User:Mary Mendoza/Notebook/CHEM 581: Experimental Chemistry I/2014/10/24

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Column Chromatography for BPA Concentration

  • The column used was a 30 cc plastic syringe. The first layer was filled with glass wool fiber and fine sand. The sand was ground by Dr. Hartings using mortar and pestle.
  • 9.9999 g of BDH Silica Gel 60 Angstroms High Purity 40-63 μm was mixed with approximately 30 mL of methanol.
BDH Silica Gel 60 Angstroms High Purity 40-63 μm
  • First, the column was washed with water. Afterwards, the silica-methanol mixture was slowly poured to leave the sand layer undisturbed.
  • After some of the solvent front, methanol, passed, the column was washed with water again. Air pressure was applied to compact the column.
  • Another water wash was performed.
  • Once the column was ready, 10 mL BPA sample was poured into the column; solvent of the BPA was drained through the column.
  • When most of the sample solvent has been drained, 10 mL of water was added into the column.
  • 2 fractions of the 10 mL water and 6, 5 mL fractions of the 30 mL methanol were collected. Each fraction was dotted onto a thin layer chromatography (TLC) paper.
  • After dotting the TLC paper, there were no observed changes. Hence, Dr. Hartings dissolved FeCl3 in methanol. FeCl3 is expected to form a blue compound once added to phenolic compounds. However, no change was observed even with the addition of FeCl3.
  • The experiment was terminated.
  • No change observed could have been that the 10 ppm BPA is too dilute of a concentration for the successful, efficacy of the TLC method.