I am trying to decompose rare earth acetate in oleic acid/octadence/oleyamine. Previous publications suggest that the end product is a white precipitation, but I keep getting a black gel like product. Someone told me that it could be pyrolysis of oleic acid or octadence.
Have you tried purging out the reaction flask with either nitrogen or argon first? I've made nanocrystals (CdSe) with those solvents up to 320 C and have not had a problem with the solvents decomposing as long as you purge the system of oxygen. For a 250 mL flask I would purge for 10-15 mins, then begin to heat the flask and continue to purge until you reach about 120 C, then remove the purge needle (I use a 12 gauge needle). Hope this helps, good luck.
Have you tried purging out the reaction flask with either nitrogen or argon first? I've made nanocrystals (CdSe) with those solvents up to 320 C and have not had a problem with the solvents decomposing as long as you purge the system of oxygen. For a 250 mL flask I would purge for 10-15 mins, then begin to heat the flask and continue to purge until you reach about 120 C, then remove the purge needle (I use a 12 gauge needle). Hope this helps, good luck.
I agree with Albert absolutely. I've used same procedure with the synthesis of rare-earth oxides nanoparticles. Start purge argon through the solution at room temperature and continue during heating up to the temperature then vapours of oleylamine/octadecene/whatever are dense enough to not let air inside the reaction vessel. I usually stop argon flow at 150C.
Again, I'm going to have to agree with Alexander and Albert. Further, I usually pull vacuum at room temperature and backfill with argon or nitrogen three times before I begin my continuous purge for the reaction.
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