Researcher

Matthew McBride

Objective

To determine the solubility of 4-chlorobenzaldehyde in ethanol at 1C and 25C and characterize any product formed using SAMS HNMR method.

Procedure

Two saturated solutions of 4-chlorobenzaldehyde were created and warmed in a 45C water bath. One solution was then placed in a 25C bath and the other was placed in a 1C bath. The supernatant of each solution were anazlyzed by 500Hz HNMR to determine solubility. Any crystals formed were analyzed for possible hemiacetal formation.

Results

SAMS Sheet [Fix permissions JCB]

Discussion

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Conclusion

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Log

2012-02-15

10:20 Filled a beaker with water and placed it on a hot plate to create a 45C water bath.
10:29 3.4295g of 4-chlorobenzaldehyde was weighed out and placed in a 20mL glass test tube labeled Tube 1.
10:32 3.0296g of 4-chlorobenzaldehyde was weighed out and placed in a 20mL glass test tube labeled Tube 2.
10:38 Ethanol was added to each test tube to create an approximately 1:1 ratio of 4-chlorobenzaldehyde to ethanol solution. The test tubes were sealed with parafilm, inverted several times and placed in the 45C water bath.
10:40 Solid was observed on the bottom of each test tube, so each tube was inverted several times to throughly mix the solutions.
10:43 A 25C water bath was created. No solid was visible in either test tube.
10:44 Placed Tube 1 in the 25C water bath.
10:54 No crystals were visible in Tube 1.
10:59 Added Tube 2 to a 4C ice bath.
11:06 White crystals were visible in Tube 2 in the ice bath. Temperature of the ice bath was at 1C.
11:14 Suction filtration with a Buchner funnel was set up.
11:15 No crystals were visible in Tube 1 in the 25C water bath.
11:21 Tube 2 was removed from the 1C ice bath and the thick crystal solution was scraped out of Tube 2 onto the Buchner funnel.
11:22 An empty vial was weighed to be 4.7201g.
11:23 The crystals (white, fluffy looking) were left on the filter paper with suction applied to the funnel to dry the crystals.
11:26 The suction was disabled and the dried crystals were scraped from the filter paper to the vial. A small amount of the crystals were lost during this exchange, because a few of the crystals were not captured by the vial.
11:34 The weight of the vial with the crystals was 5.5884g.