Spread a layer of 250 mg of finely powdered KClO3 over the bottom of a 10 ml Erlenmeyer flask equipped with a magnetic stirring bar. Add a layer of 500 mg of powdered iodine over the first layer, then add 0.250 ml of water to the flask. Set the flask atop a magentic stirring hot plate and commence stirring.
Insert a thermometer into the flask; the temperature of the reaction must be maintained below 40 C by cooling it in a water bath if necessary. Slowly add 1 ml of cencentrated HCl dropwise over a 30 minute period. The purple iodine should disappear and an orange solution form. Near the end of the stirring period, yellow crystals of product appear.
Cool the solution using an ice-water bath. Collect the crude ICl3 product under suction using a fritted glass filter. Recrystallize by dissolving in a minimal amount of hot ethanol, and colling slowly to room temperature, and then in ice. Dry crystals on a clay tile. The product is air-stable for short periods (up to about an hour)
Experiment from Microscale Inorganic Chemistry, Szafran, Z.; Pike, R. M.; Singh, M.M. John Wiley and Sons, Inc.: New York, 1991.
© 2004 by Lawrence T. Sein. All rights reserved.
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