This blog post features an update on my project that delves into Inorganic Chemistry experiments and their usability in a teaching-laboratory environment. Progress has been made on the first experiment we worked with, as mentioned in the first blog post. The experiment focused on the synthesis and activation of a Cobalt-carrying complex through the use of traditional reaction methods and reflux apparatus. This experiment was performed with initial reaction conditions differing from those outlined in a normal procedure.
The full procedure included the use of inert nitrogen gas in order to keep the reaction conditions anaerobic, or without oxygen. The oxygen is used at a later point to activate the molecule. The reaction conditions are kept anaerobic through the use of constant flushing with nitrogen. The use of nitrogen, although available, would cause difficulty when used in the experiment in the teaching-lab with students. Since this part was deemed difficult to handle, the initial reaction was performed without a nitrogen-flushed environment. This served as first test, rough-run. Analyzing the product formed from using a procedure without nitrogen would help to determine whether nitrogen reaction conditions would be truly necessary.
The experiment was performed and product was recovered. The characteristics of the product differed from the intended product’s description, so it immediately seems that nitrogen and a lack of it, would possibly play a significant role in product formation. Following this, Infrared spectra and Ultra-Violet/Visible spectra were taken from both the intermediate material and the product. At this point, the spectra from both instruments has not been analyzed, so the full chemical compositions of the intermediate and final product have not been confirmed. The picture below is an example of the modified reflux apparatus used to synthesize the final product. If nitrogen conditions were kept, the picture would show a balloon at the top of the tower filled with nitrogen, in order to preserve pressure and keep conditions anaerobic.
The following experiment that will be tested is a column separation of ion complexes through the use of differing concentrations and a column filled with an ion exchange resin. With the arrival of the necessary special-order resin, this experimental procedure will be tested and altered in the coming few weeks.