Learn the essential components of a distillation apparatus before scaling up.
Distillation is a separation technique that selectively separates a pure liquid substance from other compounds and impurities based on their boiling point. One of the most widely known example of this practice is used in steam distillation of water to provide clean pure water and distillation of ethanol from a fermentation broth. The mixed liquid is heated slowly to a temperature where the compound of interest reaches its boiling point. The temperature is held at this point until the compound has boiled away and then the temperature begins to rise again. The fumes rise in a column, constantly condensing and dripping back into the mixed liquid, until they are drawn down a side port that is cooled by recalculating water. The fumes condense on the cold surface of the condenser and drip out the exit port as a purified product.
Instructions
1. Wash all the components and allow to completely dry. You do not want any residual chemicals from previous use to be carried over into the next use.
2. Position an electrical heater with enough room to construct the distillation apparatus. Clear away items that may hit the apparatus and break the glass.
3. Clamp a round bottom flask above the electrical heater and insulate with insulating tape to contain the heat.
4. Lightly grease the ground glass fitting on the distillation column with silicone vacuum grease. This helps to prevent fumes from leaking out of the distillation apparatus during operation.
5. Place the bottom of the distillation column in the ground glass fitting in the top of the round bottom flask. Clamp the distillation tube to hold it in place.
6. Place a rubber stopper in the top port of the distillation head and thread a thermometer through the hole in the stopper. Position the bulb of the thermometer at the same level as the side exit port.
7. Coat the two ground glass fittings on the distillation head with the silicone vacuum grease and place in the top of the distillation column.
8. Install a clamp to hold the unit together. Clamping the pieces provides a stable support for the apparatus.
9. Fit the condenser onto the side port of the distillation head. The condenser must be hooked to a cold water supply at the bottom port and a drain from the upper port. Water will flow around the inner tube to provide a cold surface to condense the hot fumes. Clamp the condenser in place to provide support.
10. Apply grease to the end of the condenser and attach the vacuum takeoff on the end of the condenser. Support the end of the vacuum takeoff with a clamp.
11. Position the collection vessel under the drip tip of the vacuum takeoff. In chemical applications, a graduated vessel such as a graduated cylinder is used to allow for measuring the amount of product recovered from the mixture.
12. Remove the round bottom flask and fill with the liquid mixture to be distilled and add a few boiling chips to create even heating and boiling without explosive bumping of the liquid.
Tags: bottom flask, distillation column, distillation head, ground glass, round bottom, round bottom flask, vacuum takeoff