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We recently did a lab/demo using the NMR to observe Na ions in sodium complexes in our Inorganic Class. I understand most of the post lab questions, but there are a few that still have me stumped. Essentially what we did was create two samples: in one we added NaI to 18-crown-6 ether (with enough deuterated acetone to lock the signal) and in the other we just added NaI to deuterated acetone. 1M NaCl was used as a standard. The resulting peak of the Crown solutiion was shifted downfield approximately -17 ppm from the NaCl standard. The peak from the Na in pure acetone was only about -1.7 ppm down from the standard. My questions are as follows:
1) How would you make the Na-23 NMR peaks "sharper" for NaI/18-crown-6 ether samples?
2) Why did we acquire all spectra without rotationg the sample?
3) Why are Na-23 peaks shifted to lower ppm values when sodium is encapsulated by 18-crown-6 ether
4) How would our results change if a cryptand, such as [2,2,2]crypt was used instead of 18-crown-6 ether.
I was also wondering why sodium present in the glass NMR tube does not show up on the spectre? I realize it is in the solid phase but what effect does that have?
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