To Osmium :
I have one 125 ml sep funnel, I have someone at a glassblowing store to adapt a 24/20 joint, so I could easily make a H2SO4/HCl gas generator. I have tried to gas it, the generator worked fine, plenty of HCl gas but no crystals. I have the folowing explanations :
1) I did not use a drying stage in the HCl generator, also I used 93% H2SO4.
2) The free base had lots of brown contaminants.
3) I used a just a bit of freebase in about 200 ml toluene when I tried it, maybe I needed also greater concentration. Can someone please give a good ratio ?
4) Your inputs are welcome.
I plan later on to distill the freebase, to add the drying stage in the HCl generator and to be more careful with H20,I hope then the crystals will show up.
By the way, I have a small problem pending with the freebase distillation, I plan another post just on this one later on.
Also, I think partial success on my second try is OK, I had by far more crashes when learning to grow mushrooms. Right now if I can fix the free base distillation I thing the remaining problems are more or less easy to fix.