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Well first let me start off by saying that this is posted for informational purp

oses ONLY! Therefore if you use this information for purposes other then that, y
ou do so at your own risk, since you would most likely be breaking the law, and
WE don't break the law around here. Do WE. ;-)
That being said, the following were observations made by Gilligan during his vis
its with those well known Keebler elfs, that are always up to somethin via Methh
eads Push/Pull rxn.
First off there are no exact guidelines for this rxn, it is almost always observ
ed slightly different then the time before, but the recovered final product will
90% of the time be identical to the time before if the general idea of the rxn
is kept the same.
Meaning maybe one time it will run 1 1/2 hrs and another run 2 hours or say one
run had 1/2 gram less Red Phosphorus cause you ran short and the next had 1/2 gr
am more.
If the basic rxn concept is kept the same it will work like clock work each and
every time.
But Gilligan has only observed elfs using first class starting materials, so if
someone was to use less then first class starting materials they would be adding
their own varibles to the equation and if the rxn failed it could be attributed
directly to the use of less then first class starting materials.
First class meaning for the I2...Pure I2. Not recovered I2 from KI, or similar m
For Red Phosphorus...Red Phosphorus from chemical supplier. Not recovered from m
atch strikers.
And finally Psuedoephdrine Hydrochloride...Extracted from Nasal Decongestant, vi
a a acid/base extraction not those short-cut methods that have been posted as "t
he solution".
In Methheads own words "Short-cuts suck, DON'T use short cuts!"
The idea of this post wasn't to help with aquistion of materials so that isn't g
oing to be discussed. The I2 and Red Phosphorus well there isn't anything to be
discussed about preparation, it should be ready as is, if aquired the properly.
That leaves only the extraction of the Psuedoephedrine Hydrochloride which after
this we will refer to as Psuedo, to save time and space.
Gilligan has observed those pesky elfs getting extraction results of between 50%
and 75% of the starting weight of the psuedo (example 18grams @ 100% = 18gms//1
8gms @ 75% = 13.5gms) those elfs are sloppy but even under the best conditions d
on't expect your results to be higher then the 75% mark,
if you do get higher results then you'd be wise to refine your extraction techni
que due to the fact that those kind of results aren't typical and you most likel
y have impurities in your recovered Psuedo.
As for the technique, this was learned by those elfs while reading posts long si
nce gone, but credit still is due to Lone Ranger whether he is still around or n
1)Dissolve X amount of pills (preferably not time release pills, standard 30-60m
g pills are fine) in water
(good rule of thumb-Use between 2-3mls H2O per pill, no matter the mg of pill)

so for example: 200 60mg pills would require +/- 400-600mls H20.
Dissolve by whatever means you have, magnetic stirrer is the least work.
2)Filter any solids out of the mixture,
psuedo is water soluble so anything solid isn't wanted.
3)Ph the filtered solution to Ph 12.4,
the reason for the 12.4 is because psuedo has a Pka value of 9.4 meaning 3points
above that value and the psuedo will drop out of solution and can be extracted
with toluene.
4)Next add 50mls of toluene for each 100mls of Ph'd solution,
so using the example from above say 500mls starting solution plus the Sodium Hyd
roxide solution needed to bring the Ph to 12.4 maybe another 100mls giving us a
total of 600mls of solution to be extracted by 300mls of toluene.
Add both to your 1000ml sep funnel and invert to it 40 times,
dont forget to burp the funnel.
Then remove the toluene.
And add another 300mls of fresh toluene follow the inversion step again.
And after removing the toluene the second time,
it is a good idea to check the Ph and make sure it is still at 12.4, adjust as n
Now when adding the last 300mls toluene you'll probably want to add some regular
table salt to the mix,
this to help push the left over psuedo out of the water
and also lessen the chance of emulsions.
I don't want to go into how to solve emulsion problems, but don't over Ph the so
lution as this will result in a definite emulsion and the use of a solvent other
then toluene would be unwise too.
Now some may say 900mls of toluene is too much to use for the above example, but
remember if you are going to lose something while extracting why not make sure
you lessen those chances by making sure you have ample toluene to absorb the psu
edo and if an emulsion is formed and can't be seperated, you'll lose less due to
the fact that the discarded amount will be a smaller proportion (say 5mls) of t
he 900 mls used rather then say 300mls.
I'd sleep much easier knowning I dumped ONLY 5 mls while using 900mls then if I
had to dump 5mls while using ONLY 300mls. But who's sleeping anyway?!?:-)
5)Let the solvent set for awhile, so any droplets of the aqueous solution have a
chance to fall to the bottom, then pour off the solvent into a new beaker leavi
ng the water behind,
then if necessary the solvent can be dried by your prefered method, the use of C
alcium Sulfate (Drierite) works great,
just don't use indicating type as the solvent has a tendency to remove the blue
color if left in contact too long.
6)Set up your HCl gas generator,
simple one involves table salt and Sulfuric Acid (AND NO,I REPEAT NO HCl liquid!
You ask why? why if the salt is likely without H20 and the Sulfuric Acid is like
ly less then 10% H20 would you want to go and add something that is 63% H20?!? T
he object is to have as little water as possible.

The gas should then be dried through a gas dryer such as Sulfuric Acid since you
've already got that on hand.
And the final recovered product should then be heated to +/- 110'f to drive off
any left over solvent, since toluene's b.p. is 110'f.
As for the use of the freebase instead of the psuedo Hcl, Gilligan has observed
both ways and the HCl is the only way to go if you want predictable and acceptab
le results. If your into fireworks and don't care about the end result, then hav
e at the freebase.
The Keebler elfs use different ratios for the materials each time for no apparen
t reason,
but the basic idea is
1 part psuedo,
to 1/2 part Red Phosphorus for rxn runs of less then say 1 ounce psuedo,
more then 1 ounce then lower the Red Phosphorus to 1/3 part,
and the I2 is the one varible they play around with but hasn't shown great diffe
rencesin the end,
it must be NO less then 1 part or it is likely to cause incomplete conversion.
They have been seen using say 13-17gms for 9-10gms psuedo or say 15-18gms for 13
gms psuedo. The end always comes out the same though.
Next Gilligans observations of many runs has led him to draw his own hypothesis
about the steps of the rxn some of the basis for his hypothesis is drawn from wr
itten text also.
He ain't no rocket scientist but he does know his fair share.
The idea is-When all 3 components are mixed together,
if they are anhydrous(sp?) they will most of the time just sit there until ANY m
oisture is introduced at which time things start and aren't easily stopped.
Once going the idea is to keep the moisture down to a minimum since this is the
factor that decides whether things move quicker or slower
and when the HI comes in contact with water
the I2 wants to break apart from the H
and that is where the Red Phosphorus comes in,
it gets that free I2
and reintroduces it to another H
and the process restarts,
however if too much water is added to quickly it drives the I2 out too fast
this results in a incomplete reduction
or causes the rxn to stall causing the reaction to stop or
is incomplete due to the I2 being driven out and into the tank of water.

So the idea here is to let the reaction proceed with the addition of H20 kept t
o a minimum,
you can always add more water,
but you can't easily reverse the effect of flooding the rxn.
Once things have had time to react together for say an hour or so
the addition of H20 can be increased more rapidily then earlier.
Those elfs put the psuedo in the flask
then the Red Phosphorus in
and mix real well,
then ready the I2 ,
but prior to adding it they have been seen heating the flask as is,
one would assume possibly to drive out the moisture,
anyways after heated and it appears dry
they take it off the heat and let cool slightly
when cool enough to handle then
they quickly add the I2 and stopper it,
with a two hole stopper
one hole has the 3/8" tubing(found at home depot,
the opaque(sp?) type)
leading to the push/pull tanks usually 2 flat bottom 1000ml florence flasks
6/10ths full of water.
The other hole is fitted with a syringe or similar adding device.
Then A drop of water is added and things will start,
intermitently the flask is heated
and removed from heat once things look to be slowing down
another drop is added and again things start up along with slight to moderate p
ushing of the water in the tanks.
Then another drop say 10-15 mins along is added and then the flask is left on th
e heat
(Gilligan hasn't ever measured the temp but things can get real hot before you'l
l actually lose materials)
but let things get warm and then over the next say hour
you should maybe added 5-10 drops total,
during that time things should appear like a thick mud that is growing and bubbl
toward the last part of the hour things should be quite hot in the flask
to the point of where each drop added when it hits the bottom it instantly turn
s to vapor
and the tanks move heavily too.
Mixing or playing with the rxn isn't harmful either,
still sealed up mind you.
Once the hour to 1 1/2hr has been reached start adding water
say twice the rate as earlier,
since most of the conversion has been completed by now, probably.
To finish up the reaction and drive off the I2 that still appears as a purplish
color in the mixture you'll want to get the heat up to say 150' to 200'

and then start adding more water, once you get the water to a certain it point
it will suddenly cause the I2 to start disappering and the tanks likely will tu
rn yellowish,
at least the first one,
once the I2 is gone
it will become apparent by the Red Phosphorus color coming back
and being able to see into the flask without the mud sticking to the walls.
The one thing to note here is that it isn't necessary to get a "pull", for thin
gs to be complete.
Gilligan has never observed a pull in many runs and the results have never been
less then ideal.
When this occurs then you'll want to add alot more water.....
(example would be 300-500mls for a rxn starting with say 9-15gms psuedo/500-700m
ls for 20-25gms.
Then once your done you want to filter out the Red Phosphrous,
this will require at least 2 coffee filters doubled up possible more because th
e Red Phosphorus has a way of finding its way through the filter anyhow, so it m
ay need to be filtered twice, once filtered,
rinse the Red Phosphorus with very hot water,
reason for this is it does hold onto product and if it isn't rinsed with HOT wa
ter you'll end up short.
If you still had I2 left in the mixture or you think you did you can add Sodium
Thiosulfate a few crystals is fine,
but there shouldn't be any unless you overdosed to start with or added water to
quick. With regards to people opening the rxn and then throwing in additions wh
ile the rxn is going, it hasn't ever been observed by Gilligan, so he doesn't fe
el it is necessary and if your needing to do that then it is likely you've stray
ed from the basic concept idea.
It can be hard for someone who has never seen this rxn to think they can underst
and what they need to by just reading texts, and they expect it to go "word" for
word as someone writes up,
it is unlikely to happen that way.
Just get an idea of what is suppose to be happening like Gilligans hypothesisif
things seem to go in that genral direction then just work with it and try to fol
low the basic steps of progression.
The only things likely to happen would be to flood it, which isn't recoverable
from, without alot more knowledge then you would likely have or you wouldn't hav
e flooded it in the first place.
The other is less then ideal starting materials,
if you have to use less then ideal be prepared for less then ideal conditions t
o follow.
Not to say it won't work,
it is very possible it will, but if it doesn't you'll know why.
It is difficult to actually screw this reaction up to the point where you recov
er nothing,
unless the freebase is used, then you might as well flip a coin as to determine
the outcome cause it won't be predictable.
Laslty Gilligan didn't post this so that all the people well versed in the Chemi
stry part of the reaction (HI+H20-->H...Etc.) could show him where he was incorr
ect in his assumption of how the chemistry proceeded. This is for informational

purposes only, and isn't represented as factual. He has seen results and this is
his interpretation of those results, he ain't the professor ya know. If someone
thinks they know better, then post away. The reason for this post was to give i
nsight as to the workings of this rxn, from Skipper's "little buddie" point of v
iew. Thanks to those pesky Keebler Elves too ;-) Pyrex out of space to type
Sorry I didn't get back to ya sooner, but in regards to the temperature that wou
ld be F, should have made it clearer. And thanks for bringing this thread back
:-) For anyone who is interested here are some additional things that have been
noted since then-->Firstly this is only an observation NOT fact, but it does ap
pear that the higher the temp goes inside the reaction vessel the more likely th
e sideproduct of P2P is likely to form. Now this doesn't mean everyone should c
rank up the heat and try to make P2P from this reaction cause it ain't going to
happen that way. What I mean is that observations have been made that make it a
ppear that when this reaction is run and the heat is run say above 150'C but bel
ow 175'C that there is usually a small byproduct of P2P present in the final rea
ction mix, which if this occurs in your reaction you will have NO trouble tellin
g, as the fruity smell is like no other smell involved in this reaction...mmmm m
mm good! Now this is just a hypothesis since it wasn't completly possible to ho
ld all the varibles constant while only the heat was changed. This was attempte
d but there always seems to be something that gets out of line and therefore lea
ves the door open for something else to be causing this P2P formation other then
the heat. But in addition it was noted that when the heat was not allowed to g
o above say 125'C that the formation of P2P was not evident. So between these t
wo type observations it was thought that it would be the high heat that is respo
nsible for the P2P. But you can draw your own conclusions or do your own observ
ations, while your sleeping of course ;-) since any other way would likely be br
eaking the law. One other thing that might be useful to someone who might be wo
ndering whether or not their reaction actually worked or not would be that you c
an usually determine alot by your final reaction solution (the mixture of the re
actants mixed with DH20 and filtered of the Red P. You'll need access to a digi
tal Ph meter to do this...Check the Ph of the solution. Is it 0.25-0.75 Ph? If
so then it is likley you will be rewarded for your knowledge and hard work, cau
se the Ph wouldn't be wayy down there unless a very strong acid was formed durin
g the reaction (HI). Now when Ph'ing the solution, does it appear to resist cha
nge by requiring a considerable amount of NaOH solution before the Ph rises?? I
f so there is another good sign. And most importantly when you hit the Ph of be
tween 10.5 and 12 do you notice little droplettes of oil floating to the surface
?? If so then you know your SHI*! And the reason I say that is, because of all
the possible things that could be in that solution your Ph'ing, there is only on
e that has those properties and that would be Honey. By the way for those of yo
u who are newbees you don't stop Ph'ing at 12...the reason I didn't go farther t
hen that was cause that was as far as you'll need to go when looking for indicat
or signs. Once at 12 it would be a good idea to add your non-polar solvent (Rec
ommended solvent is Toluene)and finish up the Ph'ing until you are at 13+. The
solvent is added at 12 to give the freebase somewhere to go in case it is unhapp
y sitting on top of the Polar solution :-) And the last note is that reaction t
imes don't always need to be as high or higher then 1 1/2 hours, as observations
have been made that show that complete conversion can occur in less then one ho
ur, or at least as complete as was discernable by methods of testing that didn't
include a laboratory. Well there are your added tips, Good Luck and BEE safe!
Pyrex out of room to type