Author Topic: ozy 6 hour/12 hour steam distill (old)cure  (Read 8037 times)

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honey_badger

  • Guest
ozy 6 hour/12 hour steam distill (old)cure
« on: August 09, 2004, 03:31:00 AM »
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.


TheHitMan

  • Guest
I stopped reading after the 6'th line.
« Reply #1 on: August 09, 2004, 04:19:00 AM »
I stopped reading after the 6'th line. Learn how to use a paragraph!

abominator

  • Guest
Good work Jemma
« Reply #2 on: August 09, 2004, 03:13:00 PM »
So, the new gakk has hit OZ?  Yellow oil?  The yellow oil is the indicator, other US bees have been working on distilling as well, like Prepuce.  Swim has not, however read an approach like yours, but it sounds like a winner


honey_badger

  • Guest
emperical findings
« Reply #3 on: August 10, 2004, 05:43:00 AM »
hailz man,

ok so who can try this out on the new oz pills?
if this is a working alternative to the koh boils swim would like to know, swim cant hook a set up like this up at the moment, (living quarters)

can some bee do an illistration to thE set up DESCRIBED


PWEEEEEEEZ  :)


12cheman12

  • Guest
Well ive been reading alot of voguls 3rd ...
« Reply #4 on: August 10, 2004, 10:30:00 AM »
Well ive been reading alot of voguls 3rd edition, great stuff in there. Explains all about it. Get it over at rhodiums site.
All you pretty much do is setup your normaly distilling apparatus but the containter that holds what is to be distilled has a tube running to the bottom which introduces the steam. The steam changes something about the pressure (i think) and therfore the substance will distill over at a much lower temp then it normally will.

Read through vogel and theirs heaps of diagrams.


p2e3r4f5e6c7t8

  • Guest
Something like this ehh
« Reply #5 on: August 10, 2004, 05:36:00 PM »
Have a look at these

https://www.thevespiary.org/rhodium/Rhodium/chemistry/equipment/distillation4dummies.html#


There's a few methods in this exelent piece information, Check out the pick's on external steam distillation.


UncleFester

  • Guest
I hope it works...
« Reply #6 on: August 11, 2004, 12:37:00 AM »
I tried an experiment very similar to this one on back on the "Problems Gassing Generic 60's" thread. I was very hopeful for steam cleaning out these polymers, so much so that I put it in SOMM 6 before the release of these pills in anticipation of their arrival. In my experiment on that thread I tried sudafed pills in a VERY hot oil bath driven steam distillation. The sudo yield on the other end wan't high enough to make the sudo precipitate out of water like it should, being the water insoluble(sort of)creature that it is.
I did get burned sudo from heat frying the sudo mixed with NaOH, and the gak still sitting there, turned to a funny plastic. Upon extraction with toluene of the distillate, there wasn't much product there. This distillation by no means went on for 6 or 12 hours, but I could see where I was going. Extraction with np is the way to go, considering the volume of steam distillate, and I don't think it works with sudo, no matter how hard you try...short of making it an actual vacuum distillation at high torr. I put 4 pages in SOMM 6 with Ghetto Steam devices and procedures, but I an convinced that you can only get this process to work with ephedra and ephedrine. Good luck with your experiments.

callen

  • Guest
Steam dist. of an aq. alkaline Sudo solution
« Reply #7 on: August 11, 2004, 05:22:00 AM »
A.L.F. sez,"If I recall correctly...use a pressure cooker that has been modified to provide a jet of high pressure,super heated steam to the extraction vessel.
Steam extract meth at 100*C., ephedrine at 110* to 125*...no burnt freebase there...so what's the problem with Sudo?... None...You can get 150*C. from a pressure cooker...no problem...high enough to make P2P and methyl amine from ephedrine...to make meth from,(the old fashioned way).
BUT FIRST...you must do this...!
Powder your pills, soak overnight, or boil for 15-minutes in
gum turpentine,filter and dry the filter cake;soak filter cake in di-chloro-methylene over night or boil for 15-minutes...filter and dry the filter cake; soak the filter cake with denatured alcohol(Etoh) that has been in the freezer for about 30-minutes to an hour. The alcohol extracts the sudo from the little remaining G.A.K.K's.that are left from the previous solvent soaks.Filter out the undissolved G.A.K.K.s.Evaporate the alcohol from the filtrate and end up with very nice pinwheels of Sudo Hcl."
A.L.F. sez that it will perform the procedure again and report it's findngs...since his initial experiments were done so long ago...and will post the results at the Hive. :)


Synergetic

  • Guest
Title is misleading...
« Reply #8 on: August 11, 2004, 08:17:00 AM »
Swim already mentioned in another thread that steam distillation works on most australian pills.
Nearly every single variety of slow release formulations fall victim to the steam, as do many other formulations.
You might want to set the record straight with your title.
People may think you mean to distill for 6-12hrs...
It looks like Uncle Fester already did, shame on you Badger!


ozmosis

  • Guest
I stopped reading after the 6'th line.
« Reply #9 on: August 11, 2004, 09:03:00 AM »
well hitman i guess you have your own foolproof method for beating this new monster?
If not, then i suggest you read past the sixth line, or f#@% off until you have something constructive to add.
The badger is a mate of mine and he is only doing his best to help out fellow oz bee's(well done son).
As for these pills, the der,der, you know what-azin, swio has just wasted 120 boxes of the fuckers (12hr that is) only to find out that this new nastie has finally hit our shores.
So swio's monkeys go out for  the 6hr variety, only to discover that they have now been re-located behind the counter and are reddily available when you produce ur drivers licence.
So we can basically forget them until we come up with a cure.
Swio has access to KOH LR and AR and will give uncles method a go go when a simplified, lamens terms procedure has been written up.
The monkeys have managed to aquire 20 boxes of said 6hrs and i hear that swio is about to go to town on them....
results soon!!!

Synergetic

  • Guest
Tsk tsk, easy tiger!
« Reply #10 on: August 11, 2004, 11:44:00 AM »
Well arent you fuckin stupid for trying to extract 120 boxes without trying ONE box first!
I hope you learnt a valuable lesson, son  :P


thinkpol

  • Guest
New GAKK
« Reply #11 on: August 11, 2004, 12:43:00 PM »
Has it finally arrived down under??

SWIM is unsure, if it is across the board or just 12 hour boxes.. Any thoughts


ozmosis

  • Guest
Tsk tsk, easy tiger!
« Reply #12 on: August 11, 2004, 02:48:00 PM »
listen tosser, >:(  120 boxes is what i knock up every ftriggin week.  i have never had a problem with them until last week, lucky i'm cashed up though.
Must bee due to the fact that out of a hundred and twenty boxes (12hr sulfate), i get ~ 130 grams of dynamite birch-honey. So to drop 120 boxes is only a drop in the ocean.
But alas! i have just  extracted ~20grams of super clean freebase xtals from my 20 boxes of 6hrs. Sweeeeeet! :)
12chem, badger, method is on it's way via pm tomoz! aswell as the used by dates to watch out for. 8)

honey_badger

  • Guest
12-6 hour
« Reply #13 on: August 12, 2004, 02:43:00 AM »
great work maniacs,

and now ozy's would know that 6 hour and 12 hour mean a different thing,and not distilation!! (my bad)

to the mericano's 12 hour and 6 hour means the spacific pills, not distialtion time. lol ozmosis  8)

swim is waiting for some emperical results, and will post the procdure and pics if it all works out, let us know what happens please mate (ozmosis)

never fear ozy's, the right maniacs are onto it.


lsd

  • Guest
Aussie Pills
« Reply #14 on: October 20, 2004, 04:08:00 AM »
For the last three weeks I have had problems with reactions and after checking everything through, I conclude that the new gakks are now here.This time am going to clean pills prior to distillation. Shall let you know how I go.


Martian_A

  • Guest
Booyah
« Reply #15 on: October 22, 2004, 07:50:00 PM »
I had yanks tellin me I was practically a goose because the gakked square red packs were so called been in australia for "years". Funny that, a year ago, a simple metho/dh20/acetone extraction and purification was all that was needed... reaction fine, crystalisation perfect.

NOW! Extractions seem to work although when it gets to modifying the pH after the reaction... What happens? Oh Great! Cheddar Cheese AND ITS GREEN! .... Go the NEW PEGS!

Now what do we do? w00p, looks like im down to Straight to E! Bonus! More screwin around! Lower Yields! Lets do over W****rL*****t!

- Martian_A