Blog #3: Exploration of Inorganic Chemistry Experiments

This third blog post features an update on the progress of my project investigating potential experiments for an Inorganic Chemistry laboratory. Since the last blog, a lot of progress has been made. Unfortunately, we have had many bumps in the road of this project but have continued to work around them and make progress. Revisiting the first experiment, the product results were inconclusive and required further testing to confirm the structure. In an effort to move forward, we pushed to our second experiment utilizing the specially-ordered resin and a solvent known as Perchloric Acid.

We had all of our materials ready for this ionic column exchange experiment and were preparing to run an initial test. In science and lab work, it is imperative to know and understand the kind of materials one is going to be working with. Prior to running anything, any risks that could potentially be involved during the course of an experiment should be made well aware to every person working with the materials. In doing our preparative research, we started picking up many warnings regarding the Perchloric Acid. As it would turn out, this material could prove to be highly explosive when it is dried out and can be very caustic to many materials. Upon seeing this, we decided to scrap the experiment in favor of safety. The material has since been properly disposed of.

Following this, we found an alternative experiment that uses the same concepts of the original column experiment with mostly similar materials, aside from the Perchloric Acid. We decided to run this shortly after. The defining concept of this experiment is that it uses a pressurized system of Nitrogen gas in order to push the eluting solvent through the column and resin. This pressure forces the column experiment to proceed at a significantly faster rate and allows each run to be completed quickly. We performed this experiment using regular compressed air instead of Nitrogen due to its ease of access in each of our laboratory rooms. We also looked at an alternative method which we originally felt might be easier to do for an entire lab class full of students. This method used a small syringe and plunger to mimic the column and pressurized system on a much smaller scale and without the use of a compressed air pump. Unfortunately, problems with the syringe resulted in failure of separation of the metals. The procedure could be further adjusted and implemented in to the teaching lab with some more work. Pictures of both the initial set up and the alternative procedure are below.

 

 

 

 

The most recent experiment we ran as part of this project, is a synthesis between a Cobalt metal and Saccharin molecules. The result that is formed by this demonstrates the unique structures of metal complexes. The experimental procedure here is simple and easy to follow. The reagents involved are all typically non hazardous. The product that was formed through this experiment was then analyzed by ultra-violet visible spectroscopy and confirmed the structure of the product as a successful synthesis. This experiment could be directly implemented in the lab almost as is. A picture of the beautiful crystals that were recovered from this experiment are below.

Recently, Professor Upmacis and I attended the Society of Fellows 2017 meeting at Pace to display the work we’ve accomplished so far. Understanding this post was on the longer side, but it ultimately covered each aspect of the new work my professor and I have completed since the last blog update. Future work includes looking at another experiment to synthesize a metal-quinoline complex utilizing different common transition metals. As an additional note, this project has really been an eye-opening experience for me. It’s demonstrated that it’s a rare occurrence where everything goes perfectly and it’s more likely that something will fail or not work properly. The real world of working on new experiments and researching new procedures or creating a new methods is often full of issues that need to be worked around. A creative head is necessary to succeed and solve various problems!

Thank you for reading this long post!

Blog #2 – Exploration of Inorganic Chemistry Experiments

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.

20161018_154053-2The 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.

Blog #1 – Exploration of Inorganic Chemistry Experiments

I am Tyler Brescia and I am working on an Undergraduate Research Project with Dr. Upmacis in Inorganic Chemistry. The goal of our project is to work through and discover more experiments that can be used in a teaching-laboratory setting. As it stands, the current Inorganic Chemistry lab course includes both computational sections as well as “wet lab” work sections. In performing research on different types of experiments, we will be able to hopefully expand the wet lab work and offer a diverse set of tests that will help to teach and reinforce concepts from the classroom. We will be exploring different experiments, testing different procedures for each one, and evaluating the results, difficulty, and safety of the experiment to determine if it is suitable for use in a teaching-lab.

I’m hoping that through performing this research on different experiments, I will be able to hone my skills in a laboratory settings as well as to further deepen my own knowledge of both Inorganic Chemistry and the research process. Research has begun on our first experiment in synthesizing an oxygen-carrying Cobalt complex. The first step, creating a ligand, H2Salen, used as a precursor for the Cobalt complex has been produced. A picture is included. The next step is to test the sample to confirm and then continue with the next steps of the experiment.20161011_175200