Separation and Composition Determination of a mixture of Benzoic Acid and 4-Aminoacetophene
CH203-02
Fadwa Mekkaoui
Introduction:
The separation and composition of benzoic acid and 4-aminoacetophene undergoes a solvent -solvent extraction. The two solvents used are ethyl acetate and water. The choice was made specifically because they are insoluble in one another. Meaning the two wont dissolve in one another allowing us to see two discrete layers. The two solvents separate into two distinct layers, the less dense on the top and the denser on the bottom. In the case of water and ethyl acetate, water will be at the bottom since it has a density of 999.97 kg/m^3 and ethyl acetate at the top because its density is 897kg/m^3. Once the mixture of benzoic acid and 4-aminoacetophene is dissolved in ethyl acetate, the two phases can been separated using a separatory funnel. This experiment is green because there are no harsh conditions and is done at room temperature. Additionally the experiment is time efficient and can be done fairly quickly.
Results/Discussion:
The first layer to be separated was 4-aminoacetophene, H_2 O and HCl, once collected in a flask 12.4 mL of 3M NaOH were added until it tested neutral on pH paper and then an additional 5mL of 3M NaOH to make it basic, reaching a pH of 13. This told us that is was extremely basic. When the
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The benzoic acid had a melting range of (117℃-124℃) and a melting point of 123℃. The 4-aminoacetophene had a melting range of (106℃-112℃) and a melting point of 109℃. Since the melting points wee in the range of the melting points this means the crystals were fairly pure. The final mass of benzoic acid was obtained as 0.3043g and 0.6228g of 4-aminoacetophene were obtained. This amounted to a 46.104% recovery. Error could have occurred from not waiting for the base to
Then the reaction tube was capped but not tightly. The tube then was placed in a sand bath reflux to heat it until a brown color was formed. Then the tube was taken out of the sand bath and allowed to cool to room temperature. Then the tube was shaken until a formation of a white solid at the bottom of the tube. After formation of the white solid, diphenyl ether (2 mL) was added to the solution and heated until the white solid was completely dissolved in the solution. After heating, the tube was cooled to room temperature. Then toluene (2 mL) was added to the solution. The tube was then placed in an ice bath. Then the solution was filtered via vacuum filtration, and there was a formation of a white solid. Then the product was dried and weighed. The Final product was hexaphenylbenzene (0.094 g, 0.176 mmol,
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strong base ( contained OH ) were 100% ionized in water and they were all
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