Objectives:
The purpose of this experiment was to perform the separation of aspirin, sucrose and an unknown analgesic, which are constituents of Panacetin using the methods of filtration, extraction, and purification
Structures:
Sucrose
Unknown
Aspirin
Table of Reagents and Solvents:
Substance
MW
Wt. or Vol.
Moles
MP or BP, ºC
Density
g/mL
Hazards
Panacetin na 2.014 g na na na Harmful if swallowed or inhaled.
DCM (35 mL + 5 mL +5 mL)
84.93 g/mol
45 mL na -97
1.33
Harmful by skin contact and eye and skin irritant
5 % NaHCO3 na 30 mL na 132
Approx.
Causes serious eye irritation
6 M HCl na 2 mL na -70
Approx.
Very corrosive and can destroy many clothing materials
Procedure:
Part A
2.014 g of Panacetin was measured and put inside a 125 mL Erlenmeyer flask. 35 mL of Dichloromethane (DCM) was added to the 125 mL Erlenmeyer flask. After addition of DCM the Panacetin lumps were crushed with a stirring rod. Next a fluted filter paper was pre-weighed. The filter paper weighed around .860 g. Gravity filtration was then used to filter the mixture into a 125 mL collecting flask. The mixture was filtered in order to separate the crude sucrose from the mixture. The original container was then rinsed through the filter paper again with 5 mL of DCM and the mass of filter paper containing sucrose was measured after it was dry. The last step was to perform the isolation of Aspirin. See image below.
Part B
The mixture of DCM and Panacetin were poured from the collecting flask into a seperatory funnel and two extractions were performed, using a total of 30 mL of 5 % NaHCO3. In the first extraction 20 mL of 5 % NaHCO3 was measured and poured into the seperatory funnel. A stirring rod was then used to stir the mixture until fizzing stopped. The seperatory funnel was then stoppered and shaken and the valve was gradually turned to allow the carbon