Silk Road forums
Discussion => Drug safety => Topic started by: geedogg on July 14, 2012, 12:01 am
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This is blatantly taxed off a clear-net forum (DF) and props to Epote the original poster, I have never tried this but I feel it will be sound if one were inclined, and I know certain members have been talking about it so here it is.....A/B extraction to obtain a purer product than acetone washing.......
Acid Base extraction explained:
The acid base extraction is routinely used (and sadly routinely avoided...) at the cocaine manufacturing procedure. If you read what i wrote (and im sure you didn't so go back and read) at the cocaine extraction procedure you would see that the cocaine paste and/or base is frequently treated with some short of acid and then some short of base, with the resulting precipitate filtered. Thats what an acid base extraction is.
Essentially the cocaine alkaloid is a base, that is it makes the ph of water greater than 7. Bases are not soluble in polar solvents (like water) but are soluble in non polar solvents (like kerosene, ether etc, acetone is an exception i will explain later why). So the theory behind an acid base extraction is that when you add slowly in a basic solution (ie cocaine and alkaloids in kerosene etc) the stronger base will react first and precipitate. Depending on what is the stronger base you either discard or collect that precipitate (by filtering or by utilizing two imiscible solvents).
For example during extracting the alkaloids from the leaves, they dump the leaves in water and add some alkaline material. That forces the alkaloids to come out of the leaves into the water. Because they are bases they are not soluble in water and thus stick to the bottom. They then add kerosene witch is not miscible with water (that is it collects to the top in a separate layer). The kerosene dissolves the alkaloids and is extracted from the water.
That is the first step of an acid base extraction. The second is to add an acid. Specifically they add a relatively strong acid like sulfuric. Some alkaloids (including cocaine) form a sulfuric salt which is no longer soluble in acetone and they precipitate in the bottom. They are filtered out and collected. The point is that in that way some of the weaker bases do not react and do not precipitate, thus the end result is procedurally purer.
So what your flamingo need to perform an A/B extraction is these a) the substance to be made into base and salt b) a polar solvent (water) a non polar solvent (ether or methanol) c) a base (ammonia) d) an acid (hcl acid) d) glass beakers and rods, filters etc
Doing an acid base extraction of street cocaine
Specifically cocaine base can be dissolved in acetone which is polar. Thats an exception, but the solution is not very good, the cocaine base is dissolved in acetone but tends to concentrate on the bottom and not be completely homogeneous. Which is good for us, you will see why.
The basic steps of street cocaine purification with an acid base extraction are these:
1) dissolve cocaine in distiled water (1 gr cocaine in 60ml water ) in a glass beaker. Filter the solution to get rid of any water insoluble impurities. The 60ml water is kind of arbitrary, you just need enough water for the cocaine to properly dissolve and for the ammonia solution to be weak, i.e not overshoot the ph. Also you need enough water so that the basification proses will be easier (stirring wise)
2) titrate (i.e add very slowly, no more than a few drops each time) ammonia hydroxide solution of around 10%. It doesn't really matter actually you just need it to be very dilute (5-15. While vigorously stirring with a non porous rod (preferably coper but glass or plastic is good). At this point you must be very very careful. The theory is that the impurities will react with the ammonia BEFORE cocaine. In any case, when the first drops of ammonia hit the water the solution will get white, stir and stir for 3-4 minutes until the solution starts becoming clear. Quite possibly the impurities will start to get stuck to the walls of the beaker and the rod. A copper rod is preferable because it forces things to group up because of electrical affinity making them to stick on it instead of just precipitating also try not to touch the beaker while stirring, that tends to form crystallization nucleons that will precipitate, you don't want that. Keep adding ammonia and stirring like this. When the beaker and rod are visibly dirty by the impurities change beakers and clean up the rod. You do this in order to keep the impurities sticking to the rod and beaker instead of precipitating to the bottom. After enough ammonia is added you will observe a white crystal like deposit to the rod. It ought be like snow. This is cocaine base. At this point CHANGE BEAKERS and clean the rod. Some cocaine will be lost, but this is for the best. Keep adding ammonia and stirring you will see that when the rod and beaker are saturated the cocaine base will start falling like snowflakes to the bottom of the beaker. When the precipitation ceases (no more white cloud will be forming when adding ammonia) and the water smells strongly of ammonia the precipitation is done and you have cocaine base. Do a thorough water wash at this point. I.e add distilled water, stir and filter.
3) Filter out the precipitate which is cocaine base. Slightly press the the filter to rid of any redundant water. Use the filter to cover the cocaine base and dry it in a heat lump/the sun/or with cool air until dry to the touch, then dump the powder to a ceramic plate, chop it up and let it dry until fully dry (when it is like flour and chops up with no residue its dry, leave for a day or two). An efficient way to dry it up is using a desiccant like anhydrous magnesium sulfate. Just sprinkle some of that around the cocaine ceramic plate and cover everything air tight with a glass bawl or something, after a few hours it will be dry
Thats cocaine base, SOME impurities will have turned to their base form as well, for example amphetamine base is a stronger base (thus weaker acid in its salt form) than cocaine so it will react later, so you will not be able to get rid of it. BUT it IS slightly soluble in water (while cocaine is not) so the water wash of the cocaine base will get rid of it.
Converting cocaine base to cocaine hydrochloride:
there are several methods to do this, i will describe in detail the best in regards of end product quality and give an outline of the other.
1) dissolve the cocaine base in ether (1gr of cocaine base per 15ml ether). Filter it to get rid of any ether insoluble cuts that remained from the ammonia treatment
2) dissolve 38% lab grade hydrochloric acid in acetone (0.25ml of hcl acid per 15ml acetone per gram of base
3) add the acetone/hcl acid solution in the ether/base solution. A visible white reaction will form, crystals will start precipitating in the bottom. When the solution is no longer reacting (it will be clear no white clouds), gently stir it, leave it for a few hours for the crystals to properly grow. Run the rod up the beaker, over carrying some liquid, if no crystallization happens you are good, its done. In any case leave it 3-4 hours to properly crystallize.
4) discard the ether (leaving the cocaine in the beaker!) and do a very thorough acetone wash in order to remove any traces of ether left. After a few pours of acetone in the beaker filter out the cocaine base (just like le junk describes nothing fancy). Perform a final acetone wash over the filter. Fold the cocaine in the filter and let it dry for a couple of days. Thats called an empanada
voila cocaine as pure as it can get
the other method (ether free) is done by dissolving cocaine directly into acetone. Then dissolving hydrochloric acid (38% lab grade) in methanol. You use 0.25ml of hcl acid per gram of cocaine base and double that of methanol i.e a 1:2 solution of hcl acid/methanol. You gently swirl both beakers by hand (like rotating them) and mix them, cocaine will start precipitating. After 2 hours stir everything and let for another 4-5 hours. Then filter out the cocaine acetone wash and let it dry.
The art of crystallization
Q: Isn't ether dangerous?
A: YES! Very dangerous, i will explain later why, just bare in mind that it is, extremely flammable
Q: So assume i do this, why even use ether? Actually why not use just acetone?
A: The thing is, that you need an alcohol type (non polar) solvent in the procedure for the crystallization to happen. You see theory is that to produce crystals you must dissolve the base in a solvent in which the salt form will precipitate when you add the acid. Acetone is used because it dissolves cocaine and is miscible with hydrochloric salt. Problem is that it is polar and as an "exception" dissolves cocaine. But the way it dissolves it is problematic, and thus the crystallization CANNOT occur in just acetone. It will merely form an oily residue in the bottom when hcl acid is added. You thus need a pollar solvent that will force the cocaine base to be in solution and absorb the traces amount of water that are in the hcl acid. Ether alone cannot be used because its not miscible with hcl acid and methanol alone cannot be used because it will dissolve cocaine hcl. So a mixture is needed either ether acetone hcl acid or acetone and small amounts of methanol (or ethanol) and hcl acid. Ether is preferable because it does not dissolve many of the cuts that got away in the ammonia treatment, it properly dissolves cocaine base, is higly miscible with acetone and because it produces a visible white reaction. Simply put it produces faster, better quality, and visually pleasing crystals.
Q: Ok so do i need to stir?
A: If using ether, no you don't need to stir, although stirring will effect the size of the crystals, generally speaking more stirring = smaller more pure crystals
The science of crystal formation is that when a polar molecule is formed, other polar molecules gather close to it and form a crystal structure with self repeating patterns. The whole thing starts with the nucleation, where the solute molecules form clusters (nucleation is what happens around the straw when it enters a bubbly beverage). If the solute are not properly distributed in the solvent this will not happen properly (thus why you cant use acetone alone). If no stirring is present the nucleation spots will be few and the crystals larger, but large crystals tend to hold impurities even small amounts of solvents inside them. A fine balance between size and appearance and size and purity must be found.
Rapid changes in ph must be avoided, crystal growth must either happen all at once or very slowly, large ph differentials cause uneven and impure crystals. The finest looking crystals are those that are formed in the same time and let to grow slowly, thus the ether, acetone, hcl acid is best. Some stirring must be present to avoid uneven in size and impure crystals, though not too much because it will loose the mother of pearl sparkle that is so desirable by the connoisseure. Temperature and light conditions also effect crystal formation. Crystals grown in the dark and at stable SI temperature are far more equal in size while crystals grown with a rapid drop in temperature tend to be purer but smaller.
Experimentation is needed to find the proper procedure
a few notes about using ether
for starters everything you use during the base to hcl session must be anhydrous.
Same goes for ether.
And mind you ether is EXCEPTIONALLY dangerous. Overtime ether reacts with oxygen and form peroxides, peroxides are friction and movement unstable, meaning that the friction of the cap unscrewing can detonate them. Lucky for us, the procedure we use does not involve distillation or evaporation of ether, which makes things a bit safer. In any case store ether away from sunlight and anything that could produce a spark. If it is not stabilized do not keep it more than six months after opening.
If any visible precipitate exists in your bottle DO NOT MOVE IT, CALL SOME SPECIALIST
Ether produces vapors that are heavier than air and can concentrate in explosive amounts, and can creep up electric sockets. Always use ether in a WELL VENTILATED PLACE AWAY FROM SPARK SOURCES. Always take measures against static electricity, before handling a bottle of ether.
Finaly ether is rather intoxicating, be in a well ventilated place and breath as little of the fumes as possible.