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Laboratory Tips Safety proceedures, test reagents, drilling rubber stoppers, bending glass tubes, etc. Contributed to by chemists.

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 #1 
Old 2003-12-20, 05:34
Rosie Rosie is offline
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Default jam

I have never claimed much experience, I just wanted to see what my bro was so into that he ruined his whole life for, and found an abundance of info on it. Swim did so well the first time, guess swim thought too easy and didn't need the instructions. Swim was wrong!!! Anyway, it's in a jar with tolulene now, what do you think about getting rid of np? What should swim do?
 #2 
Old 2003-12-20, 05:45
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Default Re: jam

Extracting the meth from the non-polar solvent.

If you want the cream of batch, toss ten drops of acid in a 75 ml of dH2O and pour that into your non-polar solvent/meth solution in the separatory funnel. Shake like hell. Then shake some more, and when you are done, shake it again. Shake it like it meant something, because it does. Drain this out and evaporate it separately. Hey, so what if the pH is 8. You will already have some meth. Add another batch of water and acid, the pH falls more, you get more meth in the next pull. This is why most folks get the bigger yield on the second pull-- they have finally neutralized the mix.
 #3 
Old 2003-12-20, 05:45
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Default Re: jam

It is very important to shake each volume of aqueous HCl in the non-polar as though your life depended on it. Chanting and speaking incantations are regarded by chemists as primative superstitions and by meth cooks as humorous ways of passing off the tedium of shaking the solution. Try chanting some time, it might surprise you how well it works. Chemists like to collect these three volumes of water/acid and evaporate them.I like to combine the first two and evaporate them, then evaporate the third one separately. He does this because he frequently gets too low on the pH, has some extra nasties in the last extraction, and likes to save steps cleaning most of his product. The first two pulls will be cleaner. Your choice, as it all cleans easily enough. Besides, by this point in time he has already sampled some of the cream of the crop and has the will and desire to do all manner of unnecessary things.



If the pH falls too low again this does not happen. You can add water, base it with NaOH and send it back to fresh non-polar solvent, and do it again, but the chances are you will lose product in the process and will have a lower yield than you would if you just cleaned the product you obtain. If you must hit it just perfect, do this. Understand, you really are placing the pH in a neutral position to allow the freebase to bond with the HCl molecule. When you evaporate the water/acid solution, you are going to concentrate the acid anyway. It is not that acidity hurts the meth HCl, it does not. It may introduce other contaminants to the water mix. These will need to be cleaned, but this is not difficult to do. the easiest approach to not overshooting pH 6.8-7.0 is to use larger batches of water, add a little acid to each batch, and do multiple pulls (five or more) and evaporate each separately. You will know when you fell below pH 7.0, as the odor of evaporating HCl will burn your nostrils and you will learn the value of a fume hood. You will also find that if you follow this method, your chances of contaminating the whole batch with some nasty creation that resulted from over-basing the mix are much reduced.
 #4 
Old 2003-12-20, 05:47
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Default Re: jam

Evaporating This should be done on low heat, in a visionware bowl, or flat pyrex dish, on a hotplate or with heat lamps, with an exhaust fan exhausting fumes to the outdoors, and with a fan blowing over the top of the dish. Too much heat will result in loss of yield as some of the meth vaporizes with the heat. Patience pays. If you have to have some now, evaporate that first pull by itself, then do the rest. Do it slowly. It will form a skin, or crust, as it evaporates, and will skin over before it fully dries. Try to let it dry without building up on the sides of the dish. Before it is completely dry, flood the dish with dried acetone. This technique is called "acetone flashing" and will not only rid the dish of its remaining water content, it will precipitate methamphetamine hcl crystals in the acetone.

While this post addresses flashing pseudoephedrine, it holds true for methamphetamine as well.I recommend letting the bowl settle down and cool down, then slyly tilting the pan so the meth stays in one place and the acetone slips to another. Then you can just pour the acetone into a beaker, and not have to pour it through a filter. Filters absorb a lot of product. If you must use a filter and have a Buchner funnel, now is the time to use it. If you don't, you can pour the acetone--and meth-- through a coffee filter and let it gravity filter. Rinse with a little fresh acetone, particularly if you used too much acid. Place the filter aside to air dry, or heat with gentle heat. If you panned the acetone aside, leave the meth in the glass dish to dry. If the meth is anything other than sparkling and white, rinse the meth in fresh acetone. Do this in the dish if you have panned the meth to one side, or rinse the meth in the filter with fresh dry acetone. Do dry the acetone before use, and do save all the rinse acetone-- particularly the acetone used to flash when the dish is still warm.

Put the acetone poured off after flashing in a beaker, cover, and place this in the freezer. You can add the acetone used to rinse to this. Give this time to chill and pin crystals of methamphetamine will form. You may filter these or return them to a glass dish to pan and separate the acetone. Save the acetone, it still has gold in it.

Cleaning the methamphetamine HCl The product you have is probably usable as it is. It also can be cleaned further by rinsing with fresh acetone. True cleaning calls for recyrstalization.

Jam.
 #5 
Old 2003-12-20, 05:48
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Default Re: jam

How do you wish to proceed? Options are to gas, or extract with an aqueous solution of hydrochloric acid. A third method is to accumulate hydrogen chloride gas in alcohol, and add that to the non-polar. The author has never observed this method, let alone used it, and if you are interested, you will have to UTFSE.

Gassing is usually performed by placing the tip of the hose or wand from the gas generator just a fraction of an inch above the surface of the non-polar solvent, so that the gas being emitted contacts the surface of the non-polar solvent and the force of the gas flow pushes it down slightly. Bubblng the gas through the solvent is advocated by some proponents of gassing and condemned by others. The non-polar solvent may, but will not necessarily snow crystals. Ususally the solvent will thicken and look like applesauce. The solvent will have to be filtered through a filter and the filtrate allowed to dry.

If the gas is not dried prior to application in the non-polar your meth will disappear in the water; if you see that yellow nasty stuff at the bottom of the jar, do not despair. Separate it and evaporate it as you would if you titrated.

Newbees probably should not leave it to chance. I do not recommend that you never use pH strips or a meter, that you never learn how to boil red cabbage and use the extract. Those are all wise things to do. All the same, no newbee should despair when his water in that non-polar he extracted his honey with suddenly bottoms out on the pH scale. I learned the how-to part of it before he ever got acquainted with pH strips that measured high enough, ever had pH meter, or ever boiled red cabbage. There are sights and smells and pressures and changes you note to tell there is enough. It is not a life or death game of pH levels as far as the meth is concerned. You can over do it, and you learn not to. You can do it by touch and look and look and smell and not overdo it either. Its a lot like any AB process: you get a feel for it, a touch, a nose, whatever--- you learn where in that one quarter of a turn it becomes tight enough, or here, where the pH is low enough, to accomplish the purpose. And you learn by experience that dry acetone can be your best friend and that acetone jar you save your rinsew acetone in your salvation when you overdo it. That isn't chemist logic at all. But it works for cooks.

Jam.



[This message has been edited by Jamiroquai (edited 12-20-2003).]
 
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