Gassing the only way?

[foxy2]

Ask Dwarfer   
I heard him describe it
Do Your Part To Win The War

[Osmium]

The Stoni gassing procedure:
Plastic squeeze bottle with a lenght of clear PVC tubing attached to the screw on top. Put in some solid NaCl, add a few milliliters H2SO4, close bottle and bubble an air/HCl mixture through your solvent by squeezing the bottle. Works great. Once HCl generation slows down shake it a bit, or simply add more H2SO4.

[blaztoff]

Stonis method is the shit. No worry about smell anything. Only difference i do is attatch the hose to a jar with a lid and a fitting on top for the other hose on top. As gas is generated it slowly will fill up other container and as it comes in contact with solvent boom crystals. put a stirbar in on slow for agitation and sit back relax go out whatever you have youre crystals. Never had a problem - no equipment really needed no smell. Shit I did it in my bathroom with my wife in the other room and she never knew. Works like a charm

[Dope_Amine]

And you don't need aqueous HCl to gas, just drip sulfuric on NaCl.
something for your mind.......

[relentlesson]

This is a very interesting debate between gassing and simply adding aqueous HCl to form end product. Swim has not tried gassing but is not terribly inclined to with the success she has dreamt about dripping in ice cold (lab grade) 36.5-38% HCl into the freebase (methamph.) toluene mix and watching carefully to see when the colour equalizes between the two layers, as in their is no cloudiness in either layer and ideally the colour should be golden to golden bronze. Shake a little in sep funnel and leave to stand for around 15 min or so. If the toluene fbase mix is dry then crystal will have already formed blocking your exit from the bottom of sep. funnel. so at this point one can either filter the whole mix, or as swim prefers, add a little distilled H2O to dissolve the crystals and drain off bottom layer without any tol coming over. Putting bottom layer on hotplate to over 105^oC but below 140^o and directing a hair dryer at pyrex container (ideally in oil bath on hotplate) will bring the water off nicely and a skin will form. When skin is nice and thick the container is let to cool down a little and placed in fridge. After about an hour or so the mix is filtered, liquid reduced again, and the crystals rinsed with ice cold acetone. Recrystallization takes place with methanol and a splash of acetone. Awesome shardage! It has been noticed that if too much HCl is added the bottom layer will turn a darker colour heading towards deep purple at around pH 3-4. Does this hurt the yield swim wonders as it has never been actually determined quantitatively? Also, when the two layers as afore mentioned match in colour (just) and the cloudiness in both layers disappears the pH is usually 8-9 and the mix crystallizes fine, and then can be hit again cautiously with the HCl. Is one better off to stay above 7 or just below it? Anyways, whenever neutral is achieved in HCl addition results have always been favourable, but swim wonders if it is just fine to speed it up cautious wise and land where ever between pH 3 - 6.# ? One last question, what is the dark brown ultra fine sediment that changes the base colour so dark when re-extracting from say ones acetone wash or somewhere fucked up mixture? Attempts at removing it through NaOH and washes with water have been not all that great. Distillation would be the obvious answer but unattempted as of yet in dreamland. It would seem that this sediment only occurs when the pH is sent too far below neutral.
I know what I like, but I might like something I don't know.

[alchemy_bee]

even if you gas outside, if there is a void in wind current you're still going to burn your self if you catch a puff of HCl gas. The prefered method here is to place a cheap high velocity fan in the window, and put a couple pillows on either side and set it blowing outward. Works like a charm, all noxious gas is quickly escorted out.

Alternatly set up a distillation setup, replace condenser with column packed with drying agent. Into the boiling flask is HCl/NaCl mix - at the three way adatper between boiling flask and condenser position addition funnle containing H2SO4 - in the recieving flask place solvent/freebase. Lastly between the column and reciving flask use a vacuum adatper that has a drip tip, place a hose from drip into solvent/free base to the vacuum off nipple (nipple, teehee) attach hose running out window or into basic solution.
Can a bee be visa vis its entity when half a bee philosophically must ipso facto half not be?

[Sunlight]

I've used the method of evaporating toluene+alcohol+aqHCl till 140 C because it's very easy and you can process any amount without gassing. Now I think it produces a bit of decomposition of product, actually a mix of IPA + toluene + aq HCl is evaporated with the aspirator at low temp, water is removed with the azeotropes and crystals appear in the flask, more toluene is evaporated and finally it is filtered and the crystals in the flask are taken out and rinsered with acetone. Much better, no decomposition and maximum yields.

[relentlesson]

Wondering a couple more things and thank you much Sunlight for swis posting a reply to swims post. What is notSunlights opinion on the ideal pH to have the toluene, isopropyl, HCl(aq) mixture at before reducing to obtain the golden key to the diamond mine, and if certain solvents ie. methyl hydrate, will work better at a different pH than the one ideal for isopropyl - (the question mark isnt working on keyboard) And secondly, swim has pondered and experimented intensely for some time on how to construct a trap that will capture low boiling solvents like acetone, isopropyl, methanol, etc. for recovery and to not eat the lining of swims many assorted pumps -- swim has wondered if possibly constructing a thermos containing liquid nitrogen in the walls or perhaps setting a pyrex filter flask trap right into a bath of liquid nitrogen, would get the trap cold enough to condense all low boiling temp. solvents and stop them from getting sucked into the pump , any comments appreciated -- Also, if swim may, can isopropyl, methanol (methyl hydrate), ethanol 95%, all be used interchangeably and even mixed perhaps, in crystallization procedure (question mark) hehehe. Swim has used them all independantly with varied success but wonders if someone could point out ad and dis advantages of the threes use.

Much is grassy ass,
R
I know what I like, but I might like something I don't know.

[PoohBearium]

...and wish the best of luck to those who dream.  PB'll fall asleep one of these days, I hope  

PB
Put your left leg down - your right leg up,
Tilt your head back - let's finish the cup!

[Sunlight]

Best is IPA, methanol does not form azeotrope with water, and ethanol forms and azeotrope, but you'll have at hand the azeotrope, not absolute ethanol. IPA forms azeotrope with water and with toluene, below their respective bp, what means that you remove the water and IPA and excess toluene at < 10 C with a poor vacuum (aspirator). And yes, the problem is that if you use it, the solvents will go to the drain. Anyway, if you distill at room temp, you can't isolate the toluene and IPA, so it could be a waste and it has some ecological concerns...

[relentlesson]

Many dreams have been found to include exclusion of all three mentioned solvents, but for recrystallization. When it is time for the picnic and the chili is first pulled out it is done with just HCl(aq) and a splash of H20, set to chill after slight reduction and filtered, redone until nothing left in the basket, must be Yogi. Recrystallization done with Methanol cause of ease of accessibility, cost, and odor. No real complaints as 95% comes back as large shard. So swis, you are saying that swim would get better results in recrys. with IPA or in the initial pull by omitting any splashes of H2O and sticking to HCl + IPA into the toluene for release.(question) or could it be swim is missing quality nap and not realizing recrys. may not be necessary if IPA + HCl (aq) used solely in initial (and only then) pull. Well not to bore y all so will compare with next nights sleeep. Again, just wondering what is ideal guideline to follow regarding pH. If stopped at around 8-9 , had a dream that reoccurred several times over while waiting 30 min between naps. Could this just be a waste of time though compared to just adding more HCl(aq) and H2O or IPA down to say pH 5 right off the pillow. Swim guesses that would make interesting thing to dream about comparatively as well. Hate to waste sleep so appreciate any guidance. ZZZZZZZZZZzzzzzzzz
I know what I like, but I might like something I don't know.

[Sunlight]

I don't understand exactly what you say.
First, after extraction of the base and drying the solvent, you xtallize. There are many methods
1) PIHKAL evaporate solvent, dilute base in IPA, neutralize with conc. HCl and add 4 volumes from IPA of ether or acetone.
2) Same, but prepare IPA+ aq HCl and dry it MgSO4 or NaSO4. Neutralize the base directly with your acid IPA, then add ether or acetone.
3) Gass your dried solvent + amine (toluene or ether) with HCl, wash with acetone.
4) Dilute the base in 6 vol or so of acetone, neutralize with aq. HCl and put in the freezer, recover crystals, evaporate everything and do it again.
5) Add to your toluene extracts IPA and aq HCl to get a homogeneous mixture at pH 5, evaporate in vacuo (or at normal pressure) removing water, IPA and toluene, when you have a lot of crystals in the flask and some toluene, take them out, take the rest out with acetone, filter and wahs witha cetone.
6) and more and more...
Once you have your crystals, you can rxistallize to get more pure stuff (or specially if your crystals or not white) by diluting them in the minimum amount of boiling IPA, then add 4 volumes of cold acetone. For MDA use methanol.
If you make things correctly and get nothing, think about a failure in your production.

[relentlesson]

Please accept my apologies swiS for trying to bee too clever in swims last post. What swim was saying is that after extraction of base from reaction mixture (at this point a mix of NaOH,H2O,product,NaI and other salts(swim thinks))into 3 volumes of toluene, (so one theoretically has just base and toluene along with some impurity) all that was added was 36.5 - 38% HCl (aq) and a splash of H2O (by small swim means 50 ml or so regardless of volume in sep. funnel), however the criteria for adding the H2O is to stop the end of the sep funnel from clogging up with xtals, if the toluene is wet and no xtals are appearing at bottom of sep then no addtl. H2O is added. (had bad experience with using MgSO4 to dry cause swim was dumbass and after microwaving it, ground it into coarse powder, added it to toluene and made big gooooey mess) This bottom layer which is just slightly on the basic side of neutral is then reduced until a healthy skin covers the liquid in the pyrex tray on hotplate, at which time it is put in fridge (above zero celsius) and left for a bit. Upon return xtals have formed quite heavily and are filtered off, rinsed with acetone, dried and re-xtalized in methanol (minimum amount like swis says) with only a splash of acetone (50 ml) and not 4 x volume, will have to try that though since swim only gets two thirds original weight back each rextallization. The remaining liquid from the rextal. is reduced further and process repeated to eventually give up the aforementioned 95% original weight. What is the 4x volume of acetone for(question), is it to have greater yield on initial recrys. or is it affecting size or shape of xtals, or could it bee affording a purer end result. Overall and original point swim is trying to make here is that why use the more odorous (is that a word, hmmmm) solvents like IPA or ether when just plain old HCl(aq) and mild smelling (swim thinx anyhow) methyl hydrate seem to do very well for xtallization. Swim dont want to beat this thing to death and appreciates the patience shown 2 da rookeee.
I know what I like, but I might like something I don't know.