If you're new to extractions and separations, read this first.
The base meth molecule must be crystallized as a salt before it is consumed. Ephedrine should be made into a salt for the work that will be done with it - Not always necessary, but the salt is more soluble in an aqueous solution, and you will need to do an organic sep ("AB extraction") to it anyway.
The previous pages go through practical extractions of ephedrine pills and ephedra herb. Let's go further and generalize the extraction procedure, so that we can get a meth product out of a finished reduction solution as well, and convert it into a consumable salt.
Typical chemhack extraction procedure:
Make a saturated NaOH solution (stir lye into water until it won't dissolve anymore). Add this lye water in small portions to your target solution until a pH of 12-13 is reached. Lye pellets, which dissolve slowly, will work as well here. You should notice a characteristic fishy smell at this pH, but use indicating pH paper or a meter to check it. Now stir in some ordinary table salt until it won't dissolve anymore. If this is a large meth batch you're isolating, you can skip directly to an acid workup. Otherwise, add a portion of toluene equal to one-third the aqueous solution, seal and shake this together for a few minutes. Pour it into in a separatory funnel if it isn't already and let the layers separate. Or just decant the toluene off the top if you're using jars or the like. Don't try to get the last smidgen of toluene floating on top in this case - it doesn't add up to squat in the end, and you don't want any water in the separated toluene.
Repeat this procedure with fresh toluene two more times. Before the last toluene extraction, recheck the pH and add more lye if needed. The combined toluene is then set in a clean glass container for awhile to let any entrained water come out and cling to the glass. Slowly decant into another clean container to leave these droplets behind. (Notes on further drying the organic solvent later.) The meth or ephedrine base, and whatever other alkaloids were present, are in the toluene and ready for gassing.
(Oh, don't have any indicating pH paper handy? Don't want chem-related items like that hanging around your abode? Do it the Grizzly Adams way: Just concentrate some fresh beet extract and put a few drops in your mixture. When the pH reaches ~12.0 the red color will go away. Nice, aye? This happens to be the pH at which your HCl salt is basified, making it an excellent indicator. Basifying HCl salt is about the only use I have for testing pH, so why keep paper or meter around?)
Ok, the meth or ephed base is in an organic solvent now, time to crystalize it as an hcl salt...
The Way Of The Gas
Making Hydrogen Chloride gas is simplicity itself, if a little tedious sometimes. All the more ridiculous that the sale of cylinders of gaseous HCl is controlled to the same degree as the really naughty drug precursors. Such is the stupidity of "do something!" Drug War legislation. Anyway...
Check the hcl generator pictured below.
The lid of the first jar is drilled with two holes. In one is glued a rubber grommet or ring to provide an airtight insertion for the syringe. In the other a nipple is glued in for the hose to connect. The rest of the assembly is as shown. A small funnel is rigged as a little aspirator fume hood for the gas outlet. You might hook the aspirator hose directly to the solvent jar outlet, though this would create a vaccumn. Sure, it should still work, but the solvent will boil away for a while and get mighty cold. Alrighty then...
If you don't need lab glassware for other purposes, a mason jar version like this is EZ and appropriate, and will help keep you out of jail should Deputy Barney come looking. Nothing gets you into jail faster than laboratory glassware.
* The H2SO4 drip onto NaCl/HCl slush can allegedly be replaced by dropping aluminum foil straight into HCl acid. A correspondent did this experimentaly and recognised the aroma of HCl (it chased him out of the room in fact). It is a vigorous reaction, the clandestine chemist would be cautious and prepared for this.
* If there isn't much in there to start with you may not see anything. The solvent will just become HCl saturated (smokin). Don't throw it away yet. Seal it up, put it in the freezer overnight and see what develops.
* If you have a leak, or your fume disposal isn't what you thought, your mucus membranes will notice that fact pretty quickly - Shut the stopcock and ventilate the room.
Back to the AB extraction, the other source of HCl salt ruination is water in the organic solvent before gassing. Solubility of water is low, and is dependent on the org solvent used, but it is never zero. Obviously, it gets in there from the aqueous phase of the AB extraction, though hardware store solvents can come that way. This is easy to fix.
Actually, someone going by the name of Dickboy posted on this very subject, and since he explained it more clearly than I would, I'll use his text:
These steps apply just as well to ephedrine, though it isn't a liquid at roon temp as is meth.
The drying agents described here are non-suspicious and very cheap. Here is a list of drying agents and their usage, laboriously typed by mr pyrex.
* The success of extraction and salt-making can be rather dependent on the amount being worked with, if the process is done sloppily. This is a common newbee nightmare. Some individuals make, and have only made, larger batches. They've always got their product out because the amount lost in the wash due to undried solvents is a small portion of it. They don't even know it is occuring. They laugh at the silly people that go through drying steps. That same person working with several grams will then lose it all or most of it, and wonder what's going wrong.
* Chemists have had good results using hardware store Xylene in place of touluene. Indeed, it does dissolve less h2o, which is always desireable. It also has a higher bp, thus requiring more effort to dry the crystal product. Like a warm hairdrier or such.
For larger batches of meth, there is a simpler way to go for the final hcl crystalization of the product. Following reduction, the solution is made basic as usual (pH 12-13), saturated with table salt, and then allowed to sit in a separatory funnel for awhile. The meth freebase (an oily liquid at room temp) floats to the top. A wonderful sight for the long-suffering chemhack! The aqueous reaction layer is drained off and tossed. The meth oil is shaken together with clean water, and separated again. This is repeated until a clean amber meth oil is obtained. HCl acid is then added to the meth oil to bring it back to a slightly acidic pH of ~6.5. This solution is simply evaporated to yield the hcl salt.
Caution: Bringing the meth oil to the desired pH is tricky. It will suck down a lot of HCl acid with little apparent change in pH, then shoot down the scale into highly acidic territory. After the initial slosh of HCl acid, further additions are made slowly and pH checked carefully. Give it time after each addition so the solution can reach equlibrium.
I should add, that an acidic solution reverses the partition with a toluene layer: an alkaloid extract in toluene will go back into the aqueous layer if it is acidified. Does that mean you can do that and just evaporate the aq. layer to get the salt? Sometimes yes, sometimes it doesn't work, for reasons I just don't know. See if it will work for you, under the conditions and temps which you are working.
Ether in the home gets chemhacks in the newspaper. It is most suitable for large drug production outdoors, in barns and such like, gascans and guns. Here goes anyway:
Dissolve your base material in hcl acid - The hcl must be at least equamolar with the base alkoloid - generally, enough acid to dissolve the base will do it. Add at least an equal amount of acetone, and swirl. To this solution is added ~8 times its volume in ether. Shake it up. The salt comes out, crystalizing in the ether. Done. Pour off the ether+precipitate and filter it or evaporate to get your product.
Yup, that's a lot of ether. The idea in using this procedure is that you are out somewhere crystalizing a great deal of the salt and reusing the ether repeatedly. It's also ok for very small amounts, test tube sized, such that the procedure can be done with two hands and a thumb over the top of the test tube. This is never done inside the home or around any possible ignition source.
* Freon can be used here as well. This would be far superior to ether, natch. Easy availability of freon these days is the question.
* If you live in snow country, a good clandistine cover for test tube-sized production is under the open hood of a car, with a can of ether starter fluid visible.
Ether is more particularly useful however, in producing a good base material through an AB extraction. It can be a pain to evaporate completely the heavier organic solvents, and for some purposes you want your base as pure as you can get it. Make your aqueous solution basic, then load it up in the car along with your ether starter fluid and take a drive out somewhere. Spray the starter fluid in a bottle to collect the ether. Cap it and let it sit to let any entrained fluid or lubricant to layer out. Do your sep using the ether and pour off the ether layer. Let the ether evaporate to get your base product (this occurs very quickly). Back in and off you go!
* By allowing the can to sit upright for a while, and only collecting the first 2/3 of the can's contents (starting fluid is cheap), you can avoid most of the entrained lubricant in there. The lubricant will not evaporate as will the ether, so separating it out one way or the other is necessary if base is being extracted and the solvent evaporated.
In this variation a sulfate product is salted out by dripping concentrated sulfuric acid in an ether or toluene extract with stirring. The precipitate should form immediately. That's it.
