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Melting Points and Mixed Melting Points. Experiment 1: Identify a compound by its melting point and mixed melting points. 113 - 115 o C 188 - 189 o C 183 - 186 o C 133 - 134 o C 135 - 137 o C 113 - 115 o C 110 - 113 o C 187 - 189 o C 133 - 135 o C. Acetamide
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Melting Points and Mixed Melting Points Experiment 1: Identify a compound by its melting point and mixed melting points. 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 Acetamide p-Aminobenzoic acid Camphoric Acid trans-Cinnamic Acid Malonic Acid p-Nitrophenol Resorcinol Succinic Acid Urea
Melting Point Tube A sample is put in the bottom of a melting point tube.
Put a small amount of the compound in the open end of the melting point tube. Fill Turn over and tape the closed end on the desk top until the compound falls to the bottom.
Use a Thiele tube filled with mineral oil to heat your sample. Thiele Tube
Attach the melting point tube to a thermometer. Attach Thermometer
Heat Rate Heat about 5o per minute until within about 10o of the melting point Near the melting point heat at 1 - 2o per minute
Temperature m.p. = Start - Finish Finished melting Starts to melt
Add Salt Ice melts at 0oC What happens to the melting point if salt is added? Ice melts!
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
Mp of Mixtures 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.
Plot of melting point vs. mole fraction water for mixtures of water and acetic acid. Eutectic point
Cool a acetic acid - water solution with a mole fraction water of 0.9 AcOH - Water
Heat a acetic acid - water solution with a mole fraction water of 0.9 AcOH - Water
Heat a acetic acid - water solution with a mole fraction water of 0.2 AcOH - Water
Pure Compounds 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.
Melting points are a measure of purity m.p. = 115o - 119o m.p. = 118o - 120o m.p. = 121o - 122o
Two of these bottles contain benzoic acid and one m-nitrophenylacetic acid. How do you tell what is in each bottle? m.p. = 120o - 122o m.p. = 120o - 122o m.p. = 120o - 122o
Mixed Melting Points Grind samples together to be sure they are mixed and then measure the melting point.
Results 1 2 3 m.p. = 120o - 122o Mixed 1 and 2 m.p. = 114o - 117o Mixed 1 and 3 m.p. = 115o - 118o Mixed 2 and 3
Procedure 1. Measure the melting point of your unknown 2. Run mixed melting points to confirm identification