Experiment 5:

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Experiment 5

• COLUMN CHROMATOGRAPHIC PURIFICATION OF ANALGESICS
  

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Objectives

• To learn the separation technique of column
  chromatography.
• To separate aspirin from acetaminophen in Goodys
  Body Pain powders using this technique.
• To analyze the purity of the isolated active
  ingredients using TLC and HPLC.

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COLUMN CHROMATOGRAPHY
Polar components (b) adsorb more strongly to the
polar silica gel and elute after the less polar
components, which move more quickly with the
non-polar (relative to silica gel) solvent.
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COLUMN CHROMATOGRAPHYGeneral Procedure

• Prepare column
• Load column
• Develop column
• Collect fractions
• Analyze fractions

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EXPERIMENTAL PROCEDURE HPLC Analysis

• Place a small amount of crystals of each purified
  sample into a small autoanalyzer vial. Add 1 mL
  of HPLC solvent.
• Place sample vial into vial slot in sample tray
  and sign out on vial slot sheet.

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SAFETY CONCERNS

• Ethyl acetate and hexane are flammable. Never
  use these solvents around an open flame or hot
  hot plate.

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WASTE MANAGEMENT

• Place all organic solvent waste into container
  marked, Organic Waste (Column).
• Place used TLC capillaries in the broken glass
  container.
• Ask instructor to demonstrate method for
  evacuating SiO2 gel from column. Clean column
  with soap and water, followed by a rinse of wash
  acetone, and suspend inverted from ring stand in
  hood.