experiment 1: identify a compound by its melting point and mixed melting points. acetamide...
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Experiment 1: Identify a compound by its meltingpoint and mixed melting points.
Acetamide
p-Aminobenzoic acid
Camphoric Acid
trans-Cinnamic Acid
Malonic Acid
p-Nitrophenol
Resorcinol
Succinic Acid
Urea
113 - 115 oC
188 - 189 oC
183 - 186 oC
133 - 134 oC
135 - 137 oC
113 - 115 oC
110 - 113 oC
187 - 189 oC
133 - 135 oC
Melting Points and Mixed Melting Points
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A sample is put in the bottom of a melting point tube.
Melting Point Tube
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Put a small amount of the compound in the open end of the melting point tube.
Turn over and tape the closed end on the desk top until the compound falls to the bottom.
Filling Tube
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Sample in the melting point tube.
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Use a Thiele tube filled with mineral oil to heat your sample.
Thiele Tube
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Attach the melting point tube to a thermometer.
Using Thiele Tube
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Heat about 5o per minute until within about 10o of the melting point.
Near the melting point heat at 1 - 2o per minute
Heating Rate
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Mel-Temp in the lab
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Starts to melt Finished melting
m.p. = Start - Finish
Temperature
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Why is salt put on snow covered roads?
Salt on Roads
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What happens to the melting point if salt is added?
Ice melts!
Ice melts at 0oC
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Impurities such as salt lowers the melting point of water.
Putting salt on icy roads causes the ice to melt because it lowers the melting point of water.
Impure compounds usually melt lower than pure compounds so the melting point may be used as a measure of the purity of a compound
Impurities
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Acetic Acid, CH3COOH, is a colorless liquid that melts at 16.6oC.
Let’s look at the melting point of mixtures of water and acetic acid.
Acetic Acid
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Plot of melting point vs. mole fraction water for mixtures of water and acetic acid.
Eutectic point
Eutectic Point
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Cool a acetic acid - water solution with a mole fraction water of 0.9C
Cool
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Heat a acetic acid - water solution with a mole fraction water of 0.9
Heat
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Heat a acetic acid - water solution with a mole fraction water of 0.2
Heat
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Pure compounds usually melt over a narrow temperature range, often 1o or less.
Impure compounds melt lower than pure compounds and over a wider temperature range.
Pure - Impure
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m.p. = 115o - 119o m.p. = 118o - 120o m.p. = 121o - 122o
Melting points are a measure of purity
Purity
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m.p. = 120o - 122o m.p. = 120o - 122o m.p. = 120o - 122o
Two of these bottles contain benzoic acid and one m-nitrophenylacetic acid.
How do you tell what is in each bottle?
Unknown
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Grind samples together to be sure they are mixed and then measure the melting point.
Mixed Melting Points
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m.p. = 114o - 117o
m.p. = 120o - 122o
m.p. = 115o - 118o
Mixed 1 and 2
Mixed 1 and 3
Mixed 2 and 3
1 2 3
Results
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1. Measure the melting point of your unknown
2. Run mixed melting points to confirm identification
Summary