I encountered this phenomenon firsthand when trying to purify picric acid via recrystallization from hot 95% ethanol. There was a distinct smell of
trace NO2, and a milky blob resembling crude nitroglycerin formed and sank to the bottom. I obviously don't have a NMR available at my place of
residence, but would I be correct in assuming that this was ethyl nitrate? I thank Schrodinger that I had not used methanol. I used a very long
plastic pipette to gingerly remove the blob and dilute it with acetone before burning it outside.
Has anyone else had unfortunate encounters with this phenomenon? What steps should be taken to minimize it? And what ratio of 2,4 to 2,6 TNP is likely
in solution? |