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Distillation Procedure:

Creating the Calibration Curve:

1. Plug in the Refractometer (23) and ice bath (32).

2. Obtain ice from the Chemical Engineering office, fill the ice bath about half way with

ice, and add water.

3. Adjust the heating to keep the system at 32°F.

4. Create samples of methanol and water by mixing solutions of 0-100% (use increments of

10) methanol by volume in small test tubes (cover with para-film until testing).

5. Place sample under the illumination prism (30), look through the eye piece (24), press the

illumination button near the back of the machine then adjust the X to line up with the

vertical line using the fine tuning knob (26) and record the value of refraction.

6. Clean off sample with the provided Kimwipes and repeat for all the samples to create a

calibration curve of refraction versus volume percent of methanol.

Using the Batch Distillation Column:

1. Make sure the drain valve for the filling tank (5) is set to the “Fill” setting and the tank is

closed.

2. Measure out 1.6 L of methanol and pour it through the funnel (21) into the filling tank (5)

then add 32 L of water to the tank using the filling tank hose just above the funnel to

create 0.05% by volume mixture.

3. Once the tank is full turn the Fill/Drain valve to “Drain” then open the filling tank valve

(22) to allow the mixture to fill the round bottom flask (15) of the distillation column.
4. When the filling tank (5) is empty close the filling valve (22) and call the TA or

instructor to turn on the reboiler (16).

5. Record the temperatures of thermocouples using the digital thermometer (14) every 20

minutes until steady state is met.

6. Obtain samples of vapor and liquid from each stage using the vapor and liquid release

valves (17 and 19).

7. Use the refractometer (23) to obtain the refraction index of each sample (Use the same

procedure as the calibration curve).

8. Once all the samples are collected and measured turn off the column and allow it to drain.

9. Unplug and clean the refractometer (23) and ice bath (32).

10. Dispose of samples accordingly.

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