Today, further Spinsight processing of our multiple quantum magic angle spinning (MQMAS) spectrum for the x = 0 (pure boron oxide) glass was in order: data-shifting, phasing, fast fourier-transforming and a row-adding macro gave us a presentable MQMAS spectrum with skylines above and to the side, the image of which I will have to add to this post at a later date.
Met with Diane to talk about what we have achieved so far this term and what we have left to get done, seeing as how it's week 5 already. We need to:
- NMR our newly-made cobalt glasses, as well as the borate crystals made by Steve Feller, plus further MQMAS experiments with our x = 40 and x = 20 (again) glasses.
- Complete our set of simultaneous thermal analysis (STA) data by running our x = 0, 5, 10, 15 and 33.33 glasses through the machine.
- Ask Ben to please run the Raman spectrometer with our new cobalt glasses, so again we can compare Raman and NMR spectra.
- Correct our interim reports so that we can use them as the basis for our final reports.
- Get to work on our final reports!
Spent the afternoon working on assigning structural units to our Raman spectra peaks, which proves tricky in one or two cases. May need to review some more literature, or go back to some we may have missed details in.
Still up in the air is the apparent problem with DMFit: it seems to warp our data in a systematic way by taking a start- and end-point for the wavenumber values and assuming all the data points inbetween are equidistant (the nature of the Raman spectrometry is that they're not equidistant). Which means, on plotting the spectra in DMFit, produces a deviation from the 'correct' data which looks like the below. The correction for peak positions is simple enough, but correcting the peak integrals (that is, area under the peaks) is tougher.
Click to enlarge