wacko_reaco (Hive Bee)
09-09-02 12:59
No 354568
      oiling out of salt during gassing  Bookmark   

This has never happened before, the gassing was going fine, then I took the rod out for a look and the crystals had turned to goop. It was my fault really as the toluene was quite warm and I was gassing way too quickly as I was in a hurry. Anyway, remedy, would that just be to dump some 5%HCl solution in, then freebase again, dry, and re-gas, albeit  more slowly. Is the salt stable under these acidic conditions (that is such a stupid question but I don't really want to waste this so I will ask anyway)
Anyone had this happened before, or will the oil eventually crystallise???

wacka wacka wacka
(Chief Bee)
09-09-02 13:03
No 354569
      Yes, an acid/base extraction followed by drying ...  Bookmark   

Yes, an acid/base extraction followed by drying your non-polar solution will allow you another try with the gassing. The most probable reason for your failure is that your freebase was dirty and not vacuum distilled, as well as presence of moisture. That makes it so much easier for the amine hydrochloride to oil out into a mess.
(Hive Bee)
09-10-02 00:11
No 354693
      water  Bookmark   

the freebase was vac distilled, but for the first time I used a polyethylene tank to gas, in the past I used glass, then stainless, both of which one can flame dry. I thought the poly tank would be ok b/c the surface to volume ratio is getting quite large so the water adsorbed would be proportionately lower than with smaller tanks. I might try to wipe it out with acetone with a mag sulpate suspension before introducing the dries tol/freebase solution.
ps  does the gassing rate affect things?

wacka wacka wacka
(Chef d'Equippe)
09-11-02 13:11
No 355283
      You really need to install an inline gas-dryer ...  Bookmark   

You really need to install an inline gas-dryer device filled with fresh dri-rite somewhere in that set-up. Then you'll never have that moisture problem...........

Shoot Narcs, Not Drugs
(Hive Bee)
09-12-02 09:59
No 355566
      A Whole Host  Bookmark   

There are a whole host of drying agents that swim has tried in-line during gassing.

Neither MgSO4 nor CaCl2 gave good results, but bubbling the HCL through a 100ml bottle filled with Conc. H2SO4 does the trick time and again.

This has been swims experience with all the Amphetamines I've cryst. H2SO4 is dirt cheap and for around $1.50 I can fill my drying bottle with 80ml LG H2SO4. Hell, all you need is NaCl and H2SO4 to begin with. Keep it simple beez!!