Disposable stirbar’s geezmiester based inspiration on improved freebase titration, azeotropic toluene water distillation and anhydrous crystal formation deliberation and optimization thread
AKA
Crystals for dummies
AKA
Dean Stark-ing for dollars
AKA
Do these gassing pants make me look fat?
AKA
Crystals for dummies
AKA
Dean Stark-ing for dollars
AKA
Do these gassing pants make me look fat?
C(r)ooks instructions:
Add concentrated HCl to freebase with stirring until pH = or <3. Take your time. This gets hot. If pH paper or meter impaired just add until color changes and doesn’t change back then add a dash more.
Add at least 9x that volume of toluene.
Distill off toluene and water until the still head temp is that of pure toluene or just boil until the flask clears then remove from heat. Decant into another vessel to facilitate crystal removal if you want.
Filter beautiful crystals after cooling.
Big kid’s department:
This method really is as easy as it reads. The only thing to keep in mind is that you need a lot of toluene because first you need it to azeotropically distill off the water(80:20) and second you need a sufficient volume to keep your crystals swimming after formation so you can recover them with sufficient solvent to hold impurities. With gassing one can stop when needed to filter and/or add solvent. With this it all comes at once so you better have enough. If you make a puck it will trap what you don't want.
Even with more sensitive freebase, one could add dilute HCl till the proper pH or without equipment add dilute HCl to freebase until you only have one layer plus a dash more then distill from there, possibly needing to sep funnel your distillate and add your toluene back to the pot to get all the water.
This can also be run under vacuum if lower temps are needed.
This whole tech could be run without a single thermometer, test strip or piece of glass if you were paying attention to visual clues. Disposable stirbar loves the lazy man's way, especially when it is the right way.
Unpleasant gassing rigs are now a thing of the past.
Someone take a swing at this and see. Super low effort home run every time.
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