A Beginners Guide to the Rotary Evaporator Tom Aborn Introduction The goal of organic synthetic chemical research is to learn

about the mechanisms and products on new chemical reactions. Many chemical reactions, like the infamous baking soda and vinegar volcano reaction, occur instantaneously. Organic reactions, however, tend to be long, slow, arduous processes that take hours, days, and sometimes even weeks to run to completion. To expedite the process, chemists use solvents in their reactions. For the purposes of this guide, a solvent will refer to the low boiling, nonreactive liquid that is used to dissolve the reagents (ingredients). Solvents help to mix up the reagents of the reaction and make sure they come into contact more frequently, meaning that they will react more frequently, and thus speed up the overall process of the reaction. There is a draw back to using solvents, however. When the reaction is finally completed, the solvent will still be mixed in with the product of your reaction, meaning that your data concerning the product of your reaction will be corrupted by the solvent. This isnt too much of a problem for an undergraduate chemistry lab, because it is possible when analyzing your product to discern which data relates to the compound you made, and which data refers to the solvent that was used. In a professional pharmaceutical lab, however, you cannot present a drug you have made for testing if it still has solvent mixed into it. While solvents are great for moving chemical reactions along, they are not to be ingested and can often be harmful to the body. Therefore, it is necessary to find a way to completely remove the solvent from your product. One way of doing this is to use the rotary evaporator (rotovap). How the Rotovap Works: A basic overview

Figure 1: Diagram of a typical rotary evaporator. Photo courtesy of http://www.flickr.com/photos/danes96/18308428/.

The rotovap takes advantage of the low boiling points of solvents by creating an environment where the solvent will rapidly boil off leaving only your product. Conditions that are most conducive to boiling are: low air pressure and high temperature. The Rotovap works as such: (A) Round Bottomed Flask: This flask contains your product and the solvent you are trying to remove. It is attached to an axle that rotates the flask. This creates a thin layer of solvent mixture on the sides of the flask that will evaporate more quickly. (B) Heating Dish: The heating dish is filled with distilled water, which is heated and begins the evaporation process. (C) Condenser Coil: As the solvent begins to evaporate, the glass case surrounding the coil will begin to fill up with vapor. The condenser coil will help to condense the vapor back into liquid to avoid dangerous pressure buildups. (D) Water Hose: Attached to an external water source, the water hose runs cool water through the condenser coil (D) and keeps it cool enough to allow the vapor to condense on it. (E) Vacuum Hose: Connected to an external vacuum pump, the vacuum hose removes the air from the chamber surrounding the condenser coil (D). The removal of air pressure by the vacuum hose allows the solvent to evaporate faster and with less heat required from the heating dish (B). (F) Pressure Valve: Cuts the chamber surrounding the condenser coil off from the atmosphere, preventing any air pressure from replacing the air removed by the vacuum hose (E). (G) Collection Flask: When the evaporated solvent condenses on the condenser coil (D), it drips down into the collection flask. What you do with the extra solvent is up to you. (H) Control Panel: This panel contains the controls for raising and lowering the round bottomed flask in and out of the warm water in the heating dish (B), the controls for the speed of rotation of the flask, and controls for how warm the water in the heating dish is. Instructions for Using the Rotovap: Use the following steps to safely remove the solvent from your product. CAUTION: ALWAYS use proper eye protection when in the laboratory. 1. Pour your mixture into a round bottomed flask. Choose a flask big enough so that it is no more than half full with your mixture. If necessary, use two flasks and rotovap them separately. 2. Attach your round bottomed flask to the apparatus, using a clip to fasten it into place. 3. Attach vacuum hose (E) to the top plug, and water hose (D) to the bottom plug. 4. Close pressure valve (F) to prevent any air from entering the chamber. 5. Ensure that your collection flask (G) is clasped firmly into place.

6. Turn on the vacuum and the water flow from their external sources. The water pressure should be high enough that once it has flowed through the condenser coil, the water is gently flowing from the exit hose (not shown). 7. Some rotovaps have a pressure gauge attached to read the pressure inside the chamber. If your rotovap contains a pressure gauge, wait until it reads around 200 torr or 0.25 atmospheres (atm), based on what units of pressure the reader uses. (Note: Another unit that may be used is a Pascal. A Pascal (Pa) is equal to 1 torr.) 8. If there is no pressure gauge, wait around 10 seconds for the pressure to drop. If you have waited 10 seconds or the gauge reads the proper pressure level, you are ready to begin. 9. DO NOT turn off the vacuum or water hose, DO NOT open the pressure valve. Use the control panel to heat the water bath to 40oC. If your solvent does not evaporate at 40oC under the reduced air pressure provided by the rototvap, then you need to find another way to remove your solvent. 10. Once the bath begins to heat, use the control panel to lower the flask into the bath. It should be lowered such that the flask barely touches the water: this ensures that the mixture is heated slowly. If the mixture is heated too fast, then your mixture will bump. See caution below. 11. Once the flask is barely touching the water, use the control panel to begin rotating your sample. The flask should rotate just enough that the solvent forms a thin, filmy layer on the side of the flask. The rate of rotation required is not high, but may vary depending on flask size and the volume of your mixture. 12. Allow your sample to rotate and heat for 5-10 minutes or more, depending on the volume of your mixture. 13. There is no definite way to know you are done. Watch the volume of your mixture and the amount of solvent collected in the collection flask to make an educated guess as to how much heating/rotation is necessary. 14. When you think you are done, stop the rotation and raise the flask out of the water. 15. TURN OFF the vacuum hose. 16. Turn off the water hose. 17. OPEN the pressure valve. 18. WAIT UNTIL THE AIR PRESSURE HAS BEEN RESOTRED TO THE CHAMBER BEFORE REMOVING YOUR MIXTURE. See warning below. If your rotovap has an air pressure gauge, wait until the gauge reads around 740 torr (or PA) or around 1 atmosphere (atm). If you do not have a gauge, you can listen. When you open the valve you should hear the air rushing into the chamber, making a whistling-like sound. Wait 5-10 second until AFTER the whistling has subsided to proceed. 19. When the whistling has subsided and air pressure is restored to the chamber, you may unclip your sample and remove it from the rotovap. CAUTION: Bumping is, in laymens terms, a hard bubble: the mixture bubbles so hard that it flies out of the flask all over the chamber. That is very bad and may ruin your mixture, do not let it happen.

WARNING: If you attempt to remove your flask from the rotovap BEFORE air pressure has been restored to the chamber, your sample WILL bump. It will bump so hard that your sample will fly out all over the chamber and be lost, and you will have to start your experiment all over. Trust me, I know.