Objective: To perform a simple distillation and fractional distillation experiments of the known sample and based on the data

obtained from both the experiments, plot distillation curves for both simple and fractional distillation experiments. Perform a fractional distillation on the unknown sample and isolate the two compounds and determine the compounds and their percent concentration.

Assembly: 1) To assemble the apparatus, place a support ring with electric flask heater and attached a flask to it. 2) Place ceramic stones in the flask to promote even boiling of the liquid. 3) Apply the grease strip to all the joints and without twisting firmly fix the joints into each other, thus eliminating any air present. At this point the joints will look transparent. (Avoid over grease as this may contaminate the sample.) 4) Start a small stream of water into the condenser receiver through the nearest water supply. (The heat capacity of the water is quite high and hence a small stream is required. Take care to avoid forceful stream as this will cause the pipes to pop.) 5) Attach the distillation head to the flask using a clamp or rubber band. 6) Next attach the thermometer in the top opening of the distillation head. (Take care to avoid the contact of thermometer bulb and the liquid in the flask.) (Note: You might need to calibrate the thermometer at this point.) Procedure for simple distillation: 1) Take an oven dried 100 mL flask and place 30 mL of cyclohexane ad 30 mL of toluene along with ceramic boiling chip or stones. 2) Set up the assembly as described above. 3) Heat the flask till the liquid start to boil (heat the sample at reflux). never dry heat the sample always remember to start a stream of water. 4) As soon as the liquid starts to distillate, lower the heat till the liquid distillates at the rate of one drop per second. 5) At regular intervals record the temperature and also the volume collected. 6) As soon as 50 mL is collected, stop the heat and water supply and stop the distillation process. And store the sample for further testing. 7) Record the barometric pressure and make the any correction required for the thermometer. Plot a graph of boiling point VS volume.

The fractional distillation assembly is similar to the simple distillation assembly.

Procedure for fractional distillation: 1) Cool the earlier 100 mL flask completely and add the distillate collected back to the flask. Remove the previous boiling chips or stones and add fresh boiling chips to the flask. 2) With the use of electric heater heat the flask gradually just about till the liquid in the flask is boiling. 3) As soon as the liquid is boiling turn down the power to lowest and observe a ring of condensate which rises slowly through the column. If the ring is not visible, cautiously touch the column to observe that an area between the hot portion of column and cold portion of column. 4) At this point take care not to increase the temperature to achieve a uniform temperature gradient in the column. 5) Once the ring of condensate stops rising, slowly increase the heat. (Note it should take several minutes for the ring of condensate to rise to the top). 6) Once the distillation has started maintain the temperature such that 1 mL of distillate is collected over 1.5 to 2 mins time span. Observe the flow and increase or decrease heat as required. 7) At this point insulate the column with the use of glass wool or aluminium foil. This will avoid flooding of the column and a steady distillation can be performed. 8) Record the temperature and volume after each millilitres. Record the temperatures more frequently when there are abrupt changes in the temperature. 9) After the cylinder is filled empty it into the labelled 25 mL Erlenmeyer flasks. 10) Stop the distillation when the second constant temperature is attained. 11) Plot a distillation curve and report the observation in the column during the distillation process. 12) Combine the pure fractions and put the product in the bottle. Label it with your name, desk number, product name, boiling point range and weight. Submit the bottle. Procedure for the fractional distillation of unknown compound: 1) The unknown compound will be provided with to you by the instructor. 2) This compound will be a mixture of two soluble solvents. Both the compounds will have the melting points at least 20 0C apart. The compounds will be mixed in the concentration of 20:80, 40:60 or 50:50 percentage. 3) Perform a fractional distillation on the compound and determine the unknown sample. (Note: I could not see the last page no 100. So confirm the last step)