
2. Pushed the powder to the bottom of the tube by repeatedly pounding the
bottom of the capillary against a hard surface (preferred method).
3. Place the capillary melting point tube in the Mel-temp apparatus chamber or
oil bath. Heat slowly to acquire the most accurate results. Record the melting
range, which begins when the sample first starts to melt and ends when the
sample is completely melted.
5. Allow the Mel-Temp to cool. Obtain an unknown sample and determine its
melting range. Identify the unknown by comparing the data of the knowns the
class has obtained.

2/28/2023 8
Sample Preparation:

Careless preparation of a sample is the leading cause of inaccurate


and irreproducible results in melting point determinations.

Any substance being loaded into a melting point capillary must


be:

1. Fully dry.
2. Homogeneous.
3. In powdered form.

2/28/2023 9
Data Table:

Medical Laboratory Science (MLS) Group:______

Name: ___________________________ Date: ___/____/_____

Physical State: ______________

Known Compounds:
compound melting range - oC

compound melting range - oC

Unknown:
compound melting range - oC
Unknown : ___________
identity of
compound

2/28/2023 10
Benzil 94 - 95
Mandelic acid 119 - 121
Benzoin 134 - 136
Acetylsalicylic acid 138-140
Salicylic acid 158 - 160
Benzoic acid 122 - 124
L-tartaric acid 171 - 174

Questions:
1. Define the "melting point" of a substance.
2. What is the purpose of determining melting points?
3. Why is this method not used for finding the melting points of inorganic
compounds?

2/28/2023 11

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