IF THINGS HAVE GONE WELL TO THIS POINT, YOU OBVIOUSLY ARE DREAMING-- OR HOW TO HANDLE COMMON PROBLEMS YOU MAY ENCOUNTER BY THIS TIME.
Any number of misfortunes could have befallen the cook by this time. The principal problems Geez is personally familiar with are:
EMULSIONS: There is no single source of emulsions. Some are caused by adulterants in the precursors, some may be caused by anti-caking additives in table salt, some may be caused by ingredients added to NaOH in OTC lye preparations. Some are caused by residues on the glassware, including traces of soaps or detergents. Some emulsions are nothing more than the result of shaking oil and water together. The most common cause of emulsions is inadequate cleaning of the precursors, particularly pseudo. Using an effective extraction technique suited to the source of the precursor is the first line defense against emulsions. Recrystalizing the pseudo twice before reacting also tend to remove impurities and make emulsions less likely. Using NaOH solution rather than dry NaOH to base also helps avoid emulsions.
Other preventive measures include using rock salt or pickling salt (rather than table salt). Not using soap or detergent to clean the glassware, and rinsing glassware with acetone after washing help limit the incidence of emulsions. The next best preventive measure is to avoid shaking the polar and non polar layers togeher. Swirling is sufficient. Stirring is permissible. Shaking is asking for emulsions. Period. You do not need to shake.
Combatting emulsions:. There are several ways to combat emulsions. The first is to
let it just sit there until the emulsion goes away. Another is to take a stick and
poke at the bubbles. This works only if you are sufficiently wired to want to do this for twelve hours. Another is to
add additional non-polar solvent and stir. You may also
add a small volume of acetone to the solution and stir. This may be exciting...it may effervesce as you add it. It may do nothing. You may also
add a little TCE while stirring. This will quickly settle to the bottom, but has been reported in certain circumstances to have an effect of breaking an emulsion. The most likely successful method if waiting alone does not work is to pour all of the reaction fluid, emulsion and non-polar solvent into a flask or coffee pot or container that will take heat, and
heat it up slowly, stirring occasionally. Bring the reaction fluid to near boiling, and allow the non-polar solvent to heat up. While doing this, it may help to
salt the emulsion with ground rock salt. It may help to
add a few drops of hydrogen peroxide the the mixture. The poster has even added drops of 35% H2O2 to the mix, which gives a violent reaction, which may or may not do anything other than cause the non-polar solution to bubble out of the flask, but is a diversion to watch. While heating, add some boiling stones, broken clay pot pieces, or washed coarse sand to the flask to keep it from forming bubbles so large as to displace the volume of the container and spray you with the meth-laden non-polar solution, rendering all of your efforts a complete waste. This phenomenon is referred to as bumping. Do not let it destroy your day. It is simple to avoid. One final suggestion, used on one occasion by the poster helping a friend out of a jam, is to finely powder
activated carbon and add this to the contents of the boiling coffee pot or flask. It will float to the interface. Grind it finely, you want it to be fine. Bring the contents to a boil. At first it will appear that the carbon is blocking any meth from coming to the surface, but as the convection currents in the flask increase the carbon will beging to swirl on the top layer, and you will be able to see into the reaction fluid layer. Boil for ten minutes or so after it reaches this point, the let the mixture cool. Separate out the non-polar solution. This worked quite well when the emulsion present was suspected to be related to glycol and cellulose that was contained in the pseudoephedrine being used.
If none of the above work, suicide is an effective solution, as is starting over with clean precursors.
Lye lock and other such ideas Lye lock is the state which the reaction fluid reaches when the cooling reaction fluid is saturated with NaOH and thickens. The author has experienced something along this line once or twice. If you encounter such an event, heat the solution slowly, or add hot water to it and stir.
You got ahead of yourself and added HCl to the sep funnel. Stranger things have happened. Add more water, add more NaOH solution. That is all. If you can acidify the based reaction fluid to recover I2, you can base the acid in the reaction fluid to raise the pH.
Ker Plunking -- the variation on the Acid/Base extraction. Post 59240
(Worlock: "Ker Plunking for quality and quantity", Stimulants)Ker Plunking-- whether it is all that it is advertised to be or not-- does in fact provide an efficient way to perform an acid/base extraction of methamphetamine from the reaction fluid. While it is principally a way of heating the naptha used to collect the meth freebase to increase its solvency, the process also entails heating to combat emulsions, and a slow basing process which allows one to watch the process and visually determine that the freebase is eluting to the non-polar solvent, and to maximize that process by cues derived from the addition of base, salt, stirring, and heating. When the bubbles are eluting and are obvious and numerous, stop addition, turn the heat off an wait fifteen minutes. Separate the naptha from the reaction fluid. In the poster's experience, your yield, if you did this properly and with sufficient naptha (count on 500 ml per ounce of meth) will come in the first pull. (The poster is in the habit of letting the reaction fluid cool, adding a little more base to it, salting it a little, adding xylene, sealing the container, and letting it sit. He will return and extract from the xylene a day or two later, sometimes a week later. The second pull is usually worth doing, will yield an average of ten percent or so of the initial yield, and is usually used as fuel to power the cook through another reaction.)
For those who lack experience with the ker plunking technique, please read the intital thread, remember to use boiling stones or equivalent and do a second pull. Extract the second pull separately. You may come to the poster's conclusion about the need to do it twice. You should, however, satisfy yourself in this regard before deciding to skip a second pull.
A short synthesis of geezmeister's view of the Ker Plunk: (Not a rewriteup, nor a writeup, but some short notes on the process for the newbee too impatient to follow the links and read the whole thread.) You have you non-polar washed honey in a flask. A large Erhlenmeyer is fine, so is a coffee pot. Geez likes a white corningware coffee percolater pot, about ten inches deep and four in inner diameter. Regardless of you choice of vessel, add your honey. Add boiling stones, broken crockery, or washed coarse sand, and (do not overlook to do this under penalty of losing your whole batch to a big "bump," having a fire, bringing in the fire department who will notify law enforcement...get the picture....this is important!) Add VM&P naptha or Coleman's fuel or generic camp fuel. Naptha is the trick, here. Add heat slowly. As the reaction mixture starts to warm, you will notice gakk, if it is present, at the interface. If you have gakk, the heating itself will help, but you may also add a few drops at a time of peroxide. Three percent solution should be used, if any. There is dispute regarding whether this process is worth the time of trouble. No one has posted any side by side test results to determine whether it is or is not. HOWEVER, Geez says it never seemed to hurt, even when it was 35% H2O2, which should only be added by fools, idiots, and those who just like to see things violently bubble as if all hell were breaking loose. Some folks believe this assists in breaking down certain gakks. Results, at best, are inconclusive. Other thing one might care to add to the pot include a few drops of alcohol, supposedly to keep the NaOH you will add out of the non-polar, but since you are going to wash it later, this too appears to be an old wive's tale of unproven efficacy. Add sodium hydroxide. A little at a time. NaOH, RDL, whatever you wish to call it. If you add it dry, it will sink to the bottom and have a violent little reaction. It will also react when you stir it, and if you add too much--guess what--you can blow all the naptha right out of the pot. Other than just liking the reaction and activity, Geez sees little benefit in adding dry NaOH to the pot. He adds a 20% solution, a little at a time. He stirs after each addition. Let the heat come up slowly to where the rection fluid is just bubbling. All the while, add a little NaOH, a little more, a little more. You can measure the pH of the reaction fluid at each addition, every now and then, or not at all. Your choice. Geez likes to stop adding before it all gets milky and stays that way, and add some rock salt, a tablespoon or so, to the pot. No, no need to grind it up. It will dissolve. What doesn't is excess and will help prevent bumping. (As before, the addition of salt is a maybe yes, maybe no, old wive's tale sort of thing. Rock salt never seemed to hurt a thing. Table salt--that can be different, and you should avoid it since it probably has iodine in quantities too small to matter but anti-caking ingredients that may help emulsions form). Continue stirring, allow the temp of the naptha to rise. If you have a serious emulsion ( which is an indication your pseudo was less than clean) and it has not responded to anything else, add some ground activated charcoal. This will float to the interface layer. Stir, bring the temperature of the reaction fluid up to boiling slowly. Observe the convection currents in the reaction fluid maing the carbon roil in the pot. Keep it there at least five minutes. Then..while stirring add more NaOH a little at a time until you
have it right. How to tell you have it right: 1) measure the pH of the reaction fluid, and confirm that it is pH 12.8 or higher. Higher is likely better, just as a matter of being excessive about all things (the late appearance of orange gakk may have rendered excessively high pH counterproductive.) 1) watch the bottom layer go white, stay white and begin to elute small bubbles, like the fizz when you pour soda, only not so intense. 3) Smell the fish market smell and see the bubbles. This is Geez's method, since he is doing this in a non-glass pot.
Now, after you have it right, add just a bit more NaOH, let the bubbles really start eluting up, and turn the heat off. Leave it alone for at least fifteen minutes. When it finishes releasing the small bubbles to the non-polar layer and has cooled off a little bit, you are done. Decant or separate the naptha. If you wish to pull again (recommended) do so now. No need to add more of anything, just bring the naptha up to temp, let setle, and separate. Do three if you insist. With ker plunking, a third pull is usually a formality only.
Point of convergence For those of you who just returned here after steam distilling the freebase and have now dissolved it in non-polar solvent, you are where we are here, only with what is probably a cleaner mixture of meth and non-polar solvent. For the A/B er's, and the Ker Plunker's, we meet again at this point.
What to do with the reaction fluid. Pouring it out is not a viable solution. It is full of idodides. You can in fact recover I2 from the reaction fluid. It is there. It can be recovered.
Post 188836 (missing)
(Worlock: "Sodium Iodide recovery", Stimulants) If you do not care to do so, please take the time to neutralize the solution with acid, or at least dilute with lots of tap water, so as not to pollute the entire universe and give meth cooks a bad name with the DEQ.