Author Topic: First gassing experience..  (Read 7594 times)

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8ball

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First gassing experience..
« on: February 28, 2004, 08:41:00 PM »

geezmeister

  • Guest
did you dry it ?
« Reply #1 on: February 28, 2004, 11:31:00 PM »
Did you dry the xylene before you gassed? You need to do that to remove any free water. I know xylene stays pretty dry, but if its the least bit cloudy it probably had enough small droplets of water in it to foul a gassing attempt. TCE is the only solvent I have used to pull pseudo or meth with that I could wash and gas without drying.

You might want to wash the xylene now with some water, collect it, and evap it to see if you have some pseudo there. If you do, you could titrate for what's left in the xylene. Its still there somewhere. Don't toss anything just yet.


8ball

  • Guest
Dry
« Reply #2 on: March 01, 2004, 04:23:00 PM »
Yeah Geez everything i have is dryed i bottle everything in 300ml bottles and put a little baked epsoms in each bottle so i can garantee its dry, i acidified the wash water and evapped this as well and no joy i cant work out whats gone wrong, i have not recovered anything at all not 1 gram.


geezmeister

  • Guest
One of two places
« Reply #3 on: March 01, 2004, 06:10:00 PM »
You either did not base enough to get the pseudo freebased and it is still in the pill mass, or it is in the rinse water, or both.

Go back to the pill mass. cover with xylene again. Add dry NaOH or sodium carbonate and mix well. You want the pill mass to turn brown or tan from yellow if you didn't get anything from the last basing effort. If that doesn't work for you, cover the pill mass with nonpolar and gently heat the pill mass with stirring until the nonpolar solvent is hot. Wash the solvent, dry over epsoms, and gas.

You may have your pseudo in the wash water. This is a rare situation. I really think you did not get the pseudo freebased, and it is likely still in the pill mass.


However, I have noted recently-- for the last six weeks or so-- there is a new gakk in some pills which seems to interfere with the a/b process. I have encountered this gakk in white 60's cleaned in a way to remove orange II gakk and in those batches, I recovered meth from rinse water in both batches. One of the two gassed very effectively, the other did not respond to gassing but did produce meth when the nonpolar was washed with a weak solution of water and HCl.


8ball

  • Guest
Locked in...
« Reply #4 on: March 01, 2004, 08:52:00 PM »
I have already evaped wash water....... Nothing.
I decided to put gassed np on heat and evap, now i consider this to be dry since moisture should sit under np(xylene) especially enough moisture to hold 18 available grams of pseudo, so to my surprise, now i'm baffled as xylene is evaped to near nothing pseudo starts to appear plus a heap of orange which was still liquid with maybe 10ml max xylene so took of heat and saton a wet sponge to stop the evapp and then poured acetone from freezer onto pseudo and orange, then filtered thru 1 coffee filter and rinsed once more with acetone. Once dry  13.6gms of supa clean sparkling pseudo. All orange rinsed straight thru. This is the best recovery i've had with a/b before and probably the cleanest pseudo iv'e had yet.
But i'm still stumped on why it did'nt seem to gas.


geezmeister

  • Guest
but is it clean?
« Reply #5 on: March 01, 2004, 10:06:00 PM »
You tell me you have sparkly clean pseudo, but is it clean?
And how would you know?

If it were pseudo HCl it wouldn't be in the nonpolar anymore. It is more likely that you have freebase pseduo crystals. You have seen what Scottydog describes evaporating the nonpolar for the freebase crystals. Note that Scottydog does not consider these clean yet, either. He redissolves in fresh nonpolar and titrates that for his final crystals. I would suggest you do the same. You may have just shucked the OII gakk and (under some of the suggested scenarios at least) this may have opened the door to the new gakk that is giving people fits gassing.

Now the question is why these did not gas out. The only thing I know that came to mind is a question of how long you let the calcium chloride and HCl sit before using it. You do need to give some time for the calcium chloride to absorb the water from the acid,otherwise you are gassing with air and fumes from the HCl. Granted, this is just a matter of waiting a short time and I doubt this was your problem.


Scottydog

  • Guest
Great recovery 8ball!
« Reply #6 on: March 02, 2004, 05:00:00 AM »
Good return 8ball. It is good to see more bees starting to evap the NP to recover their freebase. Who knows, by the time the NEXT generation of gakks begins to surface in all available pillstocks, bees may not have any other choice.

I noticed that you chose to use acetone to rinse your freebase of the orange oil.

***Swim has found that after a couple acetone rinses it will start to pull pseudo freebase.***

Swim has also found that if too much of the NP is evaporated away, the oil gets too concentrated in the freebase and becomes more difficult to get rid of.

After evapping the NP, Swim finds it best to decant as much of the oil from the freebase as possible. When one gets to the point to where all that is coming off is a few drops per minute, Swim opts to add fresh Xylene. One can use a stirring rod and mix the mass of freebase with the fresh Xylene and proceed to evap it down again.

When most of the Xylene is gone, the mass of freebase will once again reappear at the bottom and what little Xylene remains will have absorbed the remainder of the residual gakk. After allowing the contents to cool to room temperature, the rest of the orange can bee removed.

It is a little more work this way, but at least one will know for sure that any loss of precursor is negligible.

By doing it this way, one can run the freebase in a rxn "AS IS" or further titrate with fresh NP and water to get the HCL salt.

Sorry for the repetition, but hopefully the rest of the swarm will catch on. Swim has been dealing with this curse for a few months now. It must have hit his area first. If you are a US bee and have yet to experience this menace, I'm sure you eventually will.  ::)


8ball

  • Guest
but is it clean...
« Reply #7 on: March 02, 2004, 07:06:00 AM »
I am guessing it is clean going on past experience and the fact that to the touch it is so soft or fragile its hard to explain but with the dirtier gear it seems to bind together because it is seemingly stickier if i pick a little of this up between two fingers and squash it basically disintergrates or melts its nothing like that sticky crap that sticks to your dish after evaping.This is that white it has a blus sheen across it when you look at it under light at different angles.
Oz bee.


SHORTY

  • Guest
My ghetto gassing apparatus.....
« Reply #8 on: March 02, 2004, 07:44:00 AM »
This is based on VE's concept with the addition of silica drying chamber and foot pump.




8ball

  • Guest
Silica gel
« Reply #9 on: March 02, 2004, 08:24:00 AM »
Silica gel is a good idea Shorty but do you think it is necessary, I use one of them Garden sprayers they are about $10.00 and hold 1 litre you pump it up and thats it you just have to clean after use other wise i think it will melt.But it saves the foot pump .


biotechdude

  • Guest
@SHORTY
« Reply #10 on: March 02, 2004, 11:20:00 AM »
Damn SHORTY, what programme do u use for your fancy diagrams?  Very impressive...

SHORTY

  • Guest
Don't last long enough
« Reply #11 on: March 02, 2004, 05:29:00 PM »
I have used the pump up sprayers and they do work great the first couple times but im too lazy to clean it up after each use.  This setup had been used for about 25 10-15g batches of pseudo and is not even past the halfway point yet.  This is why i use the silica gel cause it keeps any moisture from building up between uses.  When its no longer usable ill just neutralize it with some base and toss it out and make a new one.  At this rate it will bee good for another couple months at least.

Biotechdude,
Thanks for the complement! Beleive it or not i use AutoCad 2002 to create my drawings.


geezmeister

  • Guest
Good way to clean freebase
« Reply #12 on: March 02, 2004, 06:10:00 PM »
Scottydog: This sounds like an improvement to your previous approach. Evaporating the extra solvent is a smelly problem, but what works-- works. You may want to try washing the nonpolar with a weak NaOH solution three times, then washing with plain water until the water comes off clean. You should get a grey emulsion at the interface between the nonpolar and the wash water. If you evaporate the nonpolar down for the freebase, my guess is you won't have anywhere near as much of the oil as you have had.


8ball

  • Guest
You should get a grey .....
« Reply #13 on: March 02, 2004, 07:04:00 PM »
You should get a grey emulsion at the interface between the nonpolar and the wash water.

Would'nt that emulsion contain both freebase and impurities not wanted, resulting in an xtra loss of pseudo  if emulsion was discarded or added impurities if evaped with np.

On another note i considered myself very lucky deciding when to pull np of the heat and rinse with acetone, considering my yeild. Only trying to repeat the process will tell.


geezmeister

  • Guest
the grey emulsion
« Reply #14 on: March 02, 2004, 08:20:00 PM »
The gray emulsion seems to be related to OII gakk. It comes out with plain water washes after washing the freebase pseudo laden nonpolar solvent with NaOH solution. It did not separate into layers or break down over several days of sitting open on the bench. It did not dry out, either. It was floating beneath the nonpolar solvent, was nonpolar in nature, and formed a distinctively separate mass to itself.  Yields were approriate for the extraction and I have no reason to think this gray layer held any significant amount of pseudo. I use the term emulsion loosely, and more for descriptive reasons than anything else.

I would not want to evaporate this with the nonpolar solvent. I would want it out before I evaporated, gassed, or titrated.

I think Scottydog would see a lot less of his oily gakk when he evaporates his solvent down if he would do this first. Maybe not. If it did reduce the amount of the oily gakk he has on evaporating the solvent, we could assume we are removing the same thing by this process, and that might be helpful information to have.


callen

  • Guest
Gassing...A.L.F.'s way!
« Reply #15 on: October 21, 2004, 03:04:00 PM »
Hello Brother Bee...A.L.F sez,"Try aluminum foil and Muriatic Acid...the foil reacts wirh the acid to form Hydrogen gass...this pressurizes the Rxn vessel and since Muriat fumes off HCL gass...the Hydrogen pumps the HCL gass through the tube into your Xtract solution...out pop all those wonderful Xtals." :)


indole_amine

  • Guest
H2SO4/NaCl !!! Nothing else...
« Reply #16 on: October 22, 2004, 02:41:00 AM »
Bullshit. Use 99% sulfuric, and drip on NaCl. Generates lots of HCl gas, resulting in overpressurized vessel... (you know the rest).

No gases have to be "carried over" by other gases, the HCl just evolves in such large quantities that it WILL exit the gas generator...

(and you can determine the amount of gas produced by checking the volume of the remaining sulfuric)

BTW ghetto fanatics can also improvise with a salt-filled millers beer bottle, PVC tubing and a H2SO4-loaded syringe (and lots of duct tape/silicone) to make molar exact amounts of ghetto HCl gas... ;)


indole_amine

hypo

  • Guest
i don't buy it
« Reply #17 on: October 22, 2004, 03:23:00 AM »
> BTW ghetto fanatics can also improvise with a salt-filled millers beer bottle,
> PVC tubing and a H2SO4-loaded syringe (and lots of duct tape/silicone) to make
> molar exact amounts of ghetto HCl gas..

i don't buy that (the molar exact amounts). i always had problems getting large
amounts of HCl(g) with this method. i think the Na2SO4/NaHSO4 layer around particles
hinders diffusion or something like that, but don't quote me on that.


indole_amine

  • Guest
Not for big amnts - but exact...
« Reply #18 on: October 22, 2004, 05:37:00 AM »
Well, at least it is reproduceable: so you could set up for 0.1 mol HCl gas and bubble this through well adjusted NaOH titrating solution, contained in a washing flask and finally finish titrating the NaOH soln. with adjusted HCl soln. and a burette or similar, calculate how much HCl you have absorbed in there, how much has left the system unreacted and/or is held back by the "apparatus". Now you have a very good idea about the usual losses and can calculate the almost exact molar amount of HCl you produce (of course only if you use the same bubbler, tubing, flask, syringe, amount of H2SO4 and NaCl; else you won't get consistent results... ;) )


indole_amine

morpheus

  • Guest
gassing
« Reply #19 on: October 22, 2004, 02:28:00 PM »
The only guess on this end is maybee the ratio of
non polar to freebase xtals was way way off.Sorry I honestly don't gas but if the crystals or powder were put in clean xylene or toluene yourself and it was pretty close to being anhydrous,some snow flakes would fall
if hcl gas was introduced.Unless what I said above happened