Post-reaction Workup

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The post-reaction workup:A cook's essay on how to finish doing what you started.

by geezmeister

HTML by metanoid

The Post Reaction Workup:

This post assumes you have just completed an HI reduction of ephedrine orpseudoephedrine to methamphetamine. Perhaps you arrived here by the use ofred phosphorous and iodine, whether by push-pull, balloon, or reflux methods;by hypophoshorous acid and iodine, open or closed, safe or unsafe; thephosphorous acid synth or by the use of HI alone or with a little redphosphorous added to keep the concentration where you want it. This writeupcenters on the typical HI/ red Phosphorous reaction, and some of the commentsdo not apply to hypo or phosphorous acid synths. You have your honey, which isfreebase meth in an acidic solution that is what is left of the precursors youstarted with, the meth produced, and the byproducts of the reaction. That'swhere this post starts.

Are you finished?: Your reaction flask is full of larger bubbles and those smallones you have watched for so long are missing. When you remove the flask fromthe heat, and the flask cools enough the contents cease boiling, you should seeno small bubbling activity. If the smell you already recognize is present addsome hot water to the flask. If you are not too sure about the smell, add a littlehot water, careful not to flood the reaction out. (Geez adds as much hot water asthere is fluid in the flask at this point if the smell is right.) The red phosphorousshould fall out of the solution right away. When the flask cools just enough forthe convection currents to cease, swirl the flask and watch how fast the redphosphorous falls to the bottom. If it stays in suspension or does notcompletetly settle, or if the red slowly drifts to the bottom and the fluid isreddish orange, put it back on the hot plate and let it cook some more. Hopingall you want that it is really finished will not help you at all if it is not. If thesigns are not there, have patience and let the reaction continue until itcompletes.

HI Reduction Methamphetamine Workup - [www.... http://designer-drug.com/pte/12.162.180.114/dcd...

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If you swirl the flask and the red will settle falls to the bottom like bricks, yourreaction should be considered as finished. The reaction fluid should ideally bealmost clear, just a light tint of pale yellow. If can be dark gold, beer colored, oreven bright piss yellow. Those colors tell you that contaminants are present. Ifthe fluid is reddish-orange, but the red phosphorous falls like bricks to thebottom, you likely have an excess of iodine present in the reaction fluid. Somelike to add a single crystal of sodium thiosulfate, which will rapidly clear theiodine from the solution. Sodium thiosulfate can also be found in the aquariumarea of the big retail stores as a liquid used to remove chlorine from water. Adrop if sufficient. You can also just let the fluid in the flask boil, condenserremoved, for ten or fifteen mintues; this will clear excess iodine without usingsodium 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. Youwill not get all the red phosphorous the first time. Add more water, swirl, repeatthe process. You may find it helps to hold the flask upside down as you ceaseswirling (with a stopper in the opening of course) so the red phos will bewashed out. Rinse the flask again with near-boiling water. Rinse the redphosphorous filtered out while it is in the filter with additional hot water. Thegoal of filtering is to get the red phosphorous out of the fluid. Some particlesare very small and difficult to filter out without proper filter paper.

Filters that work: The preferred method is to use a Buchner funnel withvacuum, and if you have one, you know how to use it. If you do not have aBuchner funnel, take a funnel (do not crimp the process by using the smallestone you can find...be generous here...use one big enough to hold all of what youplan to filter if you can. Gravity filtration is usually done by pressing two orthree cotton balls in the neck of the funnel (not too tightly, but tight enough tocatch what red gets by the filters) and putting a fluted filter paper into thefunnel. Wet any filter papers and cotton balls with water before pouring thehoney 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, andthey 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 plugfor the neck of the funnel, which can be compressed if needed to filter evenfiner and finer particles. To make a Charmin plug, take a single square ofunscented Charmin toilet paper, fold it over itself lengthwise twice, or roll it upin a tube about a half inch wide, then roll it like joint. Roll it with a taper so oneend is larger than the opening in the neck of the funnel. It should be 2 -3 cmlong and a little thicker than the neck of the funnel. Press the rolled plug looselyinto the neck of the funnel. Pour a little water through it and adjust the densityof the plug by pushing it gently into the neck until you have a steady drip ofwater, one drop right after another. You can aedjust it for a fine, thin stream and


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often this will be perfect; the steady drip seems to remove more of the very finefine 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 inthe funnel and on the top of the plug, where it can be tapped into a big pile in adrying dish. Most of the red phosphorous on the plug can be wiped off the endof the plug; The first 3 or 4 mm of the plug will have red phosphorousembedded in it; tear this part of the plug off and save these in a jar. When thetime comes to clean used red phosphorous with an acid bath, these can beadded to the hot acid, which will destroy the paper and the paper fibers, leavingmainly a little ash and most of the red phosphorous. Dilute H2SO4 works verywell for this. Geez usually saves the plugs until he is either out of red or has afull jar of plugs.

Never stir toilet paper with red phosphorous on it in water. Some folks like tolay a piece of Charmin flat in the funnel. Geez does not do this. You can onlyseparate red phos from the paper when the paper is dry; you can do this with asoft brush very effectively. You cannot do it effectively from a whole sheet ofpaper. As this paper is made to fall apart in water, it does. It really does if youstir the water. This leaves all the fiber and its a big mess, and you do not wantthe paper fiber mixed with the red. It gets in the way and is a drag on thereaction. You can burn the paper out in an acid bath, but it is a better solutionto avoid having to do so at all.

Swirl the contents of the flask and pour them into the funnel. You may need toadd additional hot water to swirl, and reduce it to a small enough quantity thatit can all be dumped in the funnel at one time. (Some prefer not to worry withgetting the red phosphorous out of the flask at this point, and use sufficientwater to rinse the methamphetamine from the red phosphorous. The redphosphorous is allowed to dry in the flask, where it may remain for the nextreaction, or where it may be knocked loose and come out as powder. You needto know the clean weight of the flask if you plan to leave the phosphorous in theflask.)

When all your honey has dripped into the receiving flask, run it through thefilter one more time. If you are using a Charmin Plug, use a new plug for thisfiltration. If not using a Charmin plug, filter through the red again. Theadditional filtering has benefits. Some of the red phosphorous is very fine, andyou do want it out of your honey; the second filtration will get more red thanyou thought was in the fluid. If you filter through the red phosphorous alreadycollection, you also filter out iodine in the fluid; likely not all of it, but some of it.The cleaner the better.


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After the honey has filtered through the red phosphorous the second time, washthe red with very hot distilled water. Hot water seems to work better for thispurpose than cool water. Wash until the unique meth smell is no longer presentin the filters and red phosphorous, or at least until the smell is very faint. Youdo not want to unnecessarily thin the honey out so much the volume becomes aproblem for the extraction, but you do want a much more dilute fluid than youhave when the reaction completes. Diluting the reaction fluid it to about threetimes its original volume seems to work well. If you do not dilute at least thatmuch, 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 effectivecleaning technique of the post reaction process. Skip it at your peril! Put thehoney in a separatory funnel (or ghetto equivalent) and add an equal part ofnon-polar solvent. Choice of solvent is up to the individual, but Geez likes to usexylene for two such washes, hot naptha for one (since he extracts twice intonaptha). He will shake the sep funnel with the solvent in it, not violently, butenough to mix it well. After shaking well, let the fluids settle and separate outthe non-polar solvent. If you had a dirty reaction, you probalby picked uporange 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 insidethat aqueous reaction fluid and cannot be persuaded to jump to the non-polaruntil 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 isclean. You will most likely continue to see cloudy non-polar solvent with ayellowish coloration after such a wash. Wash until the solvent is clear. TCE isalso very useful at this point. Use smaller volumes of TCE than you would othersolvents; do not shake the sep funnel or you will have an emulsion that will needfifteen minutes or so the break down. Turning the funnel end to end slowly willdo the job quite well.

If your honey was bright yellow, or if it was particularly dirty and the non-polarsolvent continued to extract yellow tint from it, you have some contaminant likePEG in the fluid. Some bees will bring the honey to a boil in the flask withnon-polar solvent present, and report that this appears to eliminate PEG. Thelogic behind boiling the contents of the flask is apparent. Hot solvents cleanbetter and boiling the fluid makes certain there is enough convection in theflask to expose all the fluid to the solvent. Experience with pill extractionsuggests five mintues is probably sufficient time for the non-polar to absorbwhat it will; if it is saturated with trash, one may always follow with anotherboil.


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Which solvent to use? Geez suggests using an agressive solvent like xylene ortolulene; he has had a couple of bad experiences with odorless mineral spiritsnot separating from the honey and for that reason does not use mineral spiritsfor 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 napthamost of the time, and always does at least one wash with hot naptha. Washingthe reaction fluid with the solvent used to extract will remove anything in thefluid that is soluble in that solvent, which means it will not be in the fluid to beextracted with the meth. This logically translates to cleaner meth. If you planto "ker plunk" -- or extract with hot naptha, Coleman's fuel, or equivalent-- washwith hot naptha, Coleman's fuel, or equivalent at least one time. Even if you willextract with naptha, this poster recommends washing the reaction fluid withtolulene or xylene prior to washing with naptha; there is no reason to usemineral 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 thesolvent time to work. Leave that first wash in the sep funnel for five or tenminutes after shaking the two together. The difference in what you find in thesolvent after a short wait will convince you the wait is worth doing, and remindyou that patience pays.

Steam distillation or solvent extraction? At this point you will proceed to doan acid/base extraction or steam distillation of the soon-to-be-freebasemetamphetamine.

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 withacid/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 andbases" (Stimulants)

Transfer your reaction fluid in a separatory funnel (or ghetto equivalent). Addthe non-polar solvent you have selected to use to extract the methamphetamine.The amount to use is dependent on the quantity of methamphetamine you willextract and on the characteristics of the solvent you will use. Standardprocedure is to extract three times with equal volumes of solvent.


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The volume of solvent is more dependent on the quantity of meth to extractrather than the volume of the reaction fluid, which includes the water used torinse the flask, the red and the filters. Experience will give you a feel for it. Forextractions of less than one ounce of expected methamphetamine, use at leastthree 200 ml volumes of solvent. Use 300 ml volumes if using naptha or mineralspirits. You want to use enough solvent to collect the freebase without fullysaturating the solvent, but not so much that you make extraction of themethamphetamine from the non-polar solvent diffiuclt due to the volume ofsolvent itself. This poster will increase the volume of solvent by 100 ml per halfounce of anticipated methamphetamine yield. That is nothing more than his ruleof thumb, based on his experience, and it will serve as a guide to you until youdevelop a feel for the volume you need. Frankly, the poster eyeballs how manyglugs 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 youwaste 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-polarsolvent. 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 extractfreebase methamphetamine and does so with about half the volume of theother solvents mentioned. It is also much more expensive than the othersolvents. Remember it will be the bottom layer in the sep funnel.

Basing the reaction fluid. Make a twenty percent solution of NaOH. Thismeans fill a beaker on fifth full of NaOH, and fill it with water. Stir it until all theNaOH dissolves. Let it cool. (Do this before you begin filtering the redphosphorous from the reaction flask, and you will be fine. When its time to letthe reaction fluid boil off any excess iodine, make up your solution if you havenot already. You do not need cold NaOH solution. You simply want a solutionthat has dissolved and completed the reaction NaOH and water have, which isexothermic, and you want the resulting solution to have cooled to roomtemperature before using it.

You should have a separatory funnel (or ghetto equivalent) with the washedreaction fluid in it. Add the non-polar solvent chosen to extract the freebasemethamphetamine unless you choose TCE. TCE should be added after thereaction fluid is based. The solids that form with basing have a habit of findingthemselves in the TCE layer if it is present when the base is added. This doesnot seem to be a problem when the TCE is added after the base. Add the NaOHsolution a little at a time. Pour it through the non-polar solvent. Swirl thesolution after addition to distribute the NaOH. DO NOT SHAKE. Shaking justcauses emulsions. You have no need to shake the solutions. Swirling is sufficientfor all our purposes here. Watch the NaOH solution as it enters the reactionfluid. It will immediately turn milky white, then fade back into transparency.


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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 noreason to shock it with a massive dose-- you can if you want, sure. If you arenew to A/B extractions, you will want to take repeated pH readings of thereaction fluid, which is the bottom layer unless you are extracting with TCE orDCM. The non-polar solvent has no pH. It tells you nothing to measure it, perse. You are concerned with the pH of the reaction fluid. Measure the pH of thereaction fluid with a meter, a pH test strip, cabbage juice, or--gasp---your senseof sight and smell. Yes, experience helps. To gain that knowledge fromexperience 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 shedsthat HCl and becomes freebase methamphetamine, which is non-polar solubleand insoluble in polar solutions. It will find it way to the non-polar solvent whenthe reaction fluid becomes pH 12.8 Add NaOH in increments until you reachpH 12.8, testing with your pH meter.

If you happen to be a cook instead of a chemist, are out of pH strips, have ameter that no longer works, or hate the smell of boiling red cabbage, you cansimply base the reaction fluid until it is well above pH 12.8. Many cooks addbase until the reaction fluid "lye locks." Lye lock is easily undone by the additionof a little more hot water. No real purpose is served by adding enough base tolock up, and it may decrease yield by preventing the methamphetamine fromreaching the non-polar solvent.

When you first add a small splash of NaOH solution to the fluid it will turn thefluid milky where that splash mixes, then the fluid will clear again. Continue toadd NaOH solution a little at a time until the reaction fluid goes milky and staysthat way. Before it does, it will go milk white and stay that way for thirtyseconds or so. You are almost there. The next addition of a few ml of NaOHsolution will make it go white and stay white. You may even seen solidsbeginning to form. This is not a problem. SMELL THE FLASK. Smell that fishmarket smell? That is the smell of freebase amines. Learn to love it. When yousmell that smell, you are right where you want to be, regardless of pH. You aregetting the amines. That is what you are after. This is not to be confused withthe lye smell, or the solvent smell. It is a distinctive smell of three day old deadfish. You will come to love that smell. When you have milky reaction fluid andsmell the fish, your solution is at least at pH 12.8, and regardless of the precisemeasure, it is based strongly enough to freebase the methamphetamine HCl inthe fluid.

Notes on Extracting the Meth into Nonpolar Solvents:

1) SWIRL, and DO NOT SHAKE. There is no reason to shake the based reactionfluid and the non-polar solvent together. The meth will migrate to the nonpolar


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as long as there is a clean interface and some movement of the fluid. Shaking form emulsions, these emulsions trap reaction fluid and methamphetaminefreebase, keep it from migrating to the non-polar solvent, and blocks theinterface 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 allnight. After you hit the magic milky solution, give it fifteen minutes. Rule ofthumb. Not that critical, but don't be in a big hurry. Give the meth time tomigrate to the non-polar solution.

3) LATHER, RINSE, REPEAT. Separate out the nonpolar solvent. Save it inanother 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 makesure the fluid does not fall below 12.8. Chances are it will not. (Note: If youhave reason to believe orange gakk is present, only add more base if the pH isbelow 12.8.) Swirl. Let the fluids sit together for awhile. Remember the lasttime. After the two layers separate completely, separate out the non-polarsolvent. Combine with the first volume of solvent. Some cooks proceed at thispoint to a third pull with fresh solvent. Geez will add more solvent and leave thefluid for at least a day with the solvent. He gets a little better yield this way. Ifyou do a third pull right away, you may get a small amount of product. If you letthe fluid sit overnight, you can often double the amount. Patience pays.

4) SHOULD YOU ADD SALT? Many bees, Geez included, will add some tablesalt to the reaction fluid after basing. Add until no more dissolves, but no somuch you clog the sep funnel with it. In theory water is more attracted to NaClthat methamphetamine HCl and will let go of the meth to get the salt. IS ITTRUE? Who knows? Does it hurt? Probably not, at least if you don't haveemulsions. Should you use table salt? You can, but you are better served withpulverized 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 saltmay contain iodine in very very small traces and does not present a realconcern in this application. Does the salt actually increase the yield? I do notknow. I have never split a batch into two equal volumes and extracted one withsalt and one without.

5) DOING A THIRD PULL. A third pull should be done just like the first twowere. 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 areextracting mostly the rogue, stubborn meth molecules that have not let gosooner, and you should expect this to take some time. You extracted the betterpart of your yield doing the first two extractions. What yield you get from a


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third pull is "extra" and it is the stuff that did not want to come easy Giving itmore time makes sense. You may choose to save this and combine it with thenext 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 fluidspent after three pulls. Save it. Get a big plastic gas can, etc. and pour it in thatcan 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][wastenot, want not.) Whatever you do, keep everything until you have finishedeverything. That way, if you misplaced what you want, you still have it. Bepatient, and do not hurry the process.

7) ON USING TCE TO EXTRACT METH. Geez notes that the bottom-puller TCEdoes an exceptionally good job of extracting freebase meth. It will do so cleanlyif you have washed the reaction fluid with TCE prior to basing. If you omit theprebasing TCE wash, forget extracting with TCE. Use TCE if you gas; it doesnot titrate well. Add the TCE after you have based the reaction fluid. You canpour it in, but if it comes in a spray can, just direct the spray right into thebased reaction fluid. Not much swirling required. TCE will make a emulsion ofsorts but this does break down in ten to fifteen mintues in clean fluid. Give itthis time. Do not base with the TCE present in the sep funnel. The NaOHsolution 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 theproblem if you add the TCE to the based reaction fluid.

IF THINGS HAVE GONE WELL TO THIS POINT, YOU OBVIOUSLY AREDREAMING-- OR HOW TO HANDLE COMMON PROBLEMS YOU MAYENCOUNTER BY THIS TIME.

Any number of misfortunes could have befallen the cook by this time. Theprincipal problems Geez is personally familiar with are:

EMULSIONS: There is no single source of emulsions. Some are caused byadulterants in the precursors, some may be caused by anti-caking additives intable salt, some may be caused by ingredients added to NaOH in OTC lyepreparations. Some are caused by residues on the glassware, including tracesof soaps or detergents. Some emulsions are nothing more than the result ofshaking oil and water together. The most common cause of emulsions isinadequate cleaning of the precursors, particularly pseudo. Using an effectiveextraction technique suited to the source of the precursor is the first linedefense against emulsions. Recrystalizing the pseudo twice before reacting alsotend to remove impurities and make emulsions less likely. Using NaOH solutionrather than dry NaOH to base also helps avoid emulsions.

Other preventive measures include using rock salt or pickling salt (rather than


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table salt). Not using soap or detergent to clean the glassware, and rinsingglassware with acetone after washing help limit the incidence of emulsions. The next best preventive measure is to avoid shaking the polar and non polarlayers togeher. Swirling is sufficient. Stirring is permissible. Shaking is askingfor emulsions. Period. You do not need to shake.

Combatting emulsions:. There are several ways to combat emulsions. Thefirst is to let it just sit there until the emulsion goes away. Another is to take astick and poke at the bubbles. This works only if you are sufficiently wired towant to do this for twelve hours. Another is to add additional non-polarsolvent and stir. You may also add a small volume of acetone to the solutionand stir. This may be exciting...it may effervesce as you add it. It may donothing. You may also add a little TCE while stirring. This will quickly settle tothe bottom, but has been reported in certain circumstances to have an effect ofbreaking an emulsion. The most likely successful method if waiting alone doesnot work is to pour all of the reaction fluid, emulsion and non-polar solvent intoa 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 thenon-polar solvent to heat up. While doing this, it may help to salt the emulsionwith ground rock salt. It may help to add a few drops of hydrogen peroxidethe 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 thancause the non-polar solution to bubble out of the flask, but is a diversion towatch. While heating, add some boiling stones, broken clay pot pieces, orwashed coarse sand to the flask to keep it from forming bubbles so large as todisplace the volume of the container and spray you with the meth-ladennon-polar solution, rendering all of your efforts a complete waste. Thisphenomenon is referred to as bumping. Do not let it destroy your day. It issimple to avoid. One final suggestion, used on one occasion by the posterhelping a friend out of a jam, is to finely powder activated carbon and add thisto 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 willappear that the carbon is blocking any meth from coming to the surface, but asthe convection currents in the flask increase the carbon will beging to swirl onthe top layer, and you will be able to see into the reaction fluid layer. Boil for tenminutes or so after it reaches this point, the let the mixture cool. Separate outthe non-polar solution. This worked quite well when the emulsion present wassuspected to be related to glycol and cellulose that was contained in thepseudoephedrine being used.

If none of the above work, suicide is an effective solution, as is starting overwith clean precursors.

Lye lock and other such ideas Lye lock is the state which the reaction fluid


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reaches when the cooling reaction fluid is saturated with NaOH and thickens.The author has experienced something along this line once or twice. If youencounter 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. Strangerthings have happened. Add more water, add more NaOH solution. That is all. Ifyou can acidify the based reaction fluid to recover I2, you can base the acid inthe reaction fluid to raise the pH.

Ker Plunking -- the variation on the Acid/Base extraction. Worlock: "KerPlunking for quality and quantity" (Stimulants)

Ker Plunking-- whether it is all that it is advertised to be or not-- does in factprovide an efficient way to perform an acid/base extraction ofmethamphetamine from the reaction fluid. While it is principally a way ofheating the naptha used to collect the meth freebase to increase its solvency,the process also entails heating to combat emulsions, and a slow basing processwhich allows one to watch the process and visually determine that the freebaseis eluting to the non-polar solvent, and to maximize that process by cues derivedfrom the addition of base, salt, stirring, and heating. When the bubbles areeluting and are obvious and numerous, stop addition, turn the heat off an waitfifteen minutes. Separate the naptha from the reaction fluid. In the poster'sexperience, your yield, if you did this properly and with sufficient naptha (counton 500 ml per ounce of meth) will come in the first pull. (The poster is in thehabit of letting the reaction fluid cool, adding a little more base to it, salting it alittle, adding xylene, sealing the container, and letting it sit. He will return andextract from the xylene a day or two later, sometimes a week later. The secondpull is usually worth doing, will yield an average of ten percent or so of theinitial yield, and is usually used as fuel to power the cook through anotherreaction.)

For those who lack experience with the ker plunking technique, please read theintital thread, remember to use boiling stones or equivalent and do a secondpull. Extract the second pull separately. You may come to the poster'sconclusion about the need to do it twice. You should, however, satisfy yourself inthis 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 tooimpatient to follow the links and read the whole thread.) You have younon-polar washed honey in a flask. A large Erhlenmeyer is fine, so is a coffeepot. Geez likes a white corningware coffee percolater pot, about ten inches deepand 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


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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 lawenforcement...get the picture....this is important!) Add VM&P naptha orColeman'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, atthe interface. If you have gakk, the heating itself will help, but you may also adda 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. Noone 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 thingsviolently bubble as if all hell were breaking loose. Some folks believe this assistsin breaking down certain gakks. Results, at best, are inconclusive. Other thingone might care to add to the pot include a few drops of alcohol, supposedly tokeep the NaOH you will add out of the non-polar, but since you are going towash it later, this too appears to be an old wive's tale of unproven efficacy. Addsodium hydroxide. A little at a time. NaOH, RDL, whatever you wish to call it. Ifyou add it dry, it will sink to the bottom and have a violent little reaction. It willalso react when you stir it, and if you add too much--guess what--you can blowall the naptha right out of the pot. Other than just liking the reaction andactivity, 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 upslowly to where the rection fluid is just bubbling. All the while, add a littleNaOH, a little more, a little more. You can measure the pH of the reaction fluidat each addition, every now and then, or not at all. Your choice. Geez likes tostop adding before it all gets milky and stays that way, and add some rock salt, atablespoon or so, to the pot. No, no need to grind it up. It will dissolve. Whatdoesn't is excess and will help prevent bumping. (As before, the addition of saltis a maybe yes, maybe no, old wive's tale sort of thing. Rock salt never seemedto hurt a thing. Table salt--that can be different, and you should avoid it since itprobably has iodine in quantities too small to matter but anti-caking ingredientsthat may help emulsions form). Continue stirring, allow the temp of the napthato rise. If you have a serious emulsion ( which is an indication your pseudo wasless than clean) and it has not responded to anything else, add some groundactivated charcoal. This will float to the interface layer. Stir, bring thetemperature of the reaction fluid up to boiling slowly. Observe the convectioncurrents in the reaction fluid maing the carbon roil in the pot. Keep it there atleast five minutes. Then..while stirring add more NaOH a little at a time untilyou have it right.

How to tell you have it right: 1) measure the pH of the reaction fluid, andconfirm that it is pH 12.8 or higher. Higher is likely better, just as a matter ofbeing excessive about all things (the late appearance of orange gakk may haverendered excessively high pH counterproductive.) 1) watch the bottom layer go


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white, stay white and begin to elute small bubbles, like the fizz when you poursoda, 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 reallystart 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 hascooled off a little bit, you are done. Decant or separate the naptha. If you wishto pull again (recommended) do so now. No need to add more of anything, justbring the naptha up to temp, let setle, and separate. Do three if you insist. Withker plunking, a third pull is usually a formality only.

Point of convergence For those of you who just returned here after steamdistilling the freebase and have now dissolved it in non-polar solvent, you arewhere we are here, only with what is probably a cleaner mixture of meth andnon-polar solvent. For the A/B er's, and the Ker Plunker's, we meet again at thispoint.

What to do with the reaction fluid. Pouring it out is not a viable solution. It isfull of idodides. You can in fact recover I2 from the reaction fluid. It is there. Itcan be recovered. Worlock: "Sodium Iodide recovery" (Stimulants) If you do notcare to do so, please take the time to neutralize the solution with acid, or atleast dilute with lots of tap water, so as not to pollute the entire universe andgive 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 distilledwater. (Yes, sure, you can actually use tap water or spring water or creek waterif you want to...but distilled water is inexpensive and meth is not. So buy somedistilled water and use that. Tap water will get you by if you must, but you runthe risk of contamination with additives and minerals in the water. Your choice.Distilled water is seriously recommended here.) Put the non-polar solvent/methsolution in the separatory funnel (OGE) and add warm distilled water. Geez usesabout a fourth as much water as he has non-polar solvent. Shake this as thoughyour very life depended on it being shaken. Then let it sit. Remember the thingabout patience? Here is another point where it will pay. Let the wash watersettle out completely. The last stuff that falls out is the dirtiest you get. That iswhy you should wait about ten to fifteen minutes after the first wash, if you canmake yourself. Separate out the rinse water, and save it. Add cool water, samequantity, and wash. Same shaking. Look at it as it settles. Feel it when youseparate it out. If you continue to see cloudy material you need to continuewashing. If it feels slick and oily, it still needs washing.

the lye solution washIf after these two washings the wash water is noticeably


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cloudy, or if the water is slick, you should proceed to do a lye wash. Use apre-prepared twenty percent solution, one quarter the volume of the non-polarsolution, and shake like hell again. Allow to settle, separate out, and follow atonce with a warm distilled water wash. You will find the lye wash will clearsodium ions out the non-polar and will clean it of the lye remnants that may bein it from the A/B or ker plunk. Sounds like nonsense, works like magic. Do notbe afraid of it, and remember NaOH is cheap compared to trash in yourproduct.

brine wash A very good wash with much the same benefits as the lye solutionwash is the brine wash...a wash with salt-saturated hot water. This wash alsoprovides 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 ofdoing it that way for some reason. Seems to work. May even be some science toit, Geez does not know.

Cautions in washing. You can wash with water alone. Conventional wisdomis 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 nevertosses 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 ofthe rinse water alone and recovered more than a gram of meth from it (oneounce reaction). This says you can in fact wash out some of the goodies. Sodon't toss the wash water until you are through. Note that the use of NaOHsolution wash will avoid the problem with the pH of the water falling, will ridthe mix of NaOH residues and excess sodium ions, and make the washes morecomplete.

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 toaccumulate hydrogen chloride gas in alcohol, and add that to the non-polar. Theauthor has never observed this method, let alone used it, and if you areinterested, you will have to UTFSE.

On Gassing: Dry your washed non-polar solvent and freebase meth solutionbefore gassing. As to producing the gas, I recommend you review the following:http://www.rhodium.ws/chemistry/hclgas.argox.html; http://www.rhodium.ws/chemistry/hcl-gas.html; LaBTop: "Re: DETAILED METHODS forNON-CHEMISTS" (Newbee Forum) VideoEditor: "New Clean Gassing Method!"(Newbee Forum) Geez, when he gasses, uses the VideoEditor gassing apparatusas modified by Dwarfer...the Damp Rid/HCl generator with an aquariumairpump...and could not be happier with it. He gasses with the tip all the waydown in the solution, since with this method there is no moisture or suck-back.


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He filters when the mix gets thoroughly cloudy but before is gets thick likeapplesauce. Part of this is his choice of solvents when he gasses (TCE) and itsparticular drying characteristics.

Gassing is usually performed by placing the tip of the hose or wand from thegas generator just a fraction of an inch above the surface of the non-polarsolvent, so that the gas being emitted contacts the surface of the non-polarsolvent and the force of the gas flow pushes it down slightly. Bubblng the gasthrough the solvent is advocated by some proponents of gassing andcondemned by others. The non-polar solvent may, but will not necessarily snowcrystals. 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 willdisappear 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 withaqueous HCl and evaporates. People who know a great deal more aboutchemistry than Geez call this method titration, which has to do in this instancewith adding an acid to a basic solution in such a manner as to bring the pH ofthe solution to neutral, or slightly acidic pH. Your freebase methamphetaimineis dissolved in a non-polar solvent. Under basic conditions, methamphetaminewill be and remain freebase, with no HCl molecule attached. Under neutral toacidic conditions it will bond with a HCl molecule and form a salt, which iswater soluble. The methamphetamine HCl will disassociate from the non-polarsolvent and dissolve in the aqueous HCl; this water/acid mixture is insoluble inthe non-polar solvent, will separate from it in a layer that may drained from theseparatory funnel, thus collecting the methamphetamine HCl in an aqueoussolution.

The pH level is very important to chemists. It is also rather tricky, as the pHlevel at either end of the scale rises or drops at a different rate relative to theaddition of the acid or base than it does in the middle range of the scale. It willtake more acid to go from pH 13 to ph 10 than it will to go from ph 10 to ph 7. Ittakes little more than a drop to go from pH 7 to pH 5. Two drops more and thepH may fall to 3.

Geez always gets the feeling that pH 7 is like a street sign on a highway-- he'spast it before he realizes it. In Geez's experience the meth does not take on theHCl neatly at pH 7.0, which is pretty much a good thing, for it did he wouldnever have recovered his final product. It starts before you get to pH 7.0 andcontinues if you go below pH 7.0. MOST of it happens around pH 7.0. You wantto get there. You can add water and do what the chemists do, which is add aciddrop by drop, checking pH as it their lives and meth depended on it. This may


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be an advisable and worthwhile characteristic, but I suggest that it is anunnecessary one in this particular application. If you go overboard and get thepH way too low you will still get most of your product, you can clean it, and youcan grow crystals. You are going to have some nasties in that last pull youwould not otherwise have, sure...and you may cost yourself some yield. Geezhas seen folks toss straight HCl in the non-polar solvent by the shotglass, shakeit like hell, vent it to release pressure, shake some more, separate it out, andevaporate it. They get good product for the first two times they do it. Their thirdpull sure stinks, and the product from it is usually really dirty. These folks havenever seen a pH strip, let alone a meter. WizardX gave some advice a long timeback on this board to toss a few drops of HCl in water, toss it in the non-polarand shake well, then evaporate it. Keep evaporating each such pull by itselfuntil you either get no more meth or the stuff you gets is so dirty its not worthmessing with. Toss the dirty stuff back in the mix the next time around. It wassound advice, particularly for the cook without strips or a meter. It works. Anever-measure-the-pH meth extraction. You can run into some cleanupproblems 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 evapsthe first two pulls separately from the last one. All the same, it works. The folkswho toss in acid in by the shot glass wonder how Geez uses the same gallon ofacid as long as he does. He agrees their product is on the same level as his...hejust goes a hell of a lot easier on the acid. If they can pour it in like that, hittingthe right pH is overemphasized.

Newbees probably should not leave it to chance. I do not recommend that younever use pH strips or a meter, that you never learn how to boil red cabbageand use the extract. Those are all wise things to do. All the same, no newbeeshould despair when his water in that non-polar he extracted his honey withsuddenly bottoms out on the pH scale. Geez learned the how-to part of it beforehe ever got acquainted with pH strips that measured high enough, ever had pHmeter, or ever boiled red cabbage. There are sights and smells and pressuresand changes you note to tell there is enough. It is not a life or death game of pHlevels 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 alot like any AB process: you get a feel for it, a touch, a nose, whatever--- youlearn 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 byexperience that dry acetone can be your best friend and that acetone jar yousave your rinsew acetone in your salvation when you overdo it. That isn'tchemist 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 andpour 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.


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Shake it like it meant something, because it does. Drain this out and evaporateit separately. Hey, so what if the pH is 8. You will already have some meth. Addanother batch of water and acid, the pH falls more, you get more meth in thenext pull. This is why most folks get the bigger yield on the second pull-- theyhave finally neutralized the mix.

Normally, you will collect the three volumes of non-polar solvent used to extractthe meth from the reaction fluid, and will "pull" this three times with water andacid. It is not critical how much water you use. Use enough, but meth is sosoluble in water that a ml of water per gram of meth is probably enough. Usemore, 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 extractswith three volumes of 125 ml each. He has done it with less, down to 50 ml, andmore (which was a waste of time).

It is very important to shake each volume of aqueous HCl in the non-polar asthough your life depended on it. Chanting and speaking incantations areregarded by chemists as primative superstitions and by meth cooks ashumorous ways of passing off the tedium of shaking the solution. Try chantingsome time, it might surprise you how well it works. Chemists like to collectthese three volumes of water/acid and evaporate them. Geez likes to combinethe first two and evaporate them, then evaporate the third one separately. Hedoes this because he frequently gets too low on the pH, has some extra nastiesin the last extraction, and likes to save steps cleaning most of his product. Thefirst 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 thecrop 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 addwater, base it with NaOH and send it back to fresh non-polar solvent, and do itagain, but the chances are you will lose product in the process and will have alower yield than you would if you just cleaned the product you obtain. If youmust hit it just perfect, do this. Understand, you really are placing the pH in aneutral position to allow the freebase to bond with the HCl molecule. When youevaporate the water/acid solution, you are going to concentrate the acidanyway. It is not that acidity hurts the meth HCl, it does not. It may introduceother contaminants to the water mix. These will need to be cleaned, but this isnot difficult to do. Geez suggests the easiest approach to not overshooting pH6.8-7.0 is taking the advice of Worlock or WizardX to use larger batches ofwater, add a little acid to each batch, and do multiple pulls (five or more) andevaporate each separately. You will know when you fell below pH 7.0, as theodor of evaporating HCl will burn your nostrils and you will learn the value of afume hood. You will also find that if you follow this method, your chances ofcontaminating the whole batch with some nasty creation that resulted from


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over-basing the mix are much reduced.

Evaporating This should be done on low heat, in a visionware bowl, or flatpyrex dish, on a hotplate or with heat lamps, with an exhaust fan exhaustingfumes to the outdoors, and with a fan blowing over the top of the dish. Toomuch heat will result in loss of yield as some of the meth vaporizes with theheat. Patience pays. If you have to have some now, evaporate that first pull byitself, 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 onthe sides of the dish. Before it is completely dry, flood the dish with driedacetone. This technique is called "acetone flashing" and will not only rid thedish of its remaining water content, it will precipitate methamphetamine hclcrystals in the acetone.

For tips on acetone flashing: geezmeister: "Re: Acetone Crashing" (Stimulants)While this post addresses flashing pseudoephedrine, it holds true formethamphetamine as well. Geez recommends letting the bowl settle down andcool down, then slyly tilting the pan so the meth stays in one place and theacetone slips to another. Then you can just pour the acetone into a beaker, andnot have to pour it through a filter. Filters absorb a lot of product. If you mustuse 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 gravityfilter. 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 theacetone aside, leave the meth in the glass dish to dry. If the meth is anythingother than sparkling and white, rinse the meth in fresh acetone. Do this in thedish if you have panned the meth to one side, or rinse the meth in the filter withfresh dry acetone. Do dry the acetone before use, and do save all the rinseacetone-- 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 thefreezer. You can add the acetone used to rinse to this. Give this time to chill andpin crystals of methamphetamine will form. You may filter these or return themto a glass dish to pan and separate the acetone. Save the acetone, it still hasgold in it.

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

There are a number of good threads on dual solvent recrystaliziation. The basicprinciple is to dissolve the methamphetamine HCl in boiling alcohol, filterthrough a fine filter to remove trash, reduce to saturation, and combine withanother solvent such as dry acetone. Let the temperature fall slowly and give itsome time and meth crystals will form. You will find these to be much cleaner


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than the meth you started with. A good descriptive writeup can be found inChicken: "Step by Step Recrystallization of Meth" (Stimulants) although thereare plenty of others.

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The object of this post was to do a basic, if fairly comprehensive, post-reactionworkup post for meth cooks. I have no doubt omitted any and all informationhaving to do with the question which prompted you to read this post in the firstplace. This is, of course, proof positive that the universe is as it is supposed tobe, and that no good deed will go unpunished. For very long, at least. No doubtthere are those among you who will take issue at part of this post, which is as itshould be; I only intended by this post to centralize in some way the process ofleaning for the new bee intent on making meth. If I have succeeded in thatrespect, I have accomplished what I sought to accomplish.----- Geez


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Post-reaction Workup

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