Exercise 3

Exercise 3 - September 25, 2008 Sec. #13 Thu 2:30pm Chan...

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September 25, 2008 Chan Huynh Sec. #13 Thu 2:30pm Exercise 3 Title: Separation and Analysis of the Components of a Mixture Objective: To isolate different substances of an unknown drug and to identify the components by using their melting point. Reaction: Compound Melting Points, °C Aspirin 134-136 Acetanilide 112-114 Acetaminophen 169-172 Phenacetin 133-134 Salicylic Acid 158-161 Sucrose 186 (decomposes) Starting Material Amount Added Isolation of Component A Dichloromethane 6.5mL Separation of Layers 5% aqueous sodium bicarbonate solution 5.0mL Acetone 3.0mL Isolation of Component B Deionized H 2 O 0.5mL Boiling Stone 1 Isolation of Component C Hydrochloric Acid 12 drops Boiling Stone 1
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September 25, 2008 Chan Huynh Sec. #13 Thu 2:30pm
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September 25, 2008 Chan Huynh Sec. #13 Thu 2:30pm Procedure/Visual Observations: Procedure Visual Observations 1. 5.0 mL of dichloromethane was measured out and added to the vial with the unknown drug. 2. The vial was capped and shaken vigorously. 3. The solution in the original vial was added to a Hirsch funnel and vacuum filtrated. 4. Vial was rinsed with 0.5 mL of dichloromethane and the rinse was added to the funnel. 5. The filtrate in the Erlenmeyer flask was transferred to a 30mL separatory funnel. 6. The empty flask was rinsed with 1.0mL of dichloromethane and added to the funnel. 7. 2.5mL of 5% aqueous sodium bicarbonate solution was added to the solution in the funnel. 8. The funnel, capped, was shaken vigorously and then vented. This process was repeated 3 more times. The funnel was then left, uncapped, until two separate layers were formed. 9. The bottom layer was drained through the spout into a vial, labeled B. The top layer was transferred to a vial, labeled C. 10. The contents of vial B was returned to the separatory funnel. Another 2.5ml of 5% aqueous sodium bicarbonate solution was added to the separatory funnel. 11. The solution was, again, shaken
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Exercise 3 - September 25, 2008 Sec. #13 Thu 2:30pm Chan...

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