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'The Cold Method'

HTML by toast

First off, I'd like to thank all those who were kind enough to answer my post @ The Hive, so newbies like you and me can have
more methods to make meth. I appreciate it, as always... toast

Posts taken from this post, @ The Hive.

Mr.? .......... posted 06-27-99 03:08 PM

Member

maybe yo can figure this one out i've saved it for some time now and also linked it here but have
no clue as to how its read......
www.mninter.net/~publish/METHLAB/index3.htm (Note: this is an anti-drug page, I provide the post un-edited, but
if I were to do something illegal like make meth (which I'm not), I would only use this to get a dim idea of what a cold method setup
might look like)

Worlock .......... posted 06-27-99 04:12 PM

Member

www.mninter.net/~publish/METHLAB/index3.htm

"How to make meth without heat"

The honey reaction will begin spontaneously when the chemical mix is right.

The ultimate is to be in the lab at night during a lightning storm.

Prepare your solution, step to the window, and let the light energy from a lightning flash supply
the natural energy needed.

To use a camera flash-bulb would be considered crass and synthetic.

The mix is dry. It is hard to achieve because of variability in reagents, humidity, barometric
pressure, room temperature.

5 ml of Water is injected into the dry mix.

Any external energy can cause it to fire off.

The reaction is done near an ice bucket in case the initial surge gets out of hand.
A very long hose is used, to compensate for the reactions ability to shoot up the hose.
Once the initial exothermia subsides, the mix again is quite dry.
10 ml water is injected, and the reactions moves out again, as the reaction slows,
10 ml of water are added until the addition of water has no effect.
The hose is then back washed with water, to wash any meth into the reaction flask.

Good shit, the yields are fair. 70%

Worlock .......... posted 06-27-99 07:35 PM

Member

Ah am I revealing trade secrets again?

It is legendary that lightening speed is how the gods make it.

That is the combination that is considered perfect. When a flash of light will kick it in gear.
To combine your reactants so perfectly that the tiniest bit of added energy will make it go, without
blowing your ass up.
The reaction, is almost spontaneous.

Have your tape already cut into strips after adding the dry ingredients. Please stress the point to
tape the shit out of the stopper, hose, and flask. I am talking about at least half a roll of duct tape.
that flask should look pregnant at the top. The pressure goes ballistic and can blow HI
everywhere, not to mention the H2 explosion.

The last time I saw the cook, Mikey, he was very burnt from this process, not burned out but, I
mean his long hair was fried up, like from the flame and shit that got away.

The ratios, depended upon the quality of reactants but somewhere in the range of 1.5 : 1 : 1 by
weight of
Iodine : ephed : RP
You can see that the RP is at a dangerous level.!

The reaction is done in 15 minutes.

Two 5 gallon water bottles were used once, One held the reaction mixture, the second bottle had
two hoses
one to the reaction bottle and
one leading up to the roof.

The idea was if the reaction got too strong the second bottle might contain some of the product
instead of blowing it onto the roof.

I should mention that the free end of the hose was fixed to the opening of a 1 gallon plastic jug.
The bottom is cut off, filled with foam and kitty litter and foam to contain and help disperse the
gas.

The gas was something I was curious about, I managed to sneak a very faint wiff, and
immediately wished I had not.
The gas will ruin anything it gets close to.
The rapidity of the process was super.
Flash, bang, add some water, and a bit more.
Viola

Images and Stuff

Anyway, I'm going to be commenting on various cold method pictures I've found:
• What people have said, and how thier own comments relate to each picture (or seem to relate,
thier not my setup, (remember, I don't have a setup, I'm not a criminal ) of course...)
• What I think about the setup..

and finally, a link my own drawing of what a cold method setup might look like (another shitty
diagram)... with some shitty instructions... (maybe not that shitty, but theres no hope for me, yet
(no want either, I don't like competition), in competing with a seasoned bee like Worlock...)

ONWARD!!!

Image #1

Ok folks, toast here... this picture was taken from Rhodium's Clandestine Lab Photo Album
(check out his page, http://rhodium.lycaeum.org, it's my personal favorite).

Look at all those jars of what appears to be honey... sweet nectar of the gods... well, fuck the
honey, we're talking about the setup itself...

Look up in left hand corner of this image, see it there, the mighty cold method setup. Now it
appears as though there are two hoses. One of the hoses connects the two bottles (looks like a
braided hose, just like in methhead's Push/Pull, methhead is the fucking man... anyway, so it's a
braided hose. It looks almost like next to this hose theres a little tube, a pressure release tube I
would imagine, but this statement contradicts the one I'm about to make, so you figure it out...

The second hose is the red one (I dont see any other hose, do you?), it appears to be just a
normal hose. Ok, quoting Worlock (he's also the man, the FUCKING man)
>Two 5 gallon water bottles were used once, One held the reaction mixture, the second bottle
had two hoses
>one to the reaction bottle and
>one leading up to the roof.

aha, so this red hose must be the second hose, on the second bottle... it just leads out to the
ground or wherever instead of up to the roof, much less safe...

>The idea was if the reaction got too strong the second bottle might contain some of the product
instead of blowing it onto the roof.

Get it boys and girls? Neither end of the braided hose would go into the reaction content (nor very
far at all into the bottle). This allows for both HI gas, and H2 to go from bottle 1, to bottle 2, to the
the end of the red hose (and out)... and if the pressure builds up, it also allows for liquids and stuff
(in bottle 1), to go through the braided tube, and down into bottle #2, not out the red hose with the
gasses (see the red hose doesn't go far down into the bottle either, none of them do)...

it could be, however, that the little tiny tube next to the braided does exist, for escaping gas (a
small tube could be attatched), and the braided hose DOES go into the content, so that, and the
red hose, are only for liquids... this is waaaay more likely than my first theory little thing...

I think... any comments on this, e-mail me, chemistry@hushmail.com

anyway... OK! NEXT IMAGE...

Image #2
Ok chem hacks and hackettes, this picture, as you can see, was also taken from Rhodium's
Clandestine Chemistry Photo Album. Good (Rhodium is also the man... I haven't spoken with him
long enough to tell if he's THE FUCKING MAN, but he's a good guy, smart too, reeeeeeallly
knows his shit)

anyway... This cold setup is much like Picture #1, except 1 difference...

There appears in this one to also be a little tube next to the hose on bottle #1, for attatching a
tube to take care of the gasses...

There is also a second bottle, but looks like theres only one hose! well, I would assume the red
hose in picture #1 is just a precaution, incase there gets to be too much liquid... interesting either
way... next...

Image #3
AHH! leave it up to a site that provides info for law enforcement and dumb anti-drug folks
(www.mninter.net/~publish/METHLAB/index3.htm) to just plain FUCK UP! or so it seems...
maybe not though, let's try to make some sense of this oh-so-strange strange diagram.

ok... you have your reaction flask, the erlenmyer, the triangular red one... with all the reaction
contents... then you have your round bottom flask, for the excess water and what-not... but theres
other stuff...

first off, this picture sucks, if some one thinks of a good way to connect two flasks (a round
bottom and an erlenmyer) at the middle, with a hose, let me know, until then, I will say this image
sucks...

It appears as though both flasks are open at the top... however, if you use a 2 hole stopper in the
erlenmyer flask, and a 3 hole stopper (do they make these, anyone know, e-mail toast, but if they
dont make them, one could probably use a two neck flask with a 2 hole stopper and a 1 hole
stopper) on the round bottom it could work.

The first hose (the one for the HI, up top) could go in one of the holes in the erlenmyer (flask #1)
into flask #2, the round bottom one... in flask #1, it only goes down a little ways into the flask (like
I thought for the braided hose in image #1), but in flask #2 this hose goes way down into the
water, so the gas (gasses actually, as Worlock said, its HI and H2, not just HI) bubble through the
water. This has been suggested in many HI/R synths using a refluxing... one would take the
gasses in a tube off the top of the condenser, and pipe them far away into a bucket of water, and
NaOH to basify the stuff, because the gasses would make it acidic... I'm not sure if that would be
ok here, I don't know how that would work here, because of the second hose

the second hose would go in the remaining hole on the first flask, down into the contents... and
the second hole on flask #2 (if they make 3 hole stoppers... someone tell me) ANYWAY! almost
done here... the second tube, the one for the hydriodic acid, would go here (I dont see the point of
having the hydriodic automatically go into the the water as would happen with the diagram, only
incase it overflows)... just above the contents in this one...
well now, theres still 1 hole left over on flask #2? why you ask? HAVE YOU LEARNED
NOTHING? those gasses need to go somewhere, this would be the place for the tube... the tube
to the roof, or to a bucket of water, or where-ever... actually, someone could probably take the
gasses directly off the first one, and only use the second one

STEP #1 - Extraction of Pseudoephedrine

Materials - Step #1

gatorade jugss
pseudo/ephedrine pills
distilled H2O
tube (for siphoning)
coffee filters
heat source (for boiling down, electric stove recomended)
methanol ('Heet' brand works well)

....starting with your pills, crush them in a grinder, and put powder into a large washed out
gatorade jug. make sure you wash with distilled water only. 1000 60mg pills, will yield 1 ounce of
honey, at a 50% return. Next, add distilled water to the powder, and shake....let settle for a minute
or two, and siphon off the water. Repeat steps, until you can't taste the pseudo anymore. The
pseudo has a bitter taste to it.. Now, make sure that you filter the liquid through coffee filters until
the liquid is completely clear. When you have achieved this, boil it down til it's real low and put on
medium heat.....continue cooking it down, until your pseudo starts drying out, then finish with a
blow dryer... Remember not to burn your pseudo.... Scrape the powder into a small pile, and put
into another washed out Gatorade jug. Then add Methanol.... You'll notice that a binder comes
out in the methanol, but was clear in the water. Siphon, and filter, til this is clear......I use about 8
bottles of Heet brand methanol for every 4000 pills worth of powder. Again, filter til clear, then put
on stove and boil.....this time, use a fan to blow on the top of your glass bowl to make sure it
doesn't spill over and catch fire.....Do the same thing that you did with the first batch, low heat,
and blow dry.....Now you'll have pure Pseudo.....The reason for the water pull, is to make sure
you remove all the wax, because the wax is completely soluble in methanol. I forgot to mention,
that when using the water, make sure it is ICE cold. Then, the methanol will bring out the last
binder which is soluble in water. Step 2 coming up, but I have to run.

STEP #2 - Preparing the Setup

Materials - Step #2

(2) 2.5L gas cans

flask, or reaction vessel (perferably filter flask)
braided hose
tubing
PPVC spout (for excess water)
one hole stopper (for flask)
 hose clamps
duct tape
PVC connection for one hole stopper

..... okay, now you should have your pseudo ready to go......just remember the ratios that I give
you..okay...now to make the push/pull......the best thing about it, is the fact that since it's
enclosed, there is no smell and the process only takes an hour or so.......take 2 2.5 gallon plastic
gas cans....tape them together with duct tape , so that the can sit side by side. Next, take the
nozzles from the the gas cans and attach them together.....usually, I cut the end off of one, and
stick the other into it. then I hot glue them together, to seal them. so then you attach them back
onto the cans. this allows water from one side, to enter into the other side. Make sure that you
screw them back on tight, and that your seal is air tight, so that when you stand them up on their
ends, water and/or air does not leak out......Next, take the can on the right side and attach a clear
pvc tubing onto the air inlet of the gas can. This you use to run into a sink, or shower, or empty
container, cuz sometimes iodine water will get pushed out from the reaction. Make sure you use a
hose clamp and hot glue to secure it tightly. Next, take the can on the left, and attach a clear,
BRAIDED, hose to the air inlet. This is the hose that will be attached to the stopper on the flask. It
has to be braided, so that it won't collapse when the heat and pressure build up on the final rxn
phase. Make sure that you use a hose clamp, and some hot glue to attach, cuz you don't want it
to come loose. once this is down, fill one of the gas with 2 1/4 gallons of distilled water. Then
stand the gas cans on end, so that the air inlets are up, and the U connection you made with the
spouts are on the bottom. Attaching the hose to the stopper, can be a bit tricky. I use a threaded
pvc connector. PVC won't deteriorate from the acids, or the heat. There's a special name for the
type of connector I use, so it would be best if I go find out what it is and let you know, cuz the way
it's threaded, it won't get pushed out of the stopper. You can build this setup for around 30
american dollars from parts at home depot. I shall return later with the name. Anyways, after
you've connected the hose to the stopper, you're almost ready to go. The reason you have
distilled water in the cans, is so that you can create a pressure. The push comes from the
contents forcing out oxygen, and the pull comes from a complete hydrogen state, and after the
final rxn, it tries to "breathe" back in oxygen. Use distilled water, cuz sometimes the pull is so
hard, that it actually sucks water, back into the flask. Back soon with step 3.

STEP #3 - The Reaction

Materials - Step #3

heat source (electric stove)

 iodine
red phosphorous
pseudo/ephedrine
distilled H2O
duct tape
rubbermaid "server" jug
visionware bowl
fan (for cooling bowl)
towel

....to answer a couple questions real quick, fzr96.....it shouldn't have cooked for 4 hours......only
about 1 to 1 1/2 hours......and if it never pulled, then it was never done........Here, this might help
answer the questions...... I use a 4000ml vacuum, or filter flask, cuz it has a nipple on the side. I
attach a clear hose to this nipple, with a hose clamp, and pinch the hose closed with a pair of vise
grips. Then I'm ready to get started. Here's the ratio..... take whatever amount of E you have, and
match it with I. Then divide the amount of E you have, and that's how much R you need to use.
My teacher told me though, that if you were to make less than an ounce of honey, you have to
use half the amount of R, instead of 1/3. I don't know though, cuz I've never done less than 4
ounces. So, if it's 4 ounces, i should have 240 grams E, 240 grams I, and 80 grams of R. Take
the flask, and first dump in the R. Then, dump in the E. Add 3 small capfuls of distilled water. If
you're using re-used R, then add a small bump of hydrogen peroxide. Okay, now this part is the
best. Add in the I, but be sure to hurry up and stopper the flask. Then use duct tape to wrap
around the stopper and neck of flask, to ensure it doesn't pop off on you. Now, pick up the flask
and stir the contents. Sometimes it's quick, and sometimes it's not, but the contents inside should
start getting liquidy. If it happens quick, the contents will appear to start to grow. Shake more, in
order to calm it down, cuz you don't want a fast reaction. You should notice that the water is
pushing, and air maybe coming out the right side gas can. Keep stirring and shaking till the entire
contents are liquidy. If you look inside the flask, you'll notice tiny little sprinkles everywhere in the
mix. This is caused by the I reacting with the R, and creating Hydriodic acid. Keep your eye on it.
You'll notice that at first, you have to stir the contents to calm it down. Then after about 15
minutes, it calms down on its own. Then, you have to stir to keep the reaction going. Let this
stirring go on for about half an hour or so. Then, get a large stainless steel stock pot, and one of
those portable electric stoves. Make sure you use the low burning side.... I went ahead and tested
my reaction heat by getting a candy thermometer, and placing the stock pot on the stove and
turning it on, I've noticed that you don't ever want your heat to get higher than 180 degrees, and
that you should start cooking at 150 degrees... Test your stove out before you cook, and look at
the dial on the stove, as to where the certain degrees are. Now, place the stock pot on the stove,
at 150 degrees, and place the flask in the pot. Pick up the flask every few minutes and keep
stirring, replacing the flask back in the pot. After about half an hour of this, (making it 1 hour total
cook time), turn up the heat to 180 degrees and keep the stirring process up. You'll notice that the
contents will get real liquidy, and a yellow film will be inside. The mix will look like it wants to
literally grow inside the flask. After a few more shakes, let it go, you'll notice that more air and
water will get pushed out of the gas can and the reaction will get violent. At this stage, I usually
throw a towel over the top of the flask, cuz I've had accidents before, like the hose coming out of
the stopper and contents get sprayed everywhere. When the push/pull is a rockin away, then
unplug the stove and let it go. When the pushing has stopped, check the flask. The contents
should have grown, and filled the entire flask, and a swirling green/white smoke should fill the
flask. If this didn't happen, then it's not done. Plug back in the stove, and let it go. This final
reaction, is what turns your E into Honey. What happens, is the contents reach a totally hydrogen
state. The last of the I has turned into Hydriodic acid and all the oxygen gets pushed out of the
flask. This is where you get the pull from...Cuz the hydrogen state combined with heat, creates a
pressurized vacuum state. After this final reaction has happened, let the flask cool down, and
every 2 minutes, stir the contents. You do this, because when you stir up the contents, you make
sure that more E gets turned into Honey. Then when the flask has cooled down to a warm state,
keep the nipple hose pinched, and release the vice grips. Place a funnel into the hose, and add
distilled water to the funnel, then unpinch the hose and let the water into the flask. Let air get in
through the hose cuz if you don't, then as soon as the water hits the inside of the flask, the
vacuum will pick up and suck water from the push/ pull. Add more distilled water and remove the
duct tape and stopper. Shake the flask around, and pour the contents into a heavy visionware
bowl. Add more distilled water to the flask, to clean it out, and add to the visionware. Next, place
bowl on the stove, and put on high heat. Get a plastic spoon, and wash with distilled water, to use
to stir the mix. Place a fan next to the stove to use to cool the bowl down. Stir the contents to a
boil, and remove from heat. Turn the fan on, onto the bowl, and let cool down a bit. You'll notice
that all of your R has dropped to the bottom of the bowl, and it's ready to filter. You should have a
golden colored liquid. Filter, until all the R is out of the liquid, and place into a rubbermaid "server"
jug. I'll be back with the rest in a bit........THE FINAL STEPS

STEP #4 - THE FINAL STEPS

Materials - Step #4

store bought ice

coleman's fuel
'red devil' brand lye (sodium hydroxide)
gatorade bottles
distilled H2O
tube (for siphoning)
towel
shot glass
'3-way pool test strip' (pH paper)
muriatic acid
eye dropper type bottle
visionware bowl
heat source
fan
 blow dryer
ice water

FINAL STEPS>>>>>>>okay boys and ghouls, yes, this is the most important part, and if you
follow everything right, you won't even need to wash the shit......trust me, my honey has never
needed a washing YET!.....almost never leaves a residue in the pipe.....trust me... where i
live.....i'm just about number one in quality......and i'll be chatting to TOAST about
pics.............okay........ put the yellow colored liquid into the rubbermaid server jug from wal-
mart..... this is acid/honey water.......put in a small layer of ice (bag of ice bought from any store,
cuz it's allllll distilled), then add an equal portion of Colemans fuel..... if you don't use ice, you're
going to get a volcano eruption of lye/acid/colemans all over the place.......when the lye hits the
acid, it'll heat up and create alot of pressure......the ice keeps this from happening, until you shake
up the container.. next, add about 1/4 can of Red Devil Lye... in mine, it takes about a 1/2 can......
but you don't want to overkill the lye or you'll lose everything.......now screw on the pop-top lid,
and shake, with small towel over the top....just in case of leakage.... the jug should heat up and
expand.....let settle for a second, and undo the pop-top to let out pressure, close, and repeat......
add more lye as you go along, until you get a very strong cat urine/ammonia smell..... when your
nostrils have received this little message, it's time to let the mix settle, and siphon........take a
large gatorade bottle, and poke a hole in the screw top.... next, wash out the bottle, and cap
thoroughly, using distilled water........ next, siphon the colemans, into a filtered funnel, into the
gatorade bottle.......now, you should have one gatorade bottle, with honey/colemans fuel in
it........add an equal amount of distilled water to this.... then, shake the contents up..always
remember to cover the hole in the top with your finger when shaking.......turn the bottle over,
holding the hole closed, and let settle, then with your other hand, grab a 3-way pool test strip and
place over a shot glass, then let a small amount of water run over the ph part of the strip....the
color should be a violet blue........lots of honey in there folks......so, turn the jug upright again, and
remove cap......next, we have to "push" the honey into the water.... to do this, get some muriatic
acid, and a small bottle with a dropper type top on it. fill this with muriatic, and add a small squirt
into the bottle.......if you look at the water when you do this, you'll see the acid fall to the bottom,
and quickly surface. But, with the acid, you'll see ribbons of honey stay in the water........cover the
hole with your finger again, and shake..... turn the bottle over, holding the hole with your finger,
and test again.....keep repeating this, until the ph strip turns a reddish-pink color......this is the ph
level you need to keep it at.....if the strip goes yellow, that means there's too much acid and
there's nothing you can do about it... at least not if you haven't saved anything in your shot
glass......just take the water from the shot glass, and add it to the jug, then retest.......if the strip is
okay, then replace a clean visionware bowl on the stove, and drain the water into it.....bee careful
not to let the colemans fuel fall into it, or your honey will be good, but tainted......if some does get
through, take lighter, and light the top of the water, and the colemans will burn away........ now,
turn it up to a boil, and wait till you see it "cracking back". you should have the fan on it, to help it
go faster. When it starts to "crack back" alot, remove from heat, and place the bowl in ice water....
WARNING.....make sure its a Corning VisionsWare bowl....it's the only glass bowl that I know of
that can go from extreme heat and cold......other glass bowls would shatter upon even touching
the ice cold water..... after putting the bowl in ice water, make sure you get a blow dryer, and blow
air into the bowl to help it dry......if it's still too liquidy after 5 minutes, then replace on the heat for
a few more minutes and repeat.. if you're too afraid of hurting the honey, then just use the blow
dryer to dry the rest of the way..........well folks, all I can do to help you, is answer questions, take
some pictures, and MAKE THE VIDEO..... wonder if I should charge?....doubt it..... knowledge is
free.......

STEP #5 - Purification

METHOD #1
Washing is not necessarily a needed step, and is provided just a misc. information.

By toast, Inspired by Replies from Wehh, spitball (this whole thing is pretty much his idea in my words),
and Worlock

Materials - Step #5 - Method #1

acetone
funnel
acetone safe container

Find a container that is made of an acetone safe material (glass, some plastics), this will be your
"used acetone collector". Now find a funnel as big as the opening of this container. Place the
funnel so it rests in the opening, and place a coffee filter or two in the top of the funnel. On this
filter, place your "substance to be purified." The acetone for this procedure should be pre-chilled,
just put it in the freezer for awhile. Putting it in the freezer for too long could cause condensation
(thanks spitball). Pour the cold acetone over the "substance to be purified" and watch as it gets
whiter and whiter! :0) (Note: "If you're not using lab grade acetone, you're going to lose more of
the product any ways, so there's really no reason to cool it, although in small quantities it'll be a
noticable loss." - spitball)

METHOD #2

Image by toast, taken from "The Organic Chemistry Survival Manual" by James W.
Zubrick, pg. 128

Materials - Step #5 - Method #2

acetone
buchner funnel
filter paper (coffee filter)
 vacuum source
tubing
filter flask
one hole stopper

I feel much explanation for this method is not needed, seeing as how purification may not even be
a necessary step in the push/pull method (see Step #4). However, it must be clarified that the
"substance to be purified" is mixed with acetone in a seperate flask, then poured through the
funnel, with the vacuum on. The vacuum removes the acetone and the impurities, with minimal
loss of product (thanks Worlock).

Definitions

Solvent
A substance, usually a liquid, that dissolves something else
Solute
A substance that is being dissolved in something else
Solubility
How easily a substance dissolves in a certain solvent
Acid
A substance that gives up a proton easily
Base
A substance that accepts a proton easily
Salt
The product from the reaction of an acid and a base
Freebase
The natural form of a drug, hasn't been reacted with an acid.
You can change it back and forth between its freebase and salt form as many
times as you want.

Explanation of A/B (acid base) extraction

Most drugs have an amine group. This is a -NH2 attached to the molecule somewhere.
NH3 is a base (accepts protons from acids easily) so the drugs are bases also. Hence the
name freebase. When you make the drug, it usually starts out in the freebase form, which
is quite often an oil. What happens when you react an acid and a base? You get a salt. So
when you take your freebase (base) drug and react it with an acid, you get a salt, such as
a hydrochloride salt if you react it with hydrogen chloride (HCl).

Salts are usually crystalline solids rather than oils or waxy solids, which is why they are
so popular with drugs, it makes them easier to handle, and the drug properties are not
changed. Think about it, you have HCl in your stomach, and acid throughout your body,
so if you ingest a drug in either form, it will end up being in the same form (probably a
salt) in your body no matter how it started out.

Freebases and salts usually have drastically different properties. An important one is that
freebases are usually soluble (will dissolve in) in non-polar solvents such as toluene and
hot naphtha, and not soluble in polar solvents such as water. The salts are usually the
opposite, soluble in water, but not toluene etc. This is how acid/base extractions (A/B)
work.

You can basify your molecule with NaOH (lye) to form the freebase, which is not soluble
in water, but it will dissolve in a non polar solvent. So you add your non-polar solvent
and the freebase goes in to it (a lot faster if you shake it all up instead of waiting for the
freebase to float up to it). Once you have freebase in your non-polar you can wash the
non-polar solvent with water to get rid of any non-freebase drug material (such as excess
lye). The water will not remove any of your freebase.

Then to recover your hydrochloride salt (the most popular form of most drugs), you react
it with hydrochloric acid. Muriatic acid is hydrogen chloride (HCl) dissolved in water. So
if you add this to the non-polar with the freebase, the freebase will react with the HCl to
form the salt, which is now soluble in water and not in non-polar, so it will dissolve into
the water layer, which you can separate and evaporate to obtain your crystals.

Since evaporating water sucks, and quite often leaves behind impurities, it is nice to react
your freebase in non-polar with HCl without any water around. This is when gassing
comes into play. You can generate pure HCl which is a gas without any water, and
bubble this gas through your freebase/non-polar. It will react with your freebase to form
the hydrochloride salt (what you want). Since the salt is not soluble in the non-polar, it
will them fall out of solution as crystals which can be collected by filtering.

Explanation of recrystallization

Once you have your dry drug hydrochloride salt crystals, sometimes you want to get
them more pure, because impurities can be trapped inside the tiny clumps of crystals. A
good way of doing this is to recrystallize. The idea behind this is to find a solvent that the
crystals are kind of soluble in and kind of not. Alcohols usually work well for this. When
talking about solvents and solid materials, hot solvent dissolves more solid than cold
solvent, so this can be used to your advantage. (The case is opposite for gases but I won't
go into that).
Get two containers. Put some alcohol in one and bring it up to boiling. Put your crystals
in the other container. Slowly add boiling alcohol to your crystals and they will dissolve.
Use just enough alcohol to dissolve all of your crystals.

Now since cold alcohol doesn't dissolve crystals very well, cool down the alcohol/product
and the crystals will come back out (recrystallize). The slower you cool the alcohol, the
bigger the crystals are. The bigger the crystals are, the fewer impurities will be trapped
inside of them, and the purer your product will be. So big crystals = pure crystals
(usually).

One good way for ensuring that your alcohol cools down nice and slow is to put some
water in a pot and heat it to boiling and take it off of the heat. Then put your container
with hot alcohol/dissolved crystals in the pot of water being sure not to get any water into
the alcohol, cover the container, and let it cool down to room temperature. Then you can
put the container with alcohol in the refridgerator to cool more. Then into the freezer to
cool more. Then you can filter your pretty crystals out. Now there is usually still a little
bit of product left in the alcohol, so if you boil off say 75% of the alcohol and repeat the
cooling process you can get some more crystals.

There are other ways of changing the solubility of the crystals in the alcohol, such as
adding acetone or ether to the alcohol, but the temperature method works quite well, is
cheap, and simple. So newbies should use it first, then experiment with other methods if
they want to.

Related Links

• Acid/Base Extraction Tutorial (University of Alberta)

• Professor Forkey's Liquid-Liquid Extraction Tutorial
• Proper Recrystallization Technique

The most common method of purifying solid organic compounds is by recrystallization.

In this technique, an impure solid compound is dissolved in a solvent and then allowed to
slowly crystallize out as the solution cools. As the compound crystallizes from the
solution, the molecules of the other compounds dissolved in solution are excluded from
the growing crystal lattice, giving a pure solid.
Crystallization of a solid is not the same as precipitation of a solid. In crystallization,
there is a slow, selective formation of the crystal framework resulting in a pure
compound. In precipitation, there is a rapid formation of a solid from a solution that
usually produces an amorphous solid containing many trapped impurities within the
solid's crystal framework. For this reason, experimental procedures that produce a solid
product by precipitation always include a final recrystallization step to give the pure
compound.

The process of recrystallization relies on the property that for most compounds, as the
temperature of a solvent increases, the solubility of the compound in that solvent also
increases. For example, much more table sugar can be dissolved in very hot water (just
below the boiling point) than in water at room temperature. What will happen if a
concentrated solution of hot water and sugar is allowed to cool to room temperature? As
the temperature of the solution decreases, the solubility of the sugar in the water also
decreases, and the sugar molecules will begin to crystallize out of the solution. (This is
how rock candy is made.) This is the basic process that goes on in the recrystallization of
a solid.

The steps in the recrystallization of a compound are:

a. Find a suitable solvent for the recrystallization;

b. Dissolve the impure solid in a minimum volume of hot solvent;
c. Remove any insoluble impurities by filtration;
d. Slowly cool the hot solution to crystallize the desired compound from the
solution;
e. Filter the solution to isolate the purified solid compound.

Choosing a solvent

The first consideration in purifying a solid by recrystallization is to find a suitable

solvent. There are four important properties that you should look for in a good solvent for
recrystallization.

1. The compound should be very soluble at the boiling point of the solvent and only
sparingly soluble in the solvent at room temperature. This difference in solubility
at hot versus cold temperatures is essential for the recrystallization process. If the
compound is insoluble in the chosen solvent at high temperatures, then it will not
dissolve. If the compound is very soluble in the solvent at room temperature, then
getting the compound to crystallize in pure form from solution is difficult. For
example, water is an excellent solvent for the recrystallization of benzoic acid. At
10°C only 2.1 g of benzoic acid dissolves in 1 liter of water, while at 95 °C the
solubility is 68 g/L.
2. The unwanted impurities should be either very soluble in the solvent at room
temperature or insoluble in the hot solvent. This way, after the impure solid is
dissolved in the hot solvent, any undissolved impurities can be removed by
 filtration. After the solution cools and the desired compound crystallizes out, any
remaining soluble impurities will remain dissolved in the solvent.
3. The solvent should not react with the compound being purified. The desired
compound may be lost during recrystallization if the solvent reacts with the
compound.
4. The solvent should be volatile enough to be easily removed from the solvent after
the compound has crystallized. This allows for easy and rapid drying of the solid
compound after it has been isolated from the solution.

Finding a solvent with the desired properties is a search done by trial and error. First, test
the solubility of tiny samples of the compound in test tubes with a variety of different
solvents (water, ethanol, methanol, ethyl acetate, diethyl ether, hexane, toluene, etc.) at
room temperature. If the compound dissolves in the solvent at room temperature, then
that solvent is unsuitable for recrystallization. If the compound is insoluble in the solvent
at room temperature, then the mixture is heated to the solvent's boiling point to determine
if the solid will dissolve at high temperature, and then cooled to see whether it
crystallizes from the solution at room temperature.

Dissolving the solid

Once a suitable solvent is selected, place the impure solid in an Erlenmeyer flask and add
a small volume of hot solvent to the flask. Erlenmeyer flasks are preferred over beakers
for recrystallization because the conical shape of an Erlenmeyer flask decreases the
amount of solvent lost to evaporation during heating, prevents the formation of a crust
around the sides of the glass, and makes it easier to swirl the hot solution while
dissolving the solid without splashing it out of the flask.

Keep the solution in the Erlenmeyer flask warm on a hot plate or in a water bath, and add
small volumes of hot solvent to the flask until all of the solid just dissolves. Swirl the
solution between additions of solvent and break up any lumps with a stirring rod or
spatula. Occasionally there will be impurities present in the solid that are insoluble in the
chosen solvent even at high temperature. If subsequent additions of solvent to the
solution do not seem to dissolve any of the remaining solid, stop adding solvent to the
solution (as this will decrease the percent recovery of the desired compound) and filter or
decant the hot solution to remove the insoluble impurities.

Using decolorizing carbon

Colored impurities are sometimes difficult to remove from solid mixtures. These colored
impurities, often due to the presence of polar or polymeric compounds, can cause a
colorless organic solid to have a tint of color even after recrystallization. Decolorizing or
activated carbon is used to remove the colored impurities from the sample. Decolorizing
carbon is very finely divided carbon that provides high surface area to adsorb the colored
impurities.
Very little decolorizing carbon is needed to remove the colored impurities from a
solution. You must be judicious in your use of decolorizing carbon: if too much is used, it
can adsorb the desired compound from the solution as well as the colored impurities.
After the impure solid sample is dissolved in hot solvent, a small amount of decolorizing
carbon, about the size of a pea, is added to the hot solution. This must be done carefully
to avoid a surge of boiling from the hot solution. The solution is stirred and heated for a
few minutes and then filtered hot to remove the decolorizing carbon. The resulting filtrate
should be colorless and the recrystallization process continues as before.

Crystallizing the solid

After the insoluble impurities have been removed, cover the flask containing the hot
filtrate with a watch glass and set it aside undisturbed to cool slowly to room temperature.
As the solution cools, the solubility of the dissolved compound will decrease and the
solid will begin to crystallize from the solution. After the flask has cooled to room
temperature, it may be placed in an ice bath to increase the yield of solid. Do not rapidly
cool the hot solution by placing the flask in an ice bath before it has cooled to room
temperature-this will result in a rapid precipitation of the solid in an impure form because
of trapped impurities.

Sometimes the dissolved compound fails to crystallize from the solution on cooling. If
this happens, crystallization can be induced by various methods. One way to induce
crystallization is by scratching the inner wall of the Erlenmeyer flask with a glass stirring
rod. This is believed to release very small particles of glass which act as nuclei for crystal
growth. Another method of inducing crystallization is to add a small crystal of the desired
compound, called a seed crystal, to the solution. Again, this seed crystal acts as a
template on which the dissolved solid will begin crystallizing. If neither of these two
techniques results in crystallization, the compound was probably dissolved in too much
hot solvent. If you believe that you may have too much solvent for the amount of
dissolved compound, reheat the solution to boiling, boil off or distill some of the solvent,
and then allow the solution to cool to room temperature again to effect crystallization.

Isolating the solid by suction filtration

Once the compound has completely precipitated from the solution, it is separated from
the remaining solution (also called the mother liquor) by filtration. Typically this is done
by vacuum or suction filtration using a Büchner funnel. Line the bottom of the Büchner
or Hirsch funnel with a piece of filter paper that is large enough to cover the holes in the
bottom plate of the funnel without curling up on the sides of the funnel. Place a neoprene
adapter on the stem of the funnel and insert it in the top of a filter flask (a thick-walled
Erlenmeyer flask with a side-arm) that has been securely clamped to a ringstand.

Using a piece of thick-walled vacuum tubing, connect the side-arm of the filter flask to a
water aspirator. Turn the water to the aspirator on full force to create a vacuum through
the system. If necessary, carefully adjust the piece of filter paper so that it covers all of
the holes in the funnel, and then dampen it with a small volume of cold solvent; this will
create a better seal between the filter paper and the plate in the funnel, preventing any
solid from getting under the filter paper and passing through the funnel. Slowly pour the
recrystallization solution into the funnel and allow the suction to pull the mother liquor
through. Rinse the Erlenmeyer flask with a small volume of cold recrystallization solvent
to remove any remaining solid. Add this solvent to the funnel and then wash the solid in
the funnel, called the filter cake or residue, with a few milliliters of fresh, cold
recrystallization solvent to remove any remaining mother liquor and dissolved impurities.

Leave the aspirator on for a few minutes and allow air to pass through the crystals to dry
them. After pulling air through the crystals for a brief time, remove the vacuum from the
system by disconnecting the vacuum tubing from the aspirator before turning the water
off. If you turn the aspirator water off first, water can be sucked into the filter flask and
may contaminate the product. The filter cake is removed from the funnel by carefully
prying it from the filter using a spatula. The cake of crystals will still be slightly wet with
solvent and should be allowed to dry thoroughly before measuring the weight or melting
point of the solid material.