MICROSCALE

LABORATORY TECHNIQUES
Gilbert, J. C., Martin, S. F., Experimental Organic Chemistry, A Miniscale and Microscale Approach, 5th ed, p. 107-108 and 161-162.
OBJECTIVES This experiment introduces separation and purification methods widely used in medicine as well as in industry. The methods are recrystallization and extraction.
BACKGROUND Please read the theory on pages 904-101 and 153161. EXPERIMENTAL DETAILS 1. ACETANILIDE RECRYSTALLIZATION. Dissolution. Weigh out 100 mg of acetanilide and place it into a test tube. You will be provided with a metal plate that will go on the hot plate. Add 1 ml of water (regular tap water) to the test tube and put it on the metal plate touching the hot plate. Secure the test tube by clamping it and set the thermostat to high. The water must be boiling in order for the solid to dissolve. Set a small beaker of water alongside on your hot plate in case you need to add some water to increase the solubility. In order to prevent bumping, stir the mixture with a glass rod or add one or two boiling chips. When all of the solid is dissolved an oil layer might form. Continue adding hot water (portions of 3-5 drops using Pasteur pipet) until the oil disappears. Hot Vacuum Filtration and Crystallization. Set up the apparatus as shown in Figure 1. Use a Pasteur pipet to transfer some hot water from your small beaker on to the filter paper in the Bchner funnel. Pour the mixture (while hot, use test tube clamp) through the Bchner funnel. You might see crystals forming in the filter flask. Let the filtrate cool to room temperature and place it on ice for 5 minutes. In the meantime set up the apparatus again (make sure everything is clean) and collect the crystals on the Bchner funnel by vacuum filtration. Wash the crystals on the filter paper with two small portions (2x full Pasteur pipets) of cold water. Scrape the crystals onto a watchglass. Analysis. Weigh the recovered crystals of acetanilide and calculate the percent recovery. Determine the melting point of the crude and the purified product. 2. ONE BASE EXTRACTION. Follow the procedure outlined on p. 162 (Part A) from the Gilbert & Martin Textbook. Comments: The textbook procedure will be closely followed for this experiment. Familiarize yourselves regarding use of separatory funnels, Hirsch and Bchner funnels, drying and filtration techniques found throughout the textbook-the information is quite good!
POST LAB For your lab report include a clearly detailed flow diagram (equations etc) for this part of lab exercise. Weigh both products. Calculate % weight recovery of both products based on your starting weight of the mixture. POST LAB QUESTIONS Do Post Lab Questions from G & M textbook p. 112 113, #24 & #26, and p. 168 169, questions #7 & #9.

Figure 1. Apparatus set-up for vacuum filtration.