Preparation of Pure Diphenyl

The main method to manufacture ethyl ethanoate is the esterification of ethanol with acetic acid. A mixture of acetic acid and ethanol with a small amount of sulphuric acid is preheated and put into an esterfying column in which it refluxed. When the mixture is removed it goes to a second reflux column where 85% of acetate is removed. Then the water is mixed with the distillate \and then separated into two layers. One of the top layer is fed into the refluxing column from where the residue which contains 95% of ethyl acetate is distilled to remove any

Equipment- 250mL beaker, 125mL Erlenmeyer flask, cardboard square, chemical scoop, metric ruler, lab countertop, rubber stoppers, safety goggles, lab apron

A ring stand that was the base to hold everything, including the clamp and the solution calorimeter. 15 effervescent tablets, a styrofoam cup (outer insulator), and a plastic cup (reaction chamber). Plus, a stir plate and bar, and a Lab Quest unit to record the temperature changes. A 250mLs beaker, a

Grignard reagents are reactive enough to also attach esters; however, two equivalents of the Grignard reagent are usually added because less then two equivalents leave a large quantity of unreactive ester. This reaction forms a tertiary alcohol.

21) After all of the solid dissolves, move the flask from the hot plate and allow it cool to room temperature. After a while, crystals should appear in the flask.

items presently in solid form in the lab kit or purchased separately for this laboratory

The purpose of this lab is to separate a mixture and determine the percentages of each of the ingredients. Each substance will have a different boiling point due to its intrinsic properties and from that, we will be able to determine the purity of different products as we evaporate off the next level of product.

The materials needed for this experiment included test tubes, a test tube holder, the unknown compound #202, 35mL beakers, gloves, safety goggles, ethanol (to clean equipment), stirrer (to mix solutions), the 15 possible compounds that are provided, pH strips, distilled water, wooden splints, spatula to get out unknown compound #202, waste bucket, Bunsen burner, graduated cylinder, 500mL beaker for the waste, plastic dishes to measure out compound and the scale.

First, the simple distillation apparatus was set up. An oil bath was placed on a hot plate. A 100mL round-bottomed flask was submerged in the oil and held using a clamp and ring stand. The round-bottomed flask was then connected to the distillation head ensuring that the joint was greased. The thermometer was placed inside the distillation head so that the top of the bulb was level with the arm of the distillation head. The distillation head was attached then to the condenser held up by a clamp and ring

During the lab we had to use lab tubes, a pipette, beakers, safety goggles, gloves, oven top, beaker tongs, water,

Distillation of the first product began at 83 °C. A Pasteur pipette was used to remove 1-ml of the distillate into a vial. A second vial was filled with distillate until it reached 1-ml. As the second vial is being filled, observe the temperature and remove the apparatus from the heat source if there is an observed drop in temperature.

Crystallization was induced in the solution by scratching the inside of the beaker with a glass stir rod. 2. Next, an ice bath was made by partially filling a 400 mL beaker with ice and covering the ice with water. 3. The beaker containing the solution was then placed in the ice bath for approximately 15 minutes.

Transfer pipette, cleaning solution/detergent, beaker, thermometer, distilled water, top loading balance, 10ml volumetric pipette, 25mlvolumetric pipette, 100ml volumetric flask, 50ml measuring cylinder.

Once cooled, the mixture was then transferred to a separatory funnel using the funnel while avoiding adding the boiling chip. 10 ml of water was then added to the mixture. The mixture was gently shaken and the phases were allowed to separate. The funnel was then unstopped and the lower aqueous phase was drained into a beaker. 5 ml of 5% aqueous NaHCO3 was added and then shaken gently. A great deal of caution was taken into consideration because of the production of carbon dioxide gas which caused pressure to develop inside the funnel. The pressure needed to be released so the funnel was vented frequently. The phases were allowed to separate and the lower aqueous phases was drained into the beaker. After draining, 5 ml of saturated NaCl was added to the funnel and then shaken gently. Once again, the phases were allowed to separate and the lower aqueous phase was drained into a beaker. An ester product was produced and was transferred into a 25 ml Erlenmeyer flask. This organic product was then dried over anhydrous Na2SO4 to trap small amounts of water in its crystal lattices thus removing it from the product. Finally the ester was decanted, so that the drying agent was excluded from the final product.

An ice bath was prepared in a large beaker and a small cotton ball was obtained. 0.5 g of acetanilide, 0.9 g of NaBr, 3mL of ethanol and 2.5 mL acetic acid was measured and gathered into 50mL beakers. In a fume hood, the measured amounts of acetanilide, NaBr, ethanol and acetic acid were mixed in a 25mL Erlenmeyer flask with a stir bar. The flask was plugged with the cotton ball and placed in an ice bath on top of a stir plate. The stir feature was turned on a medium speed. 7mL of bleach was obtained and was slowly added to the stirring flask in the ice bath. Once all the bleach was added, stirring continued for another 2 minutes and then the flask was removed from the ice bath and left to warm up to room temperature. 0.8mL of saturated sodium thiosulfate solution and 0.5mL of NaOH solution were collected in small beakers. The two solutions were added to the flask at room temperature. The flask was gently stirred. Vacuum filtration was used to remove the crude product. The product was weighed and a melting point was taken. The crude product was placed into a clean 25mL Erlenmeyer flask. A large beaker with 50/50 ethanol/water