by geezmeister
HTML by metanoid
The Post Reaction Workup:
This post assumes you have just completed an HI reduction of ephedrine or pseudoephedrine to methamphetamine. Perhaps you arrived here by the use of red phosphorous and iodine, whether by push-pull, balloon, or reflux methods; by hypophoshorous acid and iodine, open or closed, safe or unsafe; the phosphorous acid synth or by the use of HI alone or with a little red phosphorous added to keep the concentration where you want it. This writeup centers on the typical HI/ red Phosphorous reaction, and some of the comments do not apply to hypo or phosphorous acid synths. You have your honey, which is freebase meth in an acidic solution that is what is left of the precursors you started with, the meth produced, and the byproducts of the reaction. That's where this post starts.
Are you finished?: Your reaction flask is full of larger bubbles and those small ones you have watched for so long are missing. When you remove the flask from the heat, and the flask cools enough the contents cease boiling, you should see no small bubbling activity. If the smell you already recognize is present add some hot water to the flask. If you are not too sure about the smell, add a little hot water, careful not to flood the reaction out. (Geez adds as much hot water as there is fluid in the flask at this point if the smell is right.) The red phosphorous should fall out of the solution right away. When the flask cools just enough for the convection currents to cease, swirl the flask and watch how fast the red phosphorous falls to the bottom. If it stays in suspension or does not completetly settle, or if the red slowly drifts to the bottom and the fluid is reddish orange, put it back on the hot plate and let it cook some more. Hoping all you want that it is really finished will not help you at all if it is not. If the signs are not there, have patience and let the reaction continue until it completes.
If you swirl the flask and the red will settle falls to the bottom like bricks, your reaction should be considered as finished. The reaction fluid should ideally be almost clear, just a light tint of pale yellow. If can be dark gold, beer colored, or even bright piss yellow. Those colors tell you that contaminants are present. If the fluid is reddish-orange, but the red phosphorous falls like bricks to the bottom, you likely have an excess of iodine present in the reaction fluid. Some like to add a single crystal of sodium thiosulfate, which will rapidly clear the iodine from the solution. Sodium thiosulfate can also be found in the aquarium area of the big retail stores as a liquid used to remove chlorine from water. A drop if sufficient. You can also just let the fluid in the flask boil, condenser removed, for ten or fifteen mintues; this will clear excess iodine without using sodium thiosulfate.
Fine Filtering Dilute the fluid in the flask with an equal volume of hot dH2O. Swirl until the red is in the fluid and quickly pour the fluid through a filter. You will not get all the red phosphorous the first time. Add more water, swirl, repeat the process. You may find it helps to hold the flask upside down as you cease swirling (with a stopper in the opening of course) so the red phos will be washed out. Rinse the flask again with near-boiling water. Rinse the red phosphorous filtered out while it is in the filter with additional hot water. The goal of filtering is to get the red phosphorous out of the fluid. Some particles are very small and difficult to filter out without proper filter paper.
Filters that work: The preferred method is to use a Buchner funnel with vacuum, and if you have one, you know how to use it. If you do not have a Buchner funnel, take a funnel (do not crimp the process by using the smallest one you can find...be generous here...use one big enough to hold all of what you plan to filter if you can. Gravity filtration is usually done by pressing two or three cotton balls in the neck of the funnel (not too tightly, but tight enough to catch what red gets by the filters) and putting a fluted filter paper into the funnel. Wet any filter papers and cotton balls with water before pouring the honey into the filter. Coffee filters are an often used substittute for filter paper. The problem with coffee filters is that they are no fine enough for this job, and they trap some red phosphorous in the filter fibers. A fourth method (and Geez' personal favorite) is the "Charmin Plug." This is basically a tapered paper plug for the neck of the funnel, which can be compressed if needed to filter even finer and finer particles. To make a Charmin plug, take a single square of unscented Charmin toilet paper, fold it over itself lengthwise twice, or roll it up in a tube about a half inch wide, then roll it like joint. Roll it with a taper so one end is larger than the opening in the neck of the funnel. It should be 2 -3 cm long and a little thicker than the neck of the funnel. Press the rolled plug loosely into the neck of the funnel. Pour a little water through it and adjust the density of the plug by pushing it gently into the neck until you have a steady drip of water, one drop right after another. You can aedjust it for a fine, thin stream and often this will be perfect; the steady drip seems to remove more of the very fine fine particles or red phosphorous, however. Do not use a filter on top of this, and do not lay tissues flat in the bottom of the funnel.
The beauty of the Charmin plug is that the red phosphorous particles settle in the funnel and on the top of the plug, where it can be tapped into a big pile in a drying dish. Most of the red phosphorous on the plug can be wiped off the end of the plug; The first 3 or 4 mm of the plug will have red phosphorous embedded in it; tear this part of the plug off and save these in a jar. When the time comes to clean used red phosphorous with an acid bath, these can be added to the hot acid, which will destroy the paper and the paper fibers, leaving mainly a little ash and most of the red phosphorous. Dilute H2SO4 works very well for this. Geez usually saves the plugs until he is either out of red or has a full jar of plugs.
Never stir toilet paper with red phosphorous on it in water. Some folks like to lay a piece of Charmin flat in the funnel. Geez does not do this. You can only separate red phos from the paper when the paper is dry; you can do this with a soft brush very effectively. You cannot do it effectively from a whole sheet of paper. As this paper is made to fall apart in water, it does. It really does if you stir the water. This leaves all the fiber and its a big mess, and you do not want the paper fiber mixed with the red. It gets in the way and is a drag on the reaction. You can burn the paper out in an acid bath, but it is a better solution to avoid having to do so at all.
Swirl the contents of the flask and pour them into the funnel. You may need to add additional hot water to swirl, and reduce it to a small enough quantity that it can all be dumped in the funnel at one time. (Some prefer not to worry with getting the red phosphorous out of the flask at this point, and use sufficient water to rinse the methamphetamine from the red phosphorous. The red phosphorous is allowed to dry in the flask, where it may remain for the next reaction, or where it may be knocked loose and come out as powder. You need to know the clean weight of the flask if you plan to leave the phosphorous in the flask.)
When all your honey has dripped into the receiving flask, run it through the filter one more time. If you are using a Charmin Plug, use a new plug for this filtration. If not using a Charmin plug, filter through the red again. The additional filtering has benefits. Some of the red phosphorous is very fine, and you do want it out of your honey; the second filtration will get more red than you thought was in the fluid. If you filter through the red phosphorous already collection, you also filter out iodine in the fluid; likely not all of it, but some of it. The cleaner the better.
After the honey has filtered through the red phosphorous the second time, wash the red with very hot distilled water. Hot water seems to work better for this purpose than cool water. Wash until the unique meth smell is no longer present in the filters and red phosphorous, or at least until the smell is very faint. You do not want to unnecessarily thin the honey out so much the volume becomes a problem for the extraction, but you do want a much more dilute fluid than you have when the reaction completes. Diluting the reaction fluid it to about three times its original volume seems to work well. If you do not dilute at least that much, basing will produce too many solids and make the extraction difficult. Dilute much further than that and you make the extraction more difficult.
The Non-polar solvent wash of filtered honey. How do you wash honey? With a non-polar solvent. This step may be the one single most effective cleaning technique of the post reaction process. Skip it at your peril! Put the honey in a separatory funnel (or ghetto equivalent) and add an equal part of non-polar solvent. Choice of solvent is up to the individual, but Geez likes to use xylene for two such washes, hot naptha for one (since he extracts twice into naptha). He will shake the sep funnel with the solvent in it, not violently, but enough to mix it well. After shaking well, let the fluids settle and separate out the non-polar solvent. If you had a dirty reaction, you probalby picked up orange solids, trash, and cloudy masses of whatever that might happen to be-- do not be concerned--- you do not want this stuff. Your product is safely inside that aqueous reaction fluid and cannot be persuaded to jump to the non-polar until you base the solution and strip that salt off of the meth molecule. You are [i]not going to rinse the goods out with non-polar solvents. [/i] So, do it again. Any more trash come out? Do it again. In fact, keep doing it until the solvent is clean. You will most likely continue to see cloudy non-polar solvent with a yellowish coloration after such a wash. Wash until the solvent is clear. TCE is also very useful at this point. Use smaller volumes of TCE than you would other solvents; do not shake the sep funnel or you will have an emulsion that will need fifteen minutes or so the break down. Turning the funnel end to end slowly will do the job quite well.
If your honey was bright yellow, or if it was particularly dirty and the non-polar solvent continued to extract yellow tint from it, you have some contaminant like PEG in the fluid. Some bees will bring the honey to a boil in the flask with non-polar solvent present, and report that this appears to eliminate PEG. The logic behind boiling the contents of the flask is apparent. Hot solvents clean better and boiling the fluid makes certain there is enough convection in the flask to expose all the fluid to the solvent. Experience with pill extraction suggests five mintues is probably sufficient time for the non-polar to absorb what it will; if it is saturated with trash, one may always follow with another boil.
Which solvent to use? Geez suggests using an agressive solvent like xylene or tolulene; he has had a couple of bad experiences with odorless mineral spirits not separating from the honey and for that reason does not use mineral spirits for this purpose. Use the solvent you will extract the meth with at least once, and if it is used first, use it for two washes. Geez extracts with VM&P naptha most of the time, and always does at least one wash with hot naptha. Washing the reaction fluid with the solvent used to extract will remove anything in the fluid that is soluble in that solvent, which means it will not be in the fluid to be extracted with the meth. This logically translates to cleaner meth. If you plan to "ker plunk" -- or extract with hot naptha, Coleman's fuel, or equivalent-- wash with hot naptha, Coleman's fuel, or equivalent at least one time. Even if you will extract with naptha, this poster recommends washing the reaction fluid with tolulene or xylene prior to washing with naptha; there is no reason to use mineral spirits or naptha to wash if you will extract with tolulene or xylene, except for economic reasons.
Patience: when you do these washes, don't be in such a hurry you don't give the solvent time to work. Leave that first wash in the sep funnel for five or ten minutes after shaking the two together. The difference in what you find in the solvent after a short wait will convince you the wait is worth doing, and remind you that patience pays.
Steam distillation or solvent extraction? At this point you will proceed to do an acid/base extraction or steam distillation of the soon-to-be-freebase metamphetamine.
If you elect to steam distill, the chances are you are not reading this anyway, but if you are, refer to this excellent write-up of that procedure: VideoEditor: "Easiest Post Rxn Steam & Clean for RP/I " (Stimulants)
If you will do a conventional acid/base extraction, and are unfamiliar with acid/base extractions, please review the sticky thread: MaDMAx: "LOOK! Recrystallization and A/B general info" (Newbee Forum)
You may elect to do a variant of the acid/base extraction called "ker plunking:" Worlock: "Ker Plunking for quality and quantity" (Stimulants)
The acid/base extraction: Mister_Clean: "Time to learn about acids and bases" (Stimulants)
Transfer your reaction fluid in a separatory funnel (or ghetto equivalent). Add the non-polar solvent you have selected to use to extract the methamphetamine. The amount to use is dependent on the quantity of methamphetamine you will extract and on the characteristics of the solvent you will use. Standard procedure is to extract three times with equal volumes of solvent.
The volume of solvent is more dependent on the quantity of meth to extract rather than the volume of the reaction fluid, which includes the water used to rinse the flask, the red and the filters. Experience will give you a feel for it. For extractions of less than one ounce of expected methamphetamine, use at least three 200 ml volumes of solvent. Use 300 ml volumes if using naptha or mineral spirits. You want to use enough solvent to collect the freebase without fully saturating the solvent, but not so much that you make extraction of the methamphetamine from the non-polar solvent diffiuclt due to the volume of solvent itself. This poster will increase the volume of solvent by 100 ml per half ounce of anticipated methamphetamine yield. That is nothing more than his rule of thumb, based on his experience, and it will serve as a guide to you until you develop a feel for the volume you need. Frankly, the poster eyeballs how many glugs from the can are enough, and maintains that the volume can be too much, but is not as critical as you might think. There is a range of acceptable volumes. Try to hit the middle. Too little, you leave some product behind, too much you waste solvent and risk diluting the freebase so much you cannot recover it all. You can always extract another time, a fourth, or fifth time with non-polar solvent. The 200 ml volume is a suggestion applicable to naptha, coleman's fuel, charcoal lighter fluid, and xylene. TCE is a very effective solvent to extract freebase methamphetamine and does so with about half the volume of the other solvents mentioned. It is also much more expensive than the other solvents. Remember it will be the bottom layer in the sep funnel.
Basing the reaction fluid. Make a twenty percent solution of NaOH. This means fill a beaker on fifth full of NaOH, and fill it with water. Stir it until all the NaOH dissolves. Let it cool. (Do this before you begin filtering the red phosphorous from the reaction flask, and you will be fine. When its time to let the reaction fluid boil off any excess iodine, make up your solution if you have not already. You do not need cold NaOH solution. You simply want a solution that has dissolved and completed the reaction NaOH and water have, which is exothermic, and you want the resulting solution to have cooled to room temperature before using it.
You should have a separatory funnel (or ghetto equivalent) with the washed reaction fluid in it. Add the non-polar solvent chosen to extract the freebase methamphetamine unless you choose TCE. TCE should be added after the reaction fluid is based. The solids that form with basing have a habit of finding themselves in the TCE layer if it is present when the base is added. This does not seem to be a problem when the TCE is added after the base. Add the NaOH solution a little at a time. Pour it through the non-polar solvent. Swirl the solution after addition to distribute the NaOH. DO NOT SHAKE. Shaking just causes emulsions. You have no need to shake the solutions. Swirling is sufficient for all our purposes here. Watch the NaOH solution as it enters the reaction fluid. It will immediately turn milky white, then fade back into transparency. Add a little more NaOH. The same thing will happen. Continue this process, adding a little NaOH and swirling. Take some time and give it TLC. There is no reason to shock it with a massive dose-- you can if you want, sure. If you are new to A/B extractions, you will want to take repeated pH readings of the reaction fluid, which is the bottom layer unless you are extracting with TCE or DCM. The non-polar solvent has no pH. It tells you nothing to measure it, per se. You are concerned with the pH of the reaction fluid. Measure the pH of the reaction fluid with a meter, a pH test strip, cabbage juice, or--gasp---your sense of sight and smell. Yes, experience helps. To gain that knowledge from experience you must pay attention to sights and smells of the basing process.
Chemists will base to pH 12.8, the point at which methamphetamine HCl sheds that HCl and becomes freebase methamphetamine, which is non-polar soluble and insoluble in polar solutions. It will find it way to the non-polar solvent when the reaction fluid becomes pH 12.8 Add NaOH in increments until you reach pH 12.8, testing with your pH meter.
If you happen to be a cook instead of a chemist, are out of pH strips, have a meter that no longer works, or hate the smell of boiling red cabbage, you can simply base the reaction fluid until it is well above pH 12.8. Many cooks add base until the reaction fluid "lye locks." Lye lock is easily undone by the addition of a little more hot water. No real purpose is served by adding enough base to lock up, and it may decrease yield by preventing the methamphetamine from reaching the non-polar solvent.
When you first add a small splash of NaOH solution to the fluid it will turn the fluid milky where that splash mixes, then the fluid will clear again. Continue to add NaOH solution a little at a time until the reaction fluid goes milky and stays that way. Before it does, it will go milk white and stay that way for thirty seconds or so. You are almost there. The next addition of a few ml of NaOH solution will make it go white and stay white. You may even seen solids beginning to form. This is not a problem. SMELL THE FLASK. Smell that fish market smell? That is the smell of freebase amines. Learn to love it. When you smell that smell, you are right where you want to be, regardless of pH. You are getting the amines. That is what you are after. This is not to be confused with the lye smell, or the solvent smell. It is a distinctive smell of three day old dead fish. You will come to love that smell. When you have milky reaction fluid and smell the fish, your solution is at least at pH 12.8, and regardless of the precise measure, it is based strongly enough to freebase the methamphetamine HCl in the fluid.
Notes on Extracting the Meth into Nonpolar Solvents:
1) SWIRL, and DO NOT SHAKE. There is no reason to shake the based reaction fluid and the non-polar solvent together. The meth will migrate to the nonpolar as long as there is a clean interface and some movement of the fluid. Shaking form emulsions, these emulsions trap reaction fluid and methamphetamine freebase, keep it from migrating to the non-polar solvent, and blocks the interface between the polar and non-polar layers. This results in lower yield. Swirling is sufficient.
2) LET IT SIT. This is not an instant process, even though it does not take all night. After you hit the magic milky solution, give it fifteen minutes. Rule of thumb. Not that critical, but don't be in a big hurry. Give the meth time to migrate to the non-polar solution.
3) LATHER, RINSE, REPEAT. Separate out the nonpolar solvent. Save it in another container. Add fresh non-polar solvent to the separatory funnel (OGE), let it separate from the reaction fluid. Add a little more NaOH solution to make sure the fluid does not fall below 12.8. Chances are it will not. (Note: If you have reason to believe orange gakk is present, only add more base if the pH is below 12.8.) Swirl. Let the fluids sit together for awhile. Remember the last time. After the two layers separate completely, separate out the non-polar solvent. Combine with the first volume of solvent. Some cooks proceed at this point to a third pull with fresh solvent. Geez will add more solvent and leave the fluid for at least a day with the solvent. He gets a little better yield this way. If you do a third pull right away, you may get a small amount of product. If you let the fluid sit overnight, you can often double the amount. Patience pays.
4) SHOULD YOU ADD SALT? Many bees, Geez included, will add some table salt to the reaction fluid after basing. Add until no more dissolves, but no so much you clog the sep funnel with it. In theory water is more attracted to NaCl that methamphetamine HCl and will let go of the meth to get the salt. IS IT TRUE? Who knows? Does it hurt? Probably not, at least if you don't have emulsions. Should you use table salt? You can, but you are better served with pulverized rock salt which will not contain the anti-clogging additive. Better yet, use pickling salt which does not have the anti-clogging stuff in it. Table salt may contain iodine in very very small traces and does not present a real concern in this application. Does the salt actually increase the yield? I do not know. I have never split a batch into two equal volumes and extracted one with salt and one without.
5) DOING A THIRD PULL. A third pull should be done just like the first two were. Add more NaOH solution. Swirl. Let it sit. Geez lets this one sit overnight (at least) and sometimes a couple of days. You can shake this one if you want to, since its going to sit long enough for the emulsion to break down. You are extracting mostly the rogue, stubborn meth molecules that have not let go sooner, and you should expect this to take some time. You extracted the better part of your yield doing the first two extractions. What yield you get from a third pull is "extra" and it is the stuff that did not want to come easy Giving it more time makes sense. You may choose to save this and combine it with the next batch, or do it separately. Depends on how much of a tweaker you are.
6) WHAT TO DO WITH THE REACTION FLUID. Consider the reaction fluid spent after three pulls. Save it. Get a big plastic gas can, etc. and pour it in that can until the can is full. When the jug gets full, you can extract iodine from it. Geez usually gets about half his iodine back from the reaction fluid. [i][waste not, want not.) Whatever you do, keep everything until you have finished everything. That way, if you misplaced what you want, you still have it. Be patient, and do not hurry the process.
7) ON USING TCE TO EXTRACT METH. Geez notes that the bottom-puller TCE does an exceptionally good job of extracting freebase meth. It will do so cleanly if you have washed the reaction fluid with TCE prior to basing. If you omit the prebasing TCE wash, forget extracting with TCE. Use TCE if you gas; it does not titrate well. Add the TCE after you have based the reaction fluid. You can pour it in, but if it comes in a spray can, just direct the spray right into the based reaction fluid. Not much swirling required. TCE will make a emulsion of sorts but this does break down in ten to fifteen mintues in clean fluid. Give it this time. Do not base with the TCE present in the sep funnel. The NaOH solution will fall through the aqueous layer and into the TCE, the float back up. it tends to dump solids in the TCE layer when it does this. You will not have the problem if you add the TCE to the based reaction fluid.
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. 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 [i] (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. 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.
Extracting the meth from the non-polar solvent.
washing the solvent. Yes. Washing the solvent pays dividends. Use distilled water. (Yes, sure, you can actually use tap water or spring water or creek water if you want to...but distilled water is inexpensive and meth is not. So buy some distilled water and use that. Tap water will get you by if you must, but you run the risk of contamination with additives and minerals in the water. Your choice. Distilled water is seriously recommended here.) Put the non-polar solvent/meth solution in the separatory funnel (OGE) and add warm distilled water. Geez uses about a fourth as much water as he has non-polar solvent. Shake this as though your very life depended on it being shaken. Then let it sit. Remember the thing about patience? Here is another point where it will pay. Let the wash water settle out completely. The last stuff that falls out is the dirtiest you get. That is why you should wait about ten to fifteen minutes after the first wash, if you can make yourself. Separate out the rinse water, and save it. Add cool water, same quantity, and wash. Same shaking. Look at it as it settles. Feel it when you separate it out. If you continue to see cloudy material you need to continue washing. If it feels slick and oily, it still needs washing.
the lye solution washIf after these two washings the wash water is noticeably cloudy, or if the water is slick, you should proceed to do a lye wash. Use a pre-prepared twenty percent solution, one quarter the volume of the non-polar solution, and shake like hell again. Allow to settle, separate out, and follow at once with a warm distilled water wash. You will find the lye wash will clear sodium ions out the non-polar and will clean it of the lye remnants that may be in it from the A/B or ker plunk. Sounds like nonsense, works like magic. Do not be afraid of it, and remember NaOH is cheap compared to trash in your product.
brine wash A very good wash with much the same benefits as the lye solution wash is the brine wash...a wash with salt-saturated hot water. This wash also provides a benefit in helping dry the non-polar solvent if you will gas.
temperature of washes Geez does hot lye solution or hot brine solution first, warm water second, room temp water third. Why? Hell, he got in the habit of doing it that way for some reason. Seems to work. May even be some science to it, Geez does not know.
Cautions in washing. You can wash with water alone. Conventional wisdom is to never let the ph of the wash water fall below pH 9 or 10 while doing this, as you supposedly start losing product. Geez thinks this is nonsense, but never tosses out his rinse water until he finishes up and determines he did not, in fact, throw the baby out with the wash water. And he has done an A/B extraction of the rinse water alone and recovered more than a gram of meth from it (one ounce reaction). This says you can in fact wash out some of the goodies. So don't toss the wash water until you are through. Note that the use of NaOH solution wash will avoid the problem with the pH of the water falling, will rid the mix of NaOH residues and excess sodium ions, and make the washes more complete.
Now you are ready to extract. 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.
On Gassing: Dry your washed non-polar solvent and freebase meth solution before gassing. As to producing the gas, I recommend you review the following: hclgas.argox.html; hcl-gas.html; LaBTop: "Re: DETAILED METHODS for NON-CHEMISTS" (Newbee Forum) VideoEditor: "New Clean Gassing Method!" (Newbee Forum) Geez, when he gasses, uses the VideoEditor gassing apparatus as modified by Dwarfer...the Damp Rid/HCl generator with an aquarium airpump...and could not be happier with it. He gasses with the tip all the way down in the solution, since with this method there is no moisture or suck-back. He filters when the mix gets thoroughly cloudy but before is gets thick like applesauce. Part of this is his choice of solvents when he gasses (TCE) and its particular drying characteristics.
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.
On titrating Okay, so you can tell Geez primarily extracts his meth with aqueous HCl and evaporates. People who know a great deal more about chemistry than Geez call this method titration, which has to do in this instance with adding an acid to a basic solution in such a manner as to bring the pH of the solution to neutral, or slightly acidic pH. Your freebase methamphetaimine is dissolved in a non-polar solvent. Under basic conditions, methamphetamine will be and remain freebase, with no HCl molecule attached. Under neutral to acidic conditions it will bond with a HCl molecule and form a salt, which is water soluble. The methamphetamine HCl will disassociate from the non-polar solvent and dissolve in the aqueous HCl; this water/acid mixture is insoluble in the non-polar solvent, will separate from it in a layer that may drained from the separatory funnel, thus collecting the methamphetamine HCl in an aqueous solution.
The pH level is very important to chemists. It is also rather tricky, as the pH level at either end of the scale rises or drops at a different rate relative to the addition of the acid or base than it does in the middle range of the scale. It will take more acid to go from pH 13 to ph 10 than it will to go from ph 10 to ph 7. It takes little more than a drop to go from pH 7 to pH 5. Two drops more and the pH may fall to 3.
Geez always gets the feeling that pH 7 is like a street sign on a highway-- he's past it before he realizes it. In Geez's experience the meth does not take on the HCl neatly at pH 7.0, which is pretty much a good thing, for it did he would never have recovered his final product. It starts before you get to pH 7.0 and continues if you go below pH 7.0. MOST of it happens around pH 7.0. You want to get there. You can add water and do what the chemists do, which is add acid drop by drop, checking pH as it their lives and meth depended on it. This may be an advisable and worthwhile characteristic, but I suggest that it is an unnecessary one in this particular application. If you go overboard and get the pH way too low you will still get most of your product, you can clean it, and you can grow crystals. You are going to have some nasties in that last pull you would not otherwise have, sure...and you may cost yourself some yield. Geez has seen folks toss straight HCl in the non-polar solvent by the shotglass, shake it like hell, vent it to release pressure, shake some more, separate it out, and evaporate it. They get good product for the first two times they do it. Their third pull sure stinks, and the product from it is usually really dirty. These folks have never seen a pH strip, let alone a meter. WizardX gave some advice a long time back on this board to toss a few drops of HCl in water, toss it in the non-polar and shake well, then evaporate it. Keep evaporating each such pull by itself until you either get no more meth or the stuff you gets is so dirty its not worth messing with. Toss the dirty stuff back in the mix the next time around. It was sound advice, particularly for the cook without strips or a meter. It works. A never-measure-the-pH meth extraction. You can run into some cleanup problems if you toss that third pull in with the other two. In Geez' experience, that was where the dirty stuff came in, and is one of the reasons why he evaps the first two pulls separately from the last one. All the same, it works. The folks who toss in acid in by the shot glass wonder how Geez uses the same gallon of acid as long as he does. He agrees their product is on the same level as his...he just goes a hell of a lot easier on the acid. If they can pour it in like that, hitting the right pH is overemphasized.
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. Geez 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.
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.
Normally, you will collect the three volumes of non-polar solvent used to extract the meth from the reaction fluid, and will "pull" this three times with water and acid. It is not critical how much water you use. Use enough, but meth is so soluble in water that a ml of water per gram of meth is probably enough. Use more, get it all, do not try to collect it saturated. You will evaporate it anyway. On a one ounce batch-- where Geez expects 28 grams or so of meth, he extracts with three volumes of 125 ml each. He has done it with less, down to 50 ml, and more (which was a waste of time).
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. Geez likes 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 Geez again says 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. Geez suggests the easiest approach to not overshooting pH 6.8-7.0 is taking the advice of Worlock or WizardX 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.
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.
For tips on acetone flashing: geezmeister: "Re: Acetone Crashing" (Stimulants) While this post addresses flashing pseudoephedrine, it holds true for methamphetamine as well. Geez recommends 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.
There are a number of good threads on dual solvent recrystaliziation. The basic principle is to dissolve the methamphetamine HCl in boiling alcohol, filter through a fine filter to remove trash, reduce to saturation, and combine with another solvent such as dry acetone. Let the temperature fall slowly and give it some time and meth crystals will form. You will find these to be much cleaner than the meth you started with. A good descriptive writeup can be found in Chicken: "Step by Step Recrystallization of Meth" (Stimulants) although there are plenty of others.
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The object of this post was to do a basic, if fairly comprehensive, post-reaction workup post for meth cooks. I have no doubt omitted any and all information having to do with the question which prompted you to read this post in the first place. This is, of course, proof positive that the universe is as it is supposed to be, and that no good deed will go unpunished. For very long, at least. No doubt there are those among you who will take issue at part of this post, which is as it should be; I only intended by this post to centralize in some way the process of leaning for the new bee intent on making meth. If I have succeeded in that respect, I have accomplished what I sought to accomplish.----- Geez