Extraction Lab

The extraction lab began with a .517g mixture of benzoic acid, p-nitroaniline, and azobenzene charged in a 125 mL Erlenmeyer flask mixed with 50 mL of Et2O. Once dissolved, the mixture is transferred the mixture into separatory funnel and begin acid extraction. 15 mL of 3 M HCl is added to the separatory funnel and inverted until a phase boundary is present. An additional 15 mL of 3 M HCl was then added and inverted again. The aqueous layer was removed through the separatory funnel and placed in a 250 mL Erlenmeyer flask labeled “acid.” 15 mL of a 3 M NaOH is added to the organic phase remaining in the separatory funnel and inverted until a phase boundary is formed. Another 15 mL of 3 M NaOH was added to the separatory funnel and again inverted until a phase boundary appeared. The aqueous layer was removed through the separatory funnel and placed in a 250 mL Erlenmeyer flask labeled “base.” The remaining solution present in the separatory funnel was removed from the top and placed in an Erlenmeyer flask labeled “neutral.” MgSO4 was added to the Erlenmeyer flask labeled “neutral” and set aside for 5 minutes to dry. The mixture is then filtered into a 58.4 g tared 100 mL round bottom flask, rotary evaporated, labeled “azobenzene” and placed aside to allow crude solid to dry. A portion of 6 M HCl was added to the Erlenmeyer flask labeled “base” until the solution became acidic. The solution was then placed in an ice bath for 5 minutes and filtered via vacuum filtration. Recovered solid was placed in a beaker labeled “Amine” and placed in a lab drawer to dry. A portion of 6 M NaOH …show more content…
0.004g of Benzoic Acid was recovered, 0.009g of p-Nitroanilie was recovered, and 0.057g of Azobenzene was recovered. The melting point of azobenzene was determined to be 118oC to 145oC. An insufficient amount of p-Nitroanilie and benzoic acid were recovered after recrystallization therefore the melting points could not be