Author Topic: oiling out of salt during gassing  (Read 2712 times)

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wacko_reaco

  • Guest
oiling out of salt during gassing
« on: September 09, 2002, 12:59:00 PM »
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???
ta

wacka wacka wacka

Rhodium

  • Guest
Yes, an acid/base extraction followed by drying ...
« Reply #1 on: September 09, 2002, 01:03:00 PM »
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.

wacko_reaco

  • Guest
water
« Reply #2 on: September 10, 2002, 12:11:00 AM »
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.
cheers
ps  does the gassing rate affect things?

wacka wacka wacka

baalchemist

  • Guest
You really need to install an inline gas-dryer ...
« Reply #3 on: September 11, 2002, 01:11:00 PM »
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...........

    GODISNOWHERE
Shoot Narcs, Not Drugs

cilliersb

  • Guest
A Whole Host
« Reply #4 on: September 12, 2002, 09:59:00 AM »
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!!