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Reflux

  Heating accelerates the rate of a chemical reaction by increasing the average kinetic energy of the molecules. The temperature of a reaction mixture can be controlled in several ways, the simplest and most convenient being to use a reaction solvent that has a boiling point within the desired temperature range for the reaction. The reaction is than conducted at the boiling point of the solvent, using a water-cooled condenser to return the solvent vapors to the reaction vessel and prevent their escape.

1. Position the heat source, usually a heating mantle or hot plate.

2. Select a round-bottomed flask of the proper size. The reactants should fill the flask half way.

3. Clasp the flask to the heat source.

4. Add the reactants via a funnel to the flask. Mix the reactants by swirling or stirring.

5. Insert the reflux condenser into the flask and clamp it to secure.

6. Connect the water inlet (the lower connector) on the condenser jacket to a cold-water tap with rubber tubing. Run another length of tubing from the water outlet (the upper connector) to a sink.

7. Turn on the water carefully so that the condenser jacket slowly fills with water from the bottom up. Adjust the water pressure so that a narrow stream flows from the outlet. It is important to have a flow rate that is great enough to maintain a continuos flow of water in spite of pressure changes in the water line. Also make sure to keep the condenser at the temperature of the tap water during the reaction.

8. Turn on the heat source. Adjust to maintain a gentle boiling of the solvent.

9. Reflux has started when liquid begins to drip into the flask from the condenser.

10. The vapors passing into the condenser will then form a "reflux ring" of condensate that should be clearly visible. Below this point, solvent will be seen flowing back into the flask; above it, the condenser should be dry. If the reflux ring rises more than halfway up the condenser, the heating rate should be reduced to prevent the escape of solvent vapors.

11. At the end of the reaction period, turn off the heat source and remove it from contact with the flask. Let the apparatus cool, then turn off the condenser water, and pour the reactants into a suitable container.

Simple Relux Assembly

 

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Almost Everyone's Guide to Science - Science isn't for everyone, but if you have even the faintest trace of curiosity about the world around you, Almost Everyone's Guide to Science will be a delight. Subjects for this latest project reaches new territory, expanding in breadth to cover not just physics but chemistry, geology, meteorology, and the life sciences as well.
Make Aspirin - Now that you can reflux, why not make some aspirin.
 
 

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