Week 6: Crystallization of Complex

Last week, I mentioned my attempts to synthesize a pure product from my coordination reaction.  This week, I toyed with many different solvents in order to find the perfect combination for crystallization via slow diffusion.  This technique works by dissolving the product of a reaction in a certain solvent, and then slowly adding a second solvent on top of it.  The two solvents must be miscible, but the second solvent must not dissolve the complex.  When the two progressively mix together, the product then crashes out in a crystal formation.  This week was used to find solvents that did not dissolve my complex.  The two that do not are pentanes and hexanes. I then needed to test the different solvents with pentanes and hexanes.  After much trial and error, I tried an acetone/pentanes and acetone/hexanes mix.  I am hoping to discover crystals in my vial when I go in for my last week supported by the Charles Center.

Other than crystallizations, I also started to do quenching experiments with the original, published electrocatalyst mentioned in my first blog post.  The experiments are carried out by a fluorimeter, which measures the intensity of light that passes through a sample.  I am performing catalyst concentration studies in a system including fluorescein, ethanol, water, and catalyst.  The quenching experiments will elucidate the quenching pathway that occurs in the system as well as the type of quenching (static or dynamic).  While these aspects of the catalyst has been measured before, I am currently verifying the replicability of the experiments involved. I will continue these experiments through next week.  Overall, I am seeing progress, however the fact that my complex has proven difficult to synthesize may put its standalone effectiveness as an electrocatalyst into jeopardy.