CHEM2411L Clayton State University Dr. Susan F. Hornbuckle EXPERIMENT #5 STEAM DISTILLATION PART A: ISOLATION OF THE ESSENTIAL OILS OF CLOVE Safety note: since steam is being generated, care should be taken to avoid spills and burns. Exposure to methylene chloride fumes should also be minimized. PROCEDURE: Place 10g of freshly ground spice (clove) in a 500-ml round-bottom flask, add 150ml of water and a boiling stone, and mark the water level with a grease pencil. Assemble the set-up as shown in the figure below. Use a stopper for the separatory funnel. CHEM2411L Clayton State University Dr. Susan F. Hornbuckle

Fill the dropping funnel with water, add a boiling stone, and heat the mixture until a steady distillation begins. Occasionally add water from the funnel to maintain the original level. Collect the distillate until no further droplets of oil can be seen; a minimum of 100ml should be distilled and collected. Pour the distillate into a separatory funnel, rinse the receiver with 10ml of methylene chloride, and add this to the funnel. Shake the funnel, allow the layers to separate completely, and drain the lower organic layer into a 25ml Erlenmeyer flask. Extract the aqueous layer again, using 5ml of methylene chloride, and drain the lower layer carefully into the flask. Add a small amount of sodium sulfate, swirl, and transfer the solution with a pipette and bulb through a cotton wad in a funnel into another tared flask. Evaporate the methylene chloride on a rotary evaporator until the solution has been concentrated to an oily residue. Weigh the oil and calculate the percent yield based on the weight of plant material.

PART B: GC/MS analysis of the mixture: Place one drop of the clove extract in a vial and dissolve in 1 mL of methanol. Label vial with your group name, date, and “clove oil”. Give labeled vial to your lab instructor for analysis.