Post-Reaction Workup

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The post-reaction workup:

A cook's essay on how to nish 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 or
pseudoephedrine to methamphetamine. Perhaps you arrived here by the use of
red phosphorous and iodine, whether by push-pull, balloon, or reux 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 nished?: Your reaction ask is full of larger bubbles and those small
ones you have watched for so long are missing. When you remove the ask from
the heat, and the ask 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 ask. If you are not too sure about the smell, add a little
hot water, careful not to ood the reaction out. (Geez adds as much hot water as
there is uid in the ask at this point if the smell is right.) The red phosphorous
should fall out of the solution right away. When the ask cools just enough for
the convection currents to cease, swirl the ask 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 uid is
reddish orange, put it back on the hot plate and let it cook some more. Hoping
all you want that it is really nished 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.
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If you swirl the ask and the red will settle falls to the bottom like bricks, your
reaction should be considered as nished. The reaction uid 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 uid is reddish-orange, but the red phosphorous falls like bricks to the
bottom, you likely have an excess of iodine present in the reaction uid. 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 sucient. You can also just let the uid in the ask boil, condenser
removed, for ten or fteen mintues; this will clear excess iodine without using
sodium thiosulfate.
Fine Filtering Dilute the uid in the ask with an equal volume of hot dH 2O.
Swirl until the red is in the uid and quickly pour the uid through a lter. You
will not get all the red phosphorous the rst time. Add more water, swirl, repeat
the process. You may nd it helps to hold the ask upside down as you cease
swirling (with a stopper in the opening of course) so the red phos will be
washed out. Rinse the ask again with near-boiling water. Rinse the red
phosphorous ltered out while it is in the lter with additional hot water. The
goal of ltering is to get the red phosphorous out of the uid. Some particles
are very small and dicult to lter out without proper lter 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 nd...be generous here...use one big enough to hold all of what you
plan to lter if you can. Gravity ltration 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 lters) and putting a uted lter paper into the
funnel. Wet any lter papers and cotton balls with water before pouring the
honey into the lter. Coee lters are an often used substittute for lter paper.
The problem with coee lters is that they are no ne enough for this job, and
they trap some red phosphorous in the lter bers. 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 lter even
ner and ner 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 ne, thin stream and
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often this will be perfect; the steady drip seems to remove more of the very ne
ne particles or red phosphorous, however. Do not use a lter on top of this,
and do not lay tissues at 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 o the end
of the plug; The rst 3 or 4 mm of the plug will have red phosphorous
embedded in it; tear this part of the plug o 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 bers, 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 at 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 eectively. You cannot do it eectively 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 ber and its a big mess, and you do not want
the paper ber 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 ask 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 ask at this point, and use sucient
water to rinse the methamphetamine from the red phosphorous. The red
phosphorous is allowed to dry in the ask, 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 ask if you plan to leave the phosphorous in the
ask.)
When all your honey has dripped into the receiving ask, run it through the
lter one more time. If you are using a Charmin Plug, use a new plug for this
ltration. If not using a Charmin plug, lter through the red again. The
additional ltering has benets. Some of the red phosphorous is very ne, and
you do want it out of your honey; the second ltration will get more red than
you thought was in the uid. If you lter through the red phosphorous already
collection, you also lter out iodine in the uid; likely not all of it, but some of it.
The cleaner the better.
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After the honey has ltered 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 lters 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 uid than you
have when the reaction completes. Diluting the reaction uid 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 dicult.
Dilute much further than that and you make the extraction more dicult.
The Non-polar solvent wash of ltered honey. How do you wash honey?
With a non-polar solvent. This step may be the one single most eective
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 uids 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 stu. Your product is safely inside
that aqueous reaction uid and cannot be persuaded to jump to the non-polar
until you base the solution and strip that salt o 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
fteen 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 uid. Some bees will bring the honey to a boil in the ask with
non-polar solvent present, and report that this appears to eliminate PEG. The
logic behind boiling the contents of the ask is apparent. Hot solvents clean
better and boiling the uid makes certain there is enough convection in the
ask to expose all the uid to the solvent. Experience with pill extraction
suggests ve mintues is probably sucient time for the non-polar to absorb
what it will; if it is saturated with trash, one may always follow with another
boil.
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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 rst, 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 uid with the solvent used to extract will remove anything in the
uid that is soluble in that solvent, which means it will not be in the uid 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 uid 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 rst wash in the sep funnel for ve or ten
minutes after shaking the two together. The dierence in what you nd 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 uid 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.
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The volume of solvent is more dependent on the quantity of meth to extract

rather than the volume of the reaction uid, which includes the water used to
rinse the ask, the red and the lters. 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 diuclt 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 fth time with non-polar
solvent. The 200 ml volume is a suggestion applicable to naptha, coleman's fuel,
charcoal lighter uid, and xylene. TCE is a very eective 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 uid. Make a twenty percent solution of NaOH. This
means ll a beaker on fth full of NaOH, and ll it with water. Stir it until all the
NaOH dissolves. Let it cool. (Do this before you begin ltering the red
phosphorous from the reaction ask, and you will be ne. When its time to let
the reaction uid boil o 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 uid in it. Add the non-polar solvent chosen to extract the freebase
methamphetamine unless you choose TCE. TCE should be added after the
reaction uid is based. The solids that form with basing have a habit of nding
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 sucient
for all our purposes here. Watch the NaOH solution as it enters the reaction
uid. 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 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 uid, 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 uid. Measure the pH of the
reaction uid 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 nd it way to the non-polar solvent when
the reaction uid 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 uid until it is well above pH 12.8. Many cooks add
base until the reaction uid "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 rst add a small splash of NaOH solution to the uid it will turn the
uid milky where that splash mixes, then the uid will clear again. Continue to
add NaOH solution a little at a time until the reaction uid 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 sh
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
sh. You will come to love that smell. When you have milky reaction uid and
smell the sh, 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 uid.
Notes on Extracting the Meth into Nonpolar Solvents:

1) SWIRL, and DO NOT SHAKE. There is no reason to shake the based reaction
uid 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 uid. Shaking
form emulsions, these emulsions trap reaction uid 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 sucient.
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 fteen 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 uid. Add a little more NaOH solution to make
sure the uid 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 uids sit together for awhile. Remember the last
time. After the two layers separate completely, separate out the non-polar
solvent. Combine with the rst volume of solvent. Some cooks proceed at this
point to a third pull with fresh solvent. Geez will add more solvent and leave the
uid 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 uid 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 uid 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 stu 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 rst 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 rst two extractions. What yield you get from a
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third pull is "extra" and it is the stu 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 uid
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 uid. [i][waste
not, want not.) Whatever you do, keep everything until you have nished
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 uid 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 uid. You can
pour it in, but if it comes in a spray can, just direct the spray right into the
based reaction uid. Not much swirling required. TCE will make a emulsion of
sorts but this does break down in ten to fteen mintues in clean uid. 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 oat 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 uid.
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 eective
extraction technique suited to the source of the precursor is the rst 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
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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 sucient. 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
rst 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 suciently 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 eervesce 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 eect of
breaking an emulsion. The most likely successful method if waiting alone does
not work is to pour all of the reaction uid, emulsion and non-polar solvent into
a ask or coee pot or container that will take heat, and heat it up slowly,
stirring occasionally. Bring the reaction uid 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 ask, but is a diversion to
watch. While heating, add some boiling stones, broken clay pot pieces, or
washed coarse sand to the ask 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 eorts a complete waste. This
phenomenon is referred to as bumping. Do not let it destroy your day. It is
simple to avoid. One nal suggestion, used on one occasion by the poster
helping a friend out of a jam, is to nely powder activated carbon and add this
to the contents of the boiling coee pot or ask. It will oat to the interface.
Grind it nely, you want it to be ne. Bring the contents to a boil. At rst it will
appear that the carbon is blocking any meth from coming to the surface, but as
the convection currents in the ask increase the carbon will beging to swirl on
the top layer, and you will be able to see into the reaction uid 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 eective solution, as is starting over
with clean precursors.
Lye lock and other such ideas Lye lock is the state which the reaction uid
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reaches when the cooling reaction uid 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 uid to recover I2, you can base the acid in
the reaction uid to raise the pH.
Ker Plunking -- the variation on the Acid/Base extraction.
Plunking for quality and quantity" (Stimulants)
Worlock: "Ker
Ker Plunking-- whether it is all that it is advertised to be or not-- does in fact

provide an ecient way to perform an acid/base extraction of
methamphetamine from the reaction uid. 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 o an wait
fteen minutes. Separate the naptha from the reaction uid. In the poster's
experience, your yield, if you did this properly and with sucient naptha (count
on 500 ml per ounce of meth) will come in the rst pull. (The poster is in the
habit of letting the reaction uid 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 ask. A large Erhlenmeyer is ne, so is a coee
pot. Geez likes a white corningware coee 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
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overlook to do this under penalty of losing your whole batch to a big "bump,"
having a re, bringing in the re 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% H 2O2,
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 ecacy. 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 benet 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 uid is just bubbling. All the while, add a little
NaOH, a little more, a little more. You can measure the pH of the reaction uid
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 dierent, 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 oat to the interface layer. Stir, bring the
temperature of the reaction uid up to boiling slowly. Observe the convection
currents in the reaction uid maing the carbon roil in the pot. Keep it there at
least ve 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 uid, and
conrm 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
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white, stay white and begin to elute small bubbles, like the zz when you pour
soda, only not so intense. 3) Smell the sh 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 o. Leave it alone for at least fteen minutes.
When it nishes releasing the small bubbles to the non-polar layer and has
cooled o 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 uid. Pouring it out is not a viable solution. It is
full of idodides. You can in fact recover I2 from the reaction uid. 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 stu that falls out is the dirtiest you get. That is
why you should wait about ten to fteen minutes after the rst 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
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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 nd 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 benets as the lye solution
wash is the brine wash...a wash with salt-saturated hot water. This wash also
provides a benet in helping dry the non-polar solvent if you will gas.
temperature of washes Geez does hot lye solution or hot brine solution rst,
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 nishes 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:
http://www.rhodium.ws/chemistry/hclgas.argox.html; http://www.rhodium.ws
/chemistry/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 modied 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.
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He lters 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 ow 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 ltered through a lter and the ltrate 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 stu 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 dierent 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 nal 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
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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 rst 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 stu you gets is so dirty its not worth
messing with. Toss the dirty stu 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 stu came in, and is one of the reasons why he evaps
the rst 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 dH 2O 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.
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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 nally neutralized the mix.
Normally, you will collect the three volumes of non-polar solvent used to extract
the meth from the reaction uid, 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 o 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 rst 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
rst 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 dicult 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 (ve 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 nd that if you follow this method, your chances of
contaminating 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 at
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 rst 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, ood the dish with dried
acetone. This technique is called "acetone ashing" 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 ashing: geezmeister: "Re: Acetone Crashing" (Stimulants)
While this post addresses ashing 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 lter. Filters absorb a lot of product. If you must
use a lter 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 coee lter and let it gravity
lter. Rinse with a little fresh acetone, particularly if you used too much acid.
Place the lter 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 lter with
fresh dry acetone. Do dry the acetone before use, and do save all the rinse
acetone-- particularly the acetone used to ash when the dish is still warm.
Put the acetone poured o after ashing 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 lter 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, lter
through a ne lter 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 nd these to be much cleaner
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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.
*********************************************************
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 rst
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
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Post-Reaction Workup

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HI Reduction Methamphetamine Workup - [www....

[www.rhodium.ws] [] [Chemistry Archive]

The post-reaction workup:

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

The volume of solvent is more dependent on the quantity of meth to extract

HI Reduction Methamphetamine Workup - [www....

Notes on Extracting the Meth into Nonpolar Solvents:

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

Ker Plunking-- whether it is all that it is advertised to be or not-- does in fact

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

be an advisable and worthwhile characteristic, but I suggest that it is an

HI Reduction Methamphetamine Workup - [www....

HI Reduction Methamphetamine Workup - [www....

over-basing the mix are much reduced.

HI Reduction Methamphetamine Workup - [www....

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