T minus 16 days until defense

Published April 9, 2012 by PinkEnergizerBunny

Had an experimental disaster that brought me close to tears/explosion/anger this afternoon, but I held back. Waterproof mascara is ideal for those for low-threshold lacrimal ducts 😉

In short: the experiment I had outsourced a while back (~3wks ago) I finally got back, approx 3 mg of purified material dissolved in a mixture of methanol and water. All I had to do was remove the solvent and take the NMR of the sample. After drying the samples, I saw NOTHING (other than solvent peaks) in my NMR spectrum. Read: BAD NEWS BEARS. I dried the sample further, ran the NMR experiment longer, combined with the dilute fraction, repeated ….several times. STILL NOTHING.

here is what the old me would have done: screamed, cried and wasted time online being useless, maybe even left. It is T minus 3 days, actually 2, before I have to give my dissertation to my committee after all…

here is what the “new” me did: took a walk outside to cool down, wrote an email to the mass spec administrator who gave me the sample so that hopefully we can resolve this puzzle tomorrow, and worked on a few other tasks in lab.

I collected myself. wow 🙂 I think I am growing up (as a scientist) …good timing! 😉

Review of my day otherwise:

  1. Write experimental info on compound 2 wrote about the experiment; compuledwill include NMR data later when it’s done
  2. MD-50-8 column established a solvent system and set it up for tomorrow morning
  3. Dry MD-23 samples wish I could have something to show for it!
  4. 1H NMR on MD-23 samples  hahhahahahahahhahahahhahahahaa
  5. 13C NMR on MD-23 samples
  6. Make points needed to be covered for powerpoint presentation
  7. While column is running: go through old blog posts to make sure I did not miss anything

I also worked up one reaction I had “laying around”, aka Heck variation 7, printed out “study materials,” and filled up solvent containers for tomorrow’s column. Now that I look at my list, I am 😦 that so little got done, but at the same time dealing with MD-23 samples took so many HOURS that there was no time to do much of anything else really! In the end, I am 😀 I was able to pull myself together!

Night! -.-

_______________________________________________________________________________________________________

Plan for Tuesday, April 11th:

  1. MD-50-8 column
  2. While column is running: go through old blog posts to make sure I did not miss anything
  3. Dry MD-23 sample 4
  4. Talk to mass spec administrator
  5. talk to reader 2
  6. 1H NMR on MD-23 sample 4
  7. 13C NMR on MD-23 sample 4
  8. Make points needed to be covered for powerpoint presentation
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