The Reaction
At this point, you may begin dreaming in the alpha state of mind , not unconscious sleep but an aware state of peaceful relaxation,, If you choose to come out of the alpha state, simply flex your arms and you will awaken, alert , feeling well rested and happy.
Flask
The flask used is often a flat bottom with a rubberized stopper,
boiling , erlenmeyer, or a vacuum flask.
The flask can be almost any
glass device such as a bottle, champagne bottles are preferred because the
can handle the pressure. Buy flasks and stoppers at a Home beer and wine
brewing supplier. Coke bottles can be fit with a single large diameter hose
leading outside for small batches
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Weight of Ephedrine( gm) |
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The larger the flask the more important it is to heat it evenly, A new large
flask will break on a hot plate that is too small.
In one week I broke a 12
liter and a 6 liter flask because I used too small of a heat source
Stopper and hose
The
stopper has a hole in it, to vent the gasses into the push/pull tanks, or to the
outside.
For the push pull ,It is fitted with a 3 foot length of 1/2 inch, or 3/8 inch
braided food grade plastic hose type tubing.
Almost any type of tubing may
be used. It is variable. but needs to be somewhat stiff so it will not
collapse
If venting outside, usually a 15 to 20 foot hose, longer is fine. can be thin walled since collapsing won't be a big factor when venting to the open air
The main thing is it should be clean, fairly new, and in good shape, and fit
the stopper .
A dirty deteriorating hose will taint your reaction with
particles of a deteriorated plastic hose, nasty.
Home depot has rubber
stoppers all sizes in trays near the fasteners, and mirror hangers
Filter flasks work very well for a reaction flask but are
sensitive to heat and may crack.
Larger flasks are sensitive to uneven
heating and are more difficult to heat evenly.
A 12 Liter flask on a small
hot plate will heat unevenly and crack. whereas a 6 liter will do fine on the
same hot plate
Push Pull unit - Anti smoke device
direct
In this example ,Two 2.5 gallon gas cans are used, the pour spouts are
joinded together. The air inlet is hooked to the reaction flask. The flask in
this example is a vacuum flask. The best is a long necked round bottom reaction
flask The hose leading to the push pull unit can attach to the
side port or the top.
If attached to the side, the main top opening can be
used to add water or reagents.
direct
In this example an erlenmeyer flask is used along with two plastic gatoraid
bottles, the bottles are joined with a sprinkler riser and JB weld. Notice that
the two hoses, one hose leading to the reaction flask, and the
other leading to the drain are very near the
top of the push pull units, to prevent push pull water from
being sucked into the hoses.
siphon
Use only enough water, so that if all the water ends up
being pulled into the first tank, it will not be sucked into the reaction hose,
Only fill each of the tanks 1/3 to 1/2 full of water
or
Fill the
first flask 3/4 full and leave the second flask empty
Sizes of push pull units- This is only generalized
information, gathered from 20 or so different p/p units used. No actual
experiments were performed, but the units were built and used.
Of the above
designs the "direct connection" is much more sensitive to the pressure
changes. The siphon designed tanks generally will not respond to the pull,
and they require more pressure to move the fluids on the push. In addition
the dual connections through the top with the increased pressure leads to gas
leaks.
The direct connection is best.
A pair of 5 gallon water
jugs with a siphon tube never did bubble any air into the second tank and seemed
to slow the reaction down.
The 1 gallon tea jugs are great for up to 4
ounces of E
Already have the hole near the bottom to join the two tanks and an easy to drill plastic top.
Less than one ounce - run the hose to the outside do the reaction
at night, or two 1 liter bottles
1-2 ounces - two 2
liter soda bottles
2-4 ounces - two 1 gallon glass tea jugs
4 to 16 ounces- two 2-1/2 gallon gas cans -- This is probably
the ideal size
Do not use 1 gallon water jugs, the plastic is too thin and they will
collapse on the pull phase.
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Tincture or poor quality of chems --- Matchbook RP use 2x -3x normal amount |
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My favorite uses excess iodine and RP - this insures a spontaneous reaction, and complete conversion of E to Meth, but is a rather violent reaction |
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4 oz or more good chemicals - methhead's suggested ratios |
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Lowest amount of RP used to convert 6+ ounces |
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What to use for less than an Oz |
Remember the second time around for the RP it will contain Iodide unless well
cleaned and dried , and therefore the actual amount of the RP is much less.
Because of the Iodide weight . So add 2x the RP if it was pre-used and not
cleaned.
If the RP was washed in acetone and water then dried it is almost
good as new
Some bad news 92% is the top yield of chili by weight,
theoretically possible
It is common to obtain between 50% to 75%
chili by weight and rarely 85%
The addition of aluminum to the reaction
reduces the amount of RP needed, 5-6 soda can pop tops / oz of E
Water
The common mistake
is adding too much water, or too little water and not getting any
reaction. Mix the reagents dry, then add 1 to 5 3 ml
distilled water /ounce of E.
The mixture should be a
thick wet mud,
As it fires off , the first thing that happens is it
liquefies, and becomes wetter.
This is such a touchy part of the reaction,
experience is the only way to be sure
If the reaction still does not fire,
Use heat,
If heat does not do it or the mixture is very dry still add
another 1-3 ml of water/ oz of E/
Then try heat again .
Keep alternating
until it is goo like melted taffy. this should fire with heat. for sure.
If
it is too wet, no problem, just put it on a heat source and let it boil very
lightly for 2.5 hours
The quality of the water is extremely important to the quality of the chili,
and to the yield.
Always used distilled water, and for even better results
run the distilled water through a Britta water filter to remove metals, and
other trash
Hydrogen Peroxide
If using recycled phosphorus some suggest using a capful of hydrogen
peroxide also.
I suggest you avoid using peroxide at all, if possible.
The reason is peroxide in an acid environment will digest many organic
molecules.
In addition peroxide will oxidize the RP,
In the reaction the
peroxide will change HI into I2.
The bad aspect of heat, is that
it tends to vaporize the HI . HI is reported to have a boiling point of
117 C, but this is a 58% solution with water.
The concentrations of HI
you are using is many times above that. 4 to 6.5 molar
By adding peroxide
some of this HI will turn into I2.
Peroxide will also strip off
organic molecules that may be stuck on the RP like wax, this refreshes the
RP at the same time providing I2,
and may be enough to kick in a dying
reaction.
Additional heat is my preference. But try it and judge for
yourself.
Cautionary Notes
Be prepared, the RP
hitting the I2 will often start the reaction.
It may be impossible to
see inside the flask, either from vapors or the rise of reactants. Either way,
if the surface of the reactants contents can not be seen, act fast, because
seconds count, shake it hard., or swirl the contents Keep swirling
until you can determine what is going on. Look for a nice easy bubbling.
If you fail to shake it down you will end up with very little, because the
thick smoke indicates a fire is going on in the flask, this will destroy
the E, or the contents of the flask may have expanded and are going to
soon blow down the hose, Hard shaking will stop both of these situations
allowing you to regain control, If you hesitate all will be lost
If
the mixture starts to rise up, too high, swirl it lightly
Shaking
before it blows out of the flask will save your whole reaction
, it will turn a potential disaster,
into a laughable "won't do that shit, again" story
Phosphorous fire in flask or spewing out.
Too hot of a reaction WHAT TO DO
vaporous HI acid and Phosphine (not phosgene)
Phosphorous fire not in the flask
The Reaction Proceedure . . . .
This reaction is exciting, and rapid. You must really focus your attention at
this point. It is of -primary importance, that you have your wits about you. It
is most difficult sometimes to determine if the reaction went to
completion, so observe as much as possible and you will be able to make a
determination.
Be sure to read Methhead's
reaction, and Placebos
reactions they are the best walk through. Eventually you will have the
steps memorized, then you will be able to note subtle differences between
the procedures,
Before long you will be able to design your own
procedure, this is when the fun begins. You become so aware and familiar with
the reagents and the process, that you transcend anything you can read, and
develop a sense for what to do. Creativity is the way to go, It becomes almost
impossible to fail after a while. Even if you try to screw up it still works.
Preparation and initiation of the phase one
reaction
Sometimes you will have to boot it out of phase one
into phase two, this may be accomplished in a variety of ways
Increase the heat
Add
peroxide
Add a little water
Add more I2
Add more RP
Simply shaking it well may be
enough
Add water to the reaction mixture 100 ml of water for every ounce of initial ephedrine after the reaction mixture has cooled sufficiently Boil the solution for a few minutes ( 5 minutes), this will finish the reaction and and react any remaining I2 with the RP save you time by not having to refilter the mixture several times as noted below Filtering and Purifying the Product -- GaKK Patrol
Filter using coffee filter and paper towel plug in a funnel If needed Re-filter through the same RP and filters again, continue refiltering until it has no added clearing effect. filtering should remove the cloudiness and most of the red color. It may require refilter 3 or 4 times. You end up with a clear yellow or colorless solution that can have many different odors. Can you identify the odor of meth,? If you don't refilter you may leave iodine in the stuff. Recycle the red phosphorous it is still good.
Trouble - If it refuses to clear with filtering, and remains red , and you see a iodine oil on the bottom of the flask, and it seems like iodine is everywhere!!! STOP, the reaction did not take. It is still possible to save your batch and obtain a good yield .
Collect the fluids, RP and iodine put back in flask, filter paper, water and all.
Add more I2 and RP, and a condenser and begin boiling lightly for many hours (2.5 - 4 ).You can even boil it in an open flask. You want to boil away most of the water. At the end of the boil,. it the contents are allowed to settle, there should be RP on the bottom and a yellow fluid on top. The yellow liquid is almost as viscous as motor oil.
SAVE everything until you are done and sure you have your chili Use a large glass or plastic vessel to store all the discharge in (a empty gallon water container is perfect) by spitball
To Avoid taking more than one a pH reading and still end up with great chili (click here)
Considering the shitty quality of muriatic acid, it would be great to
distill your own.
If you are consistently getting dope that smokes burns
dark and gakky , consider the source of your HCl probably also contains
sulfuric acid, and you might consider gassing it instead or distill your
HCl first.
Or simply do a recrystallization, which will give you "da
kine", smooth and sweet.
In this HCl water soluble form, it is usable,
and now illegal to posses without a
license
you may desire to
clean it up further if it is colored, stinky, gooey, tastes terrible. or
if you want a better product
Variations Notes and stuff- Variations are as numerous as the number of cooks, no two cooks use exactly the same methods and some cooks never do the same thing twice. However certain details are always the same no matter who does it.
- Some mix red and I2 first , some mix e and red, some add water at the beginning others add it later.
- some mix the reactants for hours, some barely mix them at all before beginning the reaction
- Heating the reactants before mixing is very dangerous and is 10 x as dangerous if you are using free base E. It will blow. The free base has to be handled carefully and not forced to react in any way.
- If doing over 1/2 oz and if not familiar with the free base, react the HCl salt instead.
- Variations -my latest heart throb is the use of sand placed inside of a wok or pan on the stove the reaction flask is placed in a depression in the hot sand and partially covered up. The value is the glassware does not contact the excessive heat of the stove top. Even heating, .A milder heating the sand takes a while to warm up so the reaction temperature slowly rises , This works great when evaporating solvents because the tendency toward over heating is reduced. The sand I use is the standard 60 or 30 pound washed silica sand from the hardware store it cost a couple of dollars for a 100 pound bag, the bag may not be easy for some to to carry, or even to pick up, so get some help if your not muscular . This is the same sand used in the sand filter the 60 pound is probably better it is finer grained.
- Variation - the common variation is to stir or not to stir. Certainly some mixing is desirable and too much mixing will quench the reaction. So somewhere in the middle find your niche between mixing and keeping the reaction alive.
- Definitely shake hard if things get out of control.
- It is important to be there when the phase two of the reaction kicks in, a little stirring here to keep the violent nature to a minimum and keep the reaction going is the critical link for a great yield or a pile of nothing at the end.
- Left to its own turbulent nature , if it is in a large flask the reaction will yield on the low side 50% to 70%.
- With optimal mild swirling to control the turbulence , the yield will approach 70% to 90% depending on the pills and other factors.
- Over stirring the reaction may not complete and you receive only Ephedrine as a product.
- Variation the application of heat is another area of differing opinions , some use heat no matter what others avoid it like the plague. The best method I believe is to simply add heat for a minute of two when needed to keep the reaction going.
- Use more if needed.
- All agree that too high of a temperature is not good for results.
- Dirty glassware, poor reagents, sloppy technique, from this point on affect your product in a big way.
- If you use soaps or detergents on your glassware, you introduce a sulfate that will turn your chili black and stinky when smoked
- Wash glassware with water and rinse with acetone, if something is stuck on the inside wash with acetone and salt, swirling the salt as an abrasive then rinse super good..
- At the end of the reaction, you may have heard of the chili being called an oil, well it looks golden, like an oil,
- but at this low pH (acidic), it is actually a water soluble salt of iodine.
- Considering the shitty quality of muriatic acid, it would be great to distill your own.
- If you are consistently getting dope that when smoked it burns dark, stinky and gakky, Most probably it will be fixed if you use more water in your washing of the fuel and free base. Be carefull to flush out the emmulsion with the waste water , that frothy, whitish, middle layer is full of crap. Use at least an amount of water equal to the volume of the fuel meth-base. your HCl first.
- Solubility, ions, polar, non-polar
- Variation- as to when to add the nonpolar solution is a common point of contention, you want a nice debate, this will get you into the middle of a fanatical argument. Generally it is a good idea to add the non-polar before adding the base, the non-polar attracts the free amine (free base) E and M and helps them move more rapidly out of the polar solution..
- However there are times when you do not want a non-polar compound mixed in, Steam distilling , contamination, or to observe the E and M changing solubility.
- The non-polar is not absolutely needed most of the time , it depends on concentration, it may give a better yield, and does move the E and M much faster.
- But unless you have a specific reason to not do so, most newbees would be advised to add some non-polar prior to adding the strong base. Experiment when you have a few cooks behind you.
- CAUTION adding NaOH too fast, to a hot solution is dangerous. Many bees premix a 20% NaOH solution and then add ice cubes to that, others add it straight .
- The idea is to get the pH up above pH 12.5.
- Contrary to some literature in Erowid's site, only the amines and very similar compounds have this unusual ability to freely change solubility from water to oil base when the pH is changed, the fact that this is an uncommon property is the reason the A/B has been so effective in thwarting DEA attempts to prevent the use of ephedrine.
- Morphine, codeine , heroine, and cocaine are common examples they have CH-CH skeletal structures with the N-H and OH groups exposed.
- The CH hydrocarbon chains and rings (aliphatic and aromatic) are what is a non-polar polar molecule, like methane CH4, or benzene C6H6
- The -OH adds a degree of ionic polar like quality as in methanol CH3-OH, or phenol C6H5-OH.
- But it is the mainly the nitrogen =NH changing to =NH2+ in the presence of excess H+(acid) that gives the legendary Hydrogen bonding and full water(polar)(ionic) solubility, along with attracting anions like -Cl.
- Hydrogen bonding is an ass kicking ionic bond that is 1/5 as attractive as a full bore covalent bond.
- Now that is some stickiness. You will find hydrogen bonding when N, O or Fluorine are present.
- Generally these three atoms determine if a hydrocarbon will be water soluble.
- Free ions are water soluble in acidic or basic solutions, it is only when the net charge is negated that they precipitate Ag+ + -Cl --> AgCl(insoluble)
Crush up, the chili in a bowl with minimum of dry cold acetone ( no water) Pour crystals and acetone into a filter Wash crystals by flushing with more dry acetone, until they are white, this removes the acetone soluble junk Optionally wash them with any of the non-polar solvents to remove non-polar soluble junk Wash off the non-polar solvent with acetone. Change to a clean collecting flask Keeping crystals in the same filter. Add denatured alcohol to dissolve the chili and leave most salts and insoluble crap behind. It may take 10 minutes for all the chili to fully dissolve For a quick clean evaporate the alcohol away
For a major purification use recrystallization
Boil the filtered alcohol/chili mixture until a slight skin begins to form on the alcohol, add about 10 ml of fresh alcohol to dissolve the skin again and add 20 ml of acetone, cover the container and place in freezer for 6 hours or more up to 24 hours, the longer the better and bigger will be the crystals. After the 6 hours, Filter the crystals cold and quickly, rinse lightly with a very small amount of ice cold alcohol, after the residual alcohol evaporates from the surface of the crystals this will give you some of the finest chili you have ever had. After washing with the alcohol as noted above , it is fun to place the crystals on a dark surface , spread them out to help the residual alcohol escape. Pull out the digital camera, and snap a few pictures of your beauties. These photos will be a source of enjoyment. Simply because it is rare to see so much stuff, looking so good. Soon it will be bagged and such and looses that magic quality of the untouched pure crystal. You will be one person in 1/2 of a million in the US that ever gets to see this.
Water Soluble Sulfates
If
your chili looks clean and white but when you vaporize it leaves a nasty
black residue , then you have water soluble sulfates that can be removed
using the recrystallization
method
Glass like shards and
crystals
To get the bigger clear glass crystals, the final
stage of drying should be slow, from dry alcohol seem best,
with a little acetone added, then was with alcohol only
This is the same as presented above in De-contamination
procedure
Re-crystallization of chili using methanol,
denatured alcohol, or 91% isopropyl alc. will grow some very pretty, large
crystals and will make your product more pure and much more potent. This is one
procedure that is simplicity itself and always produces a major
improvement with surprisingly little loss of product.
crystals, using denatured alc. and vision ware
(Worlock)
After the chili was pulled out of the toluene (non-polar solution)
using HCl and water, It was run through a filter and placed in a
vision ware bowl for evaporation. The water was evaporated leaving the
crude raw Crystals.
These were crushed and washed with ice cold dry acetone.
The washed Crystals were then dissolved in hot denatured alc. the alcohol
was boiled away until the first sign of skin forming or the first sign of
crystallization noted. Remove from the heat add enough alcohol to remove the
skinning so no more crystallization can be seen then add 20 ml of acetone, if it
turns cloudy add alcohol drop wise until it is clear again cover and place
in freezer 6 hours or more( overnight is great) you will return to find crystals
floating in the liquor.
Rapidly filter out the cold crystals , then wash
them with a little cold alcohol to remove any gakk on the surface and in the
outer crystal layer, set out to dry..
All three steps were performed without
ever removing the chili from the vision ware bowl.
Recrystallization details
The Chili is dissolved in a
minimum amount of dry alcohol, this is heated,
USING a Safety fan
(Always)
as needed to get it to dissolve , bring
it to a soft boil . Continue boiling until you begin to see the chili form
crystals on the surface of the alcohol. Known as the Lynrd
sign.,
(The Lynrd sign?? Skynrd?? The chili forms
a surface skin <yuk-yuk> it was a joke get it ?? Lynrd
Skynrd!!!)
This is a super saturated solution
. Add a little alcohol to dissolve the skin again, and add 20 ml of acetone
Then cover and set in freezer, as the temperature drops,
crystals will form .
Leave in freezer for 6 to 12 hours or even longer.
Generally the longer in the freezer the bigger and better will be the
crystals.
The chili re-crystallizes as the temperature drops, the alcohol
won't freeze.
As time goes on the crystals "digest".
Digestion means the crystals are slowly
re-modeled, the outer layers with impurities are stripped away a reform
without the impurities. In addition the smaller crystals dissolve and
become incorporated into the larger crystals because of volume(cubic) versus
surface area(square) considerations
After which the resulting crystals were
quickly cold filtered , washed with a little cold alcohol and
dried.
The crystals should be rinsed lightly with alcohol wash off any
of the mother liquor that is stuck to the crystals, and to remove the outer
layer of crystal which is slightly impure
note for even better results:
The super saturated solution(dissolved in
hot solvent) forms crystals faster than the hot but more dilute solution , but
the more dilute allows better digestion and more pure crystals.
Life is such
a trade off in every way.
Appearance:
The resulting crystals were sparkly, 1 cm x 2
mm x 0.5 mm very clear
up to 1 inch long and chunky
If at first you don't succeed , before you try it again, analyze what
went wrong !!!!
Other wise you will repeat the same error and will have
learned nothing
At first you may have failures,
mostly due to equipment or chemicals
Remember at this point you may
still be a little green, but you have taken the the plunge and you know much
more than you suspect you know. The amount you have learned at the hive is
enormous , so don't kid yourself into thinking your not getting it, more likely
than not your are so close, and just one little thing is stopping you.
Take advantage of a failure to learn maximally from it, A failure is an important tool, use it!!
To figure out what went wrong, Backtrack to the point that you first noticed something was not right, there is more than enough descriptions of what to look for and when you did not see what you expected to see, The error occurred immediately before that.
Believe in your own skills is what I am saying, because there is no way you could have gotten this far without developing major amounts of savvy about this stuff.
When in doubt, either put it on a light boil for two hours, or add more NaOH to bring the pH up.
One main cause of initial failure is your Chemicals, everything at
first is OTC because you have not yet developed the connections for supplies.,
and the OTC stuff has to be re-made to suit your needs.
The ephedrine must
be clean and the govt. is constantly tweaking the stuff. They will try
real hard to screw you over at least two times a year with their concoctions.
The Iodine the main source of energy for the reaction is touchy , if made
from tincture , wash it repeatedly by shaking it hard in a 2 liter container
(and not in a 4 ounce jar or by running water over it in a filter)
first wash it with "major" amounts of tap water for maybe 4-5
times , then finish it off with distilled water. You may think 4-5 washings is
excessive, but the last time I made some it was washed 8 times.
Use an
excess of iodine 1.5x to 2.0 x ratio if unsure.
RP is only a problem if match-book stuff is used, you need a shit load if from match strikers because the contaminants , glass specifically alters your weighing. I have never used the matchbook RP but I have listened to those that have, and it will work, from the amount of glass and trash that is likely to have remained in the RP it is a good idea to use an equal weight of MB RP and Ephedrine
The Equipment will be OK if you follow the sizes used here, once you go to
nano-sizes or to larger sizes you will begin to have problems, all
the equipment needs resizing together, you can not just get a bigger reaction
flask to make bigger batches, every step of the way you will be dogged by size
problems, if you do.
.
To prepare everything properly is a pain in the
ass , if doing it all OTC for the first time it may take you several days to
clean up the E and Iodine and RP., but it is the formula for success, if
it were easy anyone could do it, but everyone can't do this, it takes a
special touch, you either have it, or you must learn it.
Once you make a batch you become a major asset and people want what you can create , stuff begins to come to you as if by magic, I am amazed at what people will trade for a gram of this shit. They begin to bring you better chemicals, or you pay them in speed to acquire chems for you. and "Viola" your home free. then it is as easy as measuring it out and mixing it together.
As time goes on you become intimately familiar with the properties of these Chemicals, and it will seem too easy, you will know what to do instinctively,
You have seen it all now, at least once, so the best thing to do is to get
some experience behind you, and start cooking away, be a good observer..
90% of the screw ups are fixable easily, it is getting the stuff
to react that should be your primary focus. Once made you will get it out of the
solution, believe me you will find a way.
Save everything until absolutely sure that you have product or until you know
what went wrong.
I save everything until all the final product
accounted for.
recycle the I2 and Rp
even the nasty lye water
contains recyclable Iodine
Calculating Yield
You can use this web site
http://www.shef.ac.uk/chemistry/chemputer/reaction-yields.html
Enter these values(without the spaces)
C10 H15 N
O ---
Ephedrine Freebase
C10 H15 N O (HCl) --- Ephedrine HCl
C10 H15
N (HCl) --- Methamphetamine HCl
then enter the weights you have obtained in grams
weight of final Methamphetamine
------------------------------------- x 100% =
percentage by weight
weight of initial Ephedrine
example: yield by weight
If you began with 90 grams of Ephedrine,
and ended up with 70 grams of chili
70
--- x 100% =
77% by weight
90
(weight of final Methamphetamine-HCl / 186)
------------------------------------------ ------- x 100%
= percentage by molecule or mole
(weight of initial Ephedrine-HCl /
202)
example: yield by mole
If you began with 90 grams of Ephedrine, and
ended up with 70 grams of chili.
(70/186)
----------- x 100% = 84% by mole
(90/202)
The differemce of 16 mw units(202 - 186 = 16) is the molecular weight
of the oxygen that is removed from the ephedrine to make chili.