The Purification of Poisoned Excedrin

Introduction
As a budding organic chemist you are faced with a very common problem: a drug you need has been poisoned with an unwanted organic compound. The drug you need is Excedrin (a mixture of caffeine, acetaminophen, and aspirin), and it has been poisoned with 1,4-dimethoxybenzene. You will work in a team of two or three students. Your team's task is separate the four compounds from each other and then characterize them to find out how successful your separation was.

Theory
Read the brief section on "Chromatography: Purifying Organic Compounds" in your McMurry text on pp 431-432. View the chromatography animation on the College of Wooster chemistry website.

Pre-Lab
Your team must come up with a written strategy (showing all of the structures of the molecules) which outlines how you will be separating the mixture, characterizing the separated compounds, and determining how well your separation worked. Construct a flow chart similar to the one from the Acid-Base Extraction experiment. You only need to turn in one strategy and flow chart per team. In order to assist you, the following chemicals will be available in the lab:

pure caffeine, acetaminophen, aspirin, and 1,4-dimethoxybenzene
hexane, ether, dichloromethane, acetone, methanol, water, 3M NaOH, 3M HCl

You should probably discuss your strategy with your instructor before coming to lab. You will turn in your strategy and flow chart before lab begins (make two copies so that you have one to look at in lab).

Experimental Procedure
You will get a vial that contains 1 gram each of all four compounds. The separation procedures for each team will probably be different. Your team must be flexible: don't stick to a plan if it looks like things are not working. You will have two weeks to complete this experiment.

Results and Discussion

  1. Include all drawings of TLC plates (please don't turn in the plates).
  2. Calculate the percent recovery of all four components.
  3. Comment on the purity of each recovered component. Be sure to include a discussion of all the data you obtained for each component.
  4. Provide a written procedure of what you did in the lab (not your original strategy). How did your strategy change throughout the course of the experiment? How could the separation and characterization be improved?