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Using a clean stirring rod, place a crystal of salicylic acid into the first test tube. To each test tube add 1 drop of iron(III) chloride) solution.
SAFETY CONSIDERATIONS Wear goggles throughout this experiment.
This experiment uses salicylic acid, acetic anhydride and phosphoric acid.
After the reaction takes place, water is added to destroy the excess acetic anhydride and cause the product to crystallize.
The aspirin is then collected, purified by recrystallization, and its melting temperature measured.
If you spill some, wipe it up with a wet paper towel and throw the towel in the trash.
The acetic anhydride and sulfuric acid can cause bad burns.
If you spill a lot of either of these, notify your instructor.). Using the graduated cylinder located under the hood, measure out 7.00 m L of acetic anhydride and add this to the flask.
Transfer this to a 125 m L Erlenmeyer flask using a powder funnel. Be sure to do this in the hood and wearing your goggles.
If the crystals do not all dissolve, add 2 m L more of the ethanol and continue to warm the mixture to dissolve the crystals. When the crystals are all dissolved, add 10 m L of deionized water, cover the beaker with a watch glass, and allow the solution to cool slowly on the lab bench undisturbed for about 10 minutes. After the 10 minutes cooling on the lab bench, complete the crystallization by placing the beaker and contents in the ice bath. If crystals do not appear, you can scratch the bottom of the beaker with a stirring rod to induce crystallization. Using a clean circle of filter paper, collect the purified aspirin by suction filtration as before. Dry the crystals by pulling air through them for about 15 minutes.
(Discard the filtrate left in the filter flask into the waste container under the hood.