yes the new gakks are here as well, and swim doesent want to see his fellow bees waste pills, i have not tryed this procedure yet and am unsure if it works with the new gaks, but since so many bees have been asking swim by pm, how to work these particular things swim thought he would post it for all. thanx to 12chemman12 and lsd for this
Yep, 6 hour, 12 hour and day night.
All pills virtually work as they are amines and steam distill.
swim has a long necked, round bottom 500 ml flask. swim has several rubber table leg stoppers that slip over the top of flask. Single hole - for reflux , Dual hole - for steam distillation. Steam is generated by cappacino coffee machine that has been modified.
For steam distillation, a splash head is fitted into rubber stopper and steam is fed through a glass tube that fits the other hole. The steam must exit below the surface. Add pills and equal weight of caustic to flask, fit 2 holed rubber stopper, add water (never fill flask over half way point), fit splash head and condensor, heat flask with a flame 'til boiling then inject steam. Upon sitting, if sufficient quantity of pseudo is used, Pseudoephedrine Freebase crystals shall be seen to appear.
When steam distilling is done, ph the distillate to below neutral with hydrochloric acid and evaporate. swim uses plenty exess of hydrochloric acid, swim would rather put up with the smell of the excess hcl leaving at the end and know that I used enough hcl to convert all the freebase to the hcl salt.
If you clean the pseudo prior to steam distillation, the better it distills. 10 packs of dXXXXzin gave me about 10 grams of pseudo yesterday. Not bad seeing my steam hose died and had to stop short. No solvents, easily done. Don't just ph to 7 and evaporate, use excess hcl to make sure all is convertyed to the hcl salt, very important.
Then fit single hole stopper, add pseudo, red, I and condensor. I do dry reaction then when done I add more red, I and reflux for 3 or 4 hours more. When done add caustic, fit 2 hole rubber stopper, fit splash head and condensor and steam distill product.
A lovely smell will occur as the oil distills. When done "carefully" ph to 6.9 and evapoarate. You can then wash with cold acetone and recrystallise in alcohol if you wish or just have as is.
Metho substitutes for alcohol quite well!
Steam distillation, when forced, by heating flask to boiling then injecting steam works well. Wish I had known about it before,
This is what swim and another bee understands...
1 - Take a flask with two holes ontop.
I use a flask with a rubber table leg stopper attached
to it.
It has 2 holes, 1 small and 1 large.
The large one is for the Splash head.
The small one is for a pipe that delivers steam to
below the surface
of the liquid.
Another table leg stopper with 1 large hole is used for
reflux.(but that's another story).
By using the rubber table leg stoppers it doesn't
matter what ground joint
size you use that's all.
2 - Add pill mass and equal amount of NaoH.
Correct
3 - Add water (how much water, enough for it to all
dissolve?)
Not much, enough to make it liquid though, remember the
steam will add more water.
You can even start off dry,letting the steam add the
water to the mix.
"Don't fill fask more than 1 Third full".
4 - Then bring to a boil (does it matter how hot it is or
100C should be alright?)
Heat flask 'til boiling. Just boiling, easy.
5 - Then through one of the holes insert a pipe that goes
below the water level and send in the steam.
Pipe must be fitted before you start, really, think
about it.
6 - Then out the other hole comes the water that is evaping
and it should be collected.
Sort of, steam passes down the pipe in the small hole
in the stopper.
(bubbles) through the basic liquid, rising up through
the large hole on which a splash head and condenser has
been fitted.
7 - Once all the water has moved over, Take the water that
has been distilled and bring it down to a PH of say 6
and evap for crystals.
Bring the PH very low, like 1or 2 then evaporate.Don't
breathe fumes at end of evaporation as they are the
excess hcl boiling off.