Monday, December 30, 2013

Summer research

I was lucky enough to be accepted for a 10 week paid summer research in my school lab. I wasn't too excited, because I had spent 2 semesters doing research. The problem with the research during the school semesters was that I didn’t have enough time between reactions. Sometimes, I had to leave the lab right after I had isolated my product and came back 2 days later without knowing of my compound is still the same! So, I was very confident before starting my research this summer. I was sure that in 10 weeks I could do great things in the lab. Apparently, I was wrong.
I am working in a synthetic (bio)inorganic chemistry group and I have my own project. So, I make my own ligands, bind them to metals and so on(we all do the same by the way). First problem came by the first ligand. Since it is a known ligand, I can give the name: TACN (1,4,7-Triazacyclononane). I don’t want to go into detail, but no matter how hard I tried, I wasn’t able to make it. I’ve spent so much time reading papers describing the synthesis. I followed the same methods, modifies a little bit, did it under Argon etc. But, it didn’t work. By the way, I have found several papers with flawed data etc. If you look at the structure and synthesis, it doesn’t really look hard and I am sure for an organic chemist it is very easy. But, I’ve now learned that making macrocycles is extremely hard in some cases. So, we had to spend some money and buy the commercial one. I lost 5 weeks with this synthesis (or I’ve gained 5 weeks of experience).
After making my other ligand (which I can not name here), finally I started to do reactions with my new friend Iridium. Since I have been trying to make a new metal complex, I didn’t have procedure to follow. So, I brought in my own knowledge of organic and inorganic chemistry to work. I read papers on similar metal complexes of Rhodium. Because, one would expect that they should “behave” similar(they really don't). Of course, my mentor helped me a lot. But, most of the time he pushed me to decide on my own. So, for the first time I was in a position that I was afraid to make mistakes. Because, they were my OWN decisions and I felt responsible for them. I dealt with extremely insoluble intermediates and products. I had to find ways to characterize them and compare different spectra. Basically, the last 5 weeks went like this. Another big problem was the yields I was getting (usually 30-40%). So, I tried to maximize yields by changing the reaction conditions etc. Finally, my time was over and I couldn’t even reach half of my goals that I wrote in my proposal. I have gained a lot of experience and I will make us of them in the future. I have obtained more than 100 NMR spectra. So, I am very confident in NMR interpretation now. I have also helped my friends in other groups in finding their resonances. I kind of became the NMR guy.
In summary, now I know why a Ph.D. takes 4+ years. I now know a reaction that’s suppsed to go 3 hours can keep you busy for 3 days (isolating, characterizing etc.). I now know how hard chemistry is. I now know that NMR, IR, UV/Vis don't tell you anything unless you know how to read them and you are well aware of what you are looking for. I now know how frustrating it can be. I now know silver makes stains on your skin! And now once again I really know I want to be a chemist. Because, it is so exciting!

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