(too old to reply)
Electrolytic part 1
R***@Limestine.com
2005-04-25 13:38:58 UTC
So much has been written on Electrolytic reduction of Ephedrine that P will be posting it
in parts, Several Bees were working on it at the same tome, each in a different location ,
each with different methods.
If you follow the thread it will become apparent who the main players werwe/are.
This is pure hive jive.

The first is are[port by dwarfer to this news group
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From ***@aol.com Mon Feb 08 15:13:59 1999

Subject: Re: Interesting electrochemical process
Lines: 340

Xref: rQ alt.drugs.chemistry:54516
: alt.drugs.chemistry

http://www.lycaeum.org/~strike/cgi-bin/ubb_cgi/Ultimate.cgi


More excerpts

Go to section entitled "crystal meth", or "general discussion". look around,
use the search engine for "pressurized" or some what. If you cannot find what
you are looking for: wait, maybe i have this copied


the Hive BB
General Discussion
Peer review of sealed electrocatalytic method

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Author Topic: Peer review of sealed electrocatalytic method
dwarfer posted 01-25-99 07:24 PM CT (US)

Ok, I'll admit that I'm just full of myself with the success I have

found in a sealed 70 PSI electrocatalytic, cheap and easy,
apparatus, and I find myself going around to threads that were
helpful in providing impetus and knowledge, and posting I DID IT
AND
IT WORKS messages. There has to be a better way without becoming
obnoxious.
Is there a preferred way or place to do this? Do I just post it and

see what happens?
Is it "novel" enough to go into that subsection?
Or should i just run around and say "I did it I did it it really
works ohman you gotta try this its SO easy and cheap and its So
good
you won't believe it."???
Nah. Beneath my dignity. [Rite!]






dwarfer posted 01-25-99 03:36 PM CT (US)

Palladium and Barracuda 1965, here is the way to make the "Fester"
method work, cheap and easy, no smells, guaranteed or your money
back. Actually I think that this is the method Fester was refering
to in his post in the thread started by Strike, in which he said
something like "I think this technique is passe', but how can I
turn
you on to advanced techniques if you cannot master this one", or
words to that effect.
The "advanced technique" imho is pressurization, and the reason I
think it is is that when I ASKED if it were, I got no response and
therefore using inverse upside down scatological reverse
psychological intuitive guesswork....nevermind!
Go down to your local Payless Cashways, Home Depot, or other large
warehouse building materials dealer, and check out the availability

of threaded plastic couplings.
Find somthing that correllates to the outside diameter of a flower
pot, located in the same complex. (pick up the smallest flower pots

you can and carry them to the plastic fittings department. )
I selected a 3 inch pot: do not go bigger. (Safety concerns arising

from presssure, as you will see.)
There are several combos that will work, but starting from the
bottom up in my setup, it goes
1. plastic end piece glue welded to
2. 3" long female threaded piece.
threaded to
3. 3" long male threaded piece with
4. flower pot with hole epoxied shut epoxied into upper smooth bore

section with
5. another 3 inch long female threaded piece, threads upward, glue
welded above the rim of the pot. (Since the rim of the pot
precludes
the normal interference fit, use lots of glue here)
and finally,
5. a threaded "stopper" to seal up the upper threaded hole.
Since you have studied the original posts, I probably do not have
to
say more about what to do, but there are two more salients:
Drill and thread a hole in the "stopper" to take a pressure gauge,
available at "tools r us" or whatever, for about 10 simoleans.
You can unscrew the cathode chamber to add whatever stuff you want
to reduce: you can also make addition valves out of valves from the

"drip systems" section of the same department store, but you have
to
make the valves have an additional security by having them in the
threaded sections so that you can rotate them 90 degrees to enable
them to line up when you want to.
It is important to have such a valve in the top, in the case that
you need to "burp" the system to release overpressure.
I was disappointed to note that I got no response from the hive in
regard to safety concerns related to pressurized confinement of
chlorine and hydrogen: my concerns are abated by the 4 experiments
I
have conducted with no mishap, and the input from an on line
chemist
who assured me that there was no problem unless the confined
halogen
was flourine.

{NOTER: USE DILUTED H2SO4!)
I further communicated with him about pre pressurization of the
system with a Schraeder valve and tire pump: he had a concern about

that and said it would be far better to use nitrogen. I countered
with the acceptability of CO2, and he said that would be OK. CO2
cartridge systems are available as bicycle pump replacements from
your local bike shop.
I have not done this yet: it requires a tubeless tire valve
addition
to the "stopper".
It would be better to increase the volume of the "headspace" above
the anolyte in order to have a more gradual pressure change as the
reaction progresses.
I have used BOTH the lambskin AND the pot as semipermeable
membranes: it may be unnecessary but since it works I'm stickin' to

it.
The device is scaleable to larger volumes through the simple
expedient of inserting a longer "pipe" in the cathode wall. pi X
r^2
X height, if I recall correctly.
The height of the above is right at 1', makes no smells, could
probably be made to run unsupervised after experimentation in re
amperage vs pressure is refined: does NOT require Pd cathode (AG
works: PD/C has been used by me and is a lot less expensive:
eventually I'll try AG alone)
Oh yeah: pipe is "rated" to 60PSI: I have run up to 100 PSI
(accidentally): my understanding is that anything above 70 PSI is
unnecessary. (Why is that the magic number??)
Palladium, give this a try and you'll never have to worry about
gettin' more of that iodine! I certainly would be delighted to hear

of improvements you might suggest to this apparatus. I'm proud as
can be about the fact that this WORKS, but there are many
improvements that I have not considered, I'm sure!
And, this stuff is
SO FINE!!!!!!!!!
dANCE Baby dANCE!!


fj posted 01-27-99 04:01 PM CT (US)

dwarfer, the process and parts are jazz, but I'm missing some of
the
mechanix on the inside. Is the pressure in this thing
self-equalizing over the anolyte and catholyte? What I mean is, is
the flowerpot fit loosely, so that gas from the cathode goes up
easily into the upper chamber? Also, how are you sealing the holes
for the elec leads and gauge. Just the tape? muchos gracias

dwarfer posted 01-27-99 07:47 PM CT (US)

Yeah, the H2 blows through the pottery like it was nothin. Well,
actually I do not know if it was "nothin": I could not measure the
pressure in the cathode chamber: but looking down in the unsealed
upper anode chamber
(Prior apparatus: Face shield on: hose running outside door!!)
bubbles were appearing around the outside upper edge of the inside
of the pot. (the portion that was in the cahode chamber: obviously
not the part that is glued to the plastic wall.) There was in
essence an annular ring not filled with the catholyte which
collected the hydrogen, and it was passing through the pot. I do
not
know the molecular size of H2, but it is purty tiny: and as you
know
water will soak through a pot, and it (H2O) is someplace between 10

and 100 times as big a molecule. Plus, it has a polar moment, that
H2 doesn't.
Thats why I use the Lambskin also: (Although it isn't the type
specified): just to be on the safe side. (That's ALWAYS the reason
I
use a condom! :< ) )
I epoxy in the wires. (But make the holes as tight as you can and
still pull the wires through.) Be sure to leave enough "slack"
INSIDE the chambers so that you can "flop them out" if you want to
mess with them. The silver one I put in with about 3 "coils" of
wire
beneath it.
I've been sanding it up and re-"anodizing" it per instructions
elsewhere, but I confess ignorance as regards the "why" of it.
(Well, I know why I sand it: surface area) Firstly, I would think
"anodizing" would take place at an "anode" wouldn't you?
I really do not understand catalysts and WHY they work: I suspect
it
may be over my head, although this projection is based on my
assumption that it involves quantum dynamics.
Interestingly enough in all the chemistry courses I took there was
VERY LITTLE about catalysts: just the definition. AND, there was
very little more on electro assisted chemistry.
Oh, pardon the disjoint: because of the SEVERITY OF CONSEQUENCE of
a
spark in the anode headspace, (with Cl2 and H2) I have about 4
wraps
of the wire around the carbon welding rod, and I use that
Aluminox??
stuff to ASSURE good contact. (Comes in a small white tube, I think

it is a light grease infused with carbon: used on aluminum wires in

household circuits to eliminate the hazard associated with aluminum

house wiring. THAT hazard arises from the expansion and contraction

of the aluminum wire over thousands of cycles of on\off: which
gives
rise to an "annealing?" of the aluminum; it eventually begins to
minutely ARC, that causes GREATER heating, and eventually you have
a
fire. THIS stuff makes sure that the arcing never happens because
it
is a good conductor in its own right.)
You know, these start out to be small little answers!
After wrapping the wire around the carbon, smearing on some
Aluminox, and tying the wire back to itself and pigtailing it to
assure tightness, I kinda monkey with the wire to make a
multi-turned (about 3 to 5 turns) not tight but not loose spiral
loop, slide on the condom and "unscrew" the electrode (you gotta
visualize this) which expands the loops of wire, which presses out
the condom and provides a convenient hangar for same. you can use
whatever you dream up to attach, or hold, the condom up to the
wire.
I use a couple of pieces of solid core about 8 guage covered
insulated copper wire whose ends I have sealed with epoxy.
You will have enough slack at the top of the condom to drape it
around the wire: the clip can be pretty "soft" and still be
effective. I also made a couple out of plastic coffee can lids,
like
an old fashioned wood clotheshangar: the plastic wa too soft, but a

little better grade of plastic would work. I think the plastic
paper
clips would be ideal, and I'm going to get some next time I see
them.
If you cannot arrange the wire to your satisfaction to hold open
the
primary anode cell, you CAN successfully manufacture a "hold open
device spacer" from the coffee can lids.
I'm probably getting involved in too much minutia here: these are
just what I did, with available materials. I'll bet you will have
better answers to some of the dilemmas that face you when you
construct this baby.
Go for it!

fj posted 01-27-99 08:03 PM CT (US)

Damn I thought I could dual-use it as a home defense cannon. heheh
This design is pretty cool, you deserve to be congratulated.

dwarfer posted 01-27-99 08:21 PM CT (US)

I never fail to be amazed at the personal difference that
consideration of anothers perspective can give rise to.
You could not in my apparatus leave the pot "loose" in the
structure: the anolyte covers the pot entirely: if it were loose it

would mess up the separation. (Of anolyte and catholyte)
Also, I was guided by prior posts that recommended that the
catholyte not be in contact with the air, and it was that fact that

started me down the path I have taken.
In the step-wise evolution of the "dwarfer" machine the sealed
cathode chamber was to exclude air, : I then read about pressure
maybe being "the answer", and I thought of the feed tubes (which
were also "burp" tubes) being filled and elevated up about 5
stories
(Wasn't lookin' forward to climbin' that TREE, but I was Workin on
it, dammit!)
Then I got a concern about the flower pot taking the pressure,
again
a consideration arising from someone elses post. Actually, I have
no
problem with a 3" pot taking this pressure, but (1) acids under
pressure bothers me; and (2) deterioration of the pot bothered me.
(Clays have an ionic bond that holds them together: and as I have
noted, acids concern me, and I do not know enough about electric
currents effect on clays to be confident)[ But I HAVE torn up some
pots making NaOH from table salt: much more current, though!)
Anyway, thats when I tried to engineer the seriousness of "Pot
Failure" out of the loop by encasing the whole shebang: no pressure

differential of substance across the pottery!
OF course that swapped a physical failure hazard for an explosion
hazard (confinement of potentially reactive gasses): not a good
trade on the face of it, but in my considered opinion actually a
good one. (Several other benefits: particularly the ability to
measure pressure.)
ANYWAY back to the point of ANOTHER "short" missive that has taken
on a life of it's own:
I do not know if there WOULD be a problem with an independant
flower
pot not sealed to the sides of the chamber: I would suspect that
the
H2 would keep the Cl2 "blown out " of the cathode chamber, but I
really do not know if there would be a problem even IF the Cl2 was
in a gaseous form over the catholyte.
I suspect it would not be a good idea, but the seriousness of the
issue could be commented on by others: or be a subject for your own

experimentation!
If it were not a problem (although I suspect it may be) I suppose
the pot could be done away with in theory: but it DOES make a good
"standing place" for the anode, and it DOES, I think, make the
charge source as "seen" by the cathode more diffuse and
symettrical.

When you think about it the pot is semi permeable as regards ionic
species that flow across it, and permeable as regards H2.
Anybody know why no further functional benefit is realized as
pressure exceeds 72 PSI, as alleged by my on-line chemistry magus??
http://www.lycaeum.org/~strike/cgi-bin/ubb_cgi/Ultimate.cgi

Go to section entitled "crystal meth", or "general discussion". look around,
use the search engine for "pressurized" or some what. If you cannot find what
you are looking for: wait, maybe i have this copied


the Hive BB
General Discussion
Peer review of sealed electrocatalytic method










99999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999999




Unknown
Introductory University Chemistry
Applications of Electrochemistry
Electrolysis: Principles
When an electric current is forced to pass through an electrolyte or electrolyte solution,
chemical reactions take place both at the anode and at the cathode. The stoichiometry of
these reactions obeys Faraday's laws of electrolysis. However, when several different
reactions are possible at an electrode of an electrolytic cell then the process which
actually does take place will be determined by the potential of the electrode. The
reactions which take place in electrolytic cells are those reactions which require the
least potential difference between the two electrodes.

The reactions which occur at the electrodes during electrolysis will be the oxidation and
the reduction of the solvent unless some solute is more easily oxidized or reduced than is
the solvent. Electrolysis of an aqueous solution of Na2SO4 will produce hydrogen at the
cathode and oxygen at the anode because reduction of H+(aq) is easier than is reduction of
Na+(aq) and oxidation of water is easier than is oxidation of aqueous sulfate ion. The
actual potentials will be close to the standard potentials, and the standard potential of
H+(aq)/H2(g) is less negative than is the standard potential of Na+(aq)/Na, while the
standard potential of O2(g)/H2O is less positive than the standard potential of sulfate
oxidation. The standard potential of sulfate oxidation is so positive that it is
meaningless in aqueous solutions, in which no higher oxidation state than six has been
found for sulfur.

Electrolysis of an aqueous solution of copper sulfate will produce copper at the cathode,
because both the Cu2+/Cu+ and Cu+/Cu couples have standard potentials which are
considerably less negative than the standard potential of hydrogen. The electrolysis will
again produce oxygen at the anode, because Cu2+(aq) cannot be further oxidized in aqueous
solution.

Electrolysis of an aqueous solution of NaBr will produce hydrogen at the cathode, as the
aqueous sodium sulfate solution did, because neither Na+(aq) nor Br-(aq) can be reduced at
potentials which are less negative than standard hydrogen. The electrolysis of aqueous
NaBr solutions will produce bromine at the anode because the standard potential of bromide
oxidation is less positive than that of the oxidation of water.

Electrolysis of a solution of aqueous CuBr2 will produce copper at the cathode and bromine
at the anode because these are the least negative possible reduction and the least
positive possible oxidation reactions in that solution. The anode reaction in any
electrolysis will always be the oxidation which occurs at the least positive potential and
the cathode reaction will always be the reduction which occurs at the least negative
potential.

Potentials which are not reversible have values which depend on the current which flows
through them. The difference between the reversible potential of an electrode and its
actual potential when current does flow through it is called overpotential. The
overpotential depends upon the current and other electrode conditions and its
determination is beyond our scope. However, when currents through aqueous electrodes are
small or moderate the overpotentials at those electrodes are generally not more than a few
mV unless the electrode reaction consumes or generates a gas.

Electrode reactions involving gas evolution can have overpotentials as high as a full
volt. Overpotential can lead to different electrode processes in the electrolysis of
aqueous solutions.
Example. An aqueous solution is 1.0 molar in Pb2+ and 1.0 molar in Sn2+, as well as 1.0
molar in H+; the other ions present are electrochemically inert. The reactions which will
occur on electrolysis and the reversible cell potential under standard conditions can be
determined as follows.

The anode reaction will be Sn2+ --> Sn4+ + 2e- at +0.1539 V, since oxidation of water to
produce oxygen could occur only at a much more positive potential. The cathode reaction at
first would appear to be 2H+ + 2e- --> H2(g) at 0.000 V, and on platinum electrodes this
might be observed, but on most metals hydrogen overpotential is at least 0.5 V. With any
significant overpotential the cathode reaction will be Pb2+ + 2e- --> Pb at -0.1266 V,
which will occur in preference to Sn2+ + 2e- --> Sn at -0.1410 V. The usual cell potential
difference will then be DE0 = 0.2805 V, the lead electrode being negative.
[NEXT: Electrolytic Processes: Metals]
[PREVIOUS: Electrochemical Power Sources]
[MAIN HEAD] [COURSE OUTLINE]
Copyright 1995 James A. Plambeck (***@ualberta.ca). Updated



oooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooooo



the Hive BB
Crystal Meth
Electrocatalytic Hydrogenation

Post New Topic Post A Reply
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Author Topic: Electrocatalytic Hydrogenation
Wizard X
Member posted 10-29-98 06:40 PM Click Here to See the Profile for Wizard X
Supplementary Procedure for Festers Method
DISCLAIMER : THE FOLLOWING INFORMATION IS FOR INFORMATIONAL
PURPOSES OR ACADEMIC STUDY ONLY. CHECK YOUR LOCAL, STATE AND
FEDERAL LAWS, AND PROCURE THE NECESSARY PERMITS BEFORE
UNDERTAKING ANY OF THE REACTIONS DESCRIBED BELOW.
WIZARD X SHALL NOT BE HELD LIABLE AND INDEMNIFIED FROM IMPEACHMENT
FOR THE USE, MISUSE, INJURY, DEATH, IMPRISIONMENT OR FELLATION DUE TO THE
APPLICATION OF THIS INFORMATION.

PERFACE

Let me begin firstly, and congratulate Fester and Bozakium in publishing this procedure.
And all the busy bees in the Hive in attempting too do or keep the dream alive.

I have been reading the Hive BB on this topic and decided to give all you busy bees some
help. Also Fester and Bozakium can use my dreams and ideas, as we all are buzzing in the
same Hive.

In this revised supplementary procedure of Festers hydrogenation I will dream of 70% - 90%
yields. dreaming of 90% greater yields using this method is pure BS as medium to high
hydrogen pressure is needed. There is however, only one method that I know that gives 100%
yield at one normal hydrogen atmosphere ( 1Atm ) pressure, at 10 deg C, for 20 hours
hydrogenation. The catalyst however, is very very difficult to make.

The greater efficiency in this revised supplementary procedure is due to cell design and
hydrogen adsorbtion.

Let's Begin !

CONTENTS

1 Power Supplies

2 Current Regulator

3 Tests : [ 1 ] Ester test
[ 2 ] Polarity test

4 Catalyst : 30 % Palladium on Carbon

5 Cell Dividers

6 Cell Design

7 Cell Resistance

8 Multiple Parallel Cell Arrangement

9 Revised Supplementary Procedure


POWER SUPPLIES

The power supply is important, but not crucial. Have two power packs that step-down from
the mains :
( 1 ) 12 Volt, 1.5 - 2 Amps and ( 2 ) 12 - 15 Volts, voltage regulated if possible at 350
mA to 500 mA.
Power pack 1 is used to pre-treat or anodize the Pd ingot, and nothing more. Power pack 2
is used in the main electrocatalytic hydrogenation. Simply there is no need to try and
lower the current from Power pack 1 down to a useful level. Power packs are cheap and
easy.

CURRENT REGULATOR
Look at file D_1 Figure 1.

This circuit is optional, but it does two things, regulate and fix the voltage by the
Zener diode, and the current regulated by the transistor BC 640. The wire wound variable
resistor determines or sets the regulated amount of current, sent through the ammeter. The
transistor BC 640 can handle up to 1 Amp at its collector, but use no more then 900 - 950
mA.


TESTS

ESTER TEST : Hydroxamic acid test for esters.
By comparing the colour of two samples produced before the hydrogenation and after, you
can determine the amount of ester reduced ( hydrogenated ).

Pre - test : To 1 drop of the Ephedrine acetic ester mixture in a small test tube before
the hydrogenation, add 1ml of 95% ethanol and 1ml of 1N HCl. Then add 1 drops of 5 % iron
( III ) chloride solution. If a violet , blue , red or orange colour develops, then the
test below can not be used as something ( contamination ) else is reacting with the iron (
III ) chloride.

[ 1 ] Place 3 drops of the Ephedrine acetic ester in a small test tube before the
hydrogenation. Place another 3 drops in a second small test tube after the
electrocatalytic hydrogenation is complete. Now add to both test tubes 3 drops of a
saturated solution of Hydroxylamine hydrochloride in methanol ( or 1ml of a 6 % solution
of Hydroxylamine hydrochloride in methanol to both test tubes ).
[ 2 ] Add to both test tubes 6 drops of saturated Potassium hydroxide in methanol
solution, or until distinctly alkaline to litmus. Remember add to both test tubes equal
amounts. Heat the mixture gentle just to boil, the cool to room temperature.
[ 3 ] Acidify both test tubes with equal amounts of dilute HCl ( 2N ) and then add to both
test tubes 2 drops of 5 % iron ( III ) chloride solution. A reddish ( burgundy ) or violet
( magenta ) colour will indicated the presents of ester.
Sample taken before hydrogenation is the control, assuming 100% Ephedrine converted into
the acetic ester.
The second test tube having the sample after the electrocatalytic hydrogenation will
indicate the amount of ester not hydrogenated.

POLARITY TEST

Look at file D_1 Figure 3.

Some power supplies have the current flowing from positive + to negative - And so, errors
can occur when wiring up the cell. To ensure that this does not happen follow this
polarity test procedure. When current flows in the A lead ( anode, long lead ) of a Light
Emitting Diode, and out the K lead ( cathode, short lead ) it glows. If it is reversed it
does not. Solder a 560 ohm resistor on the A lead ( anode, long lead ) making sure not to
over heat the lead. The A lead with resistor connects (wired ) to the positive + terminal
of the power supply, and the K lead connects (wired ) to the Pd ingot. Now, connect (wired
) the Pb electrode to the negative - terminal. By touching the two electrodes together (
make sure clean oxide free surface ), if the LED glows then the current polarity is
correct. The current is flowing from positive + to negative - .This means the positive +
terminal is the cathode and reduction occurs, and the negative - terminal is the anode
where oxidation occurs.

If the LED does not glow, then reverse the wires at the terminals. Make sure at all times
good connection is made.

REMEMBER ! ONCE YOU HAVE DETERMINED THE POLARITIES OF THE ELECTRODES, REMOVE THE LED
TESTER FROM THE CELL CIRCUIT.


CATALYST : 30 % PALLADIUM ON CARBON

Palladium is the superior catalyst in this reaction. Platinum is the second, but can also
attack the aromatic ring of the Ephedrine.

30 % Palladium on Carbon preparation. Prepare a solution of 8.25 grams of palladium
chloride, or 9.93 grams of palladium chloride dihydrate in 5 mls of concentrated
hydrochloric acid ( HCl ) and dilute with 50 mls of distilled water. Cool the solution in
an ice-salt bath and add 50 mls of 40 % formaldehyde solution and 11grams of acid-washed
activated charcoal. ( Any of the commercial forms of activated charcoal, "Norit or Darco",
may be employed ; the carbon should be heated on a steam bath with 10 % nitric acid for
2-3 hours, and then washed free of acid with distilled water and dried at 100 deg C before
use. )

Stir the mixture mechanically and add a solution of 50 grams of potassium hydroxide in 50
mls of water, keeping the temperature below 5 deg C. When the addition is complete, raise
the temperature to 60 deg C for 15 minutes. Wash the catalyst thoroughly by decantation
with distilled water and finally with 1N acetic acid. Collect on a suction filter and wash
with distilled water until free from chlorides and alkali. Dry at 100 deg C, and store in
a desiccator.

This makes plenty of catalyst ( approx 12 grams ) for many runs, as only half a gram is
needed for each run. The catalyst used in that run is filtered and used again, and again
until that first half a grams becomes non-active. Usually, 10-15 runs per half a grams.


CELL DIVIDERS

Look at file D_1 Figure 2. The green colour denotes the porous diaphragm or membrane.


Figure 2 a : filter paper extraction thimbles, used in Soxhlet extraction apparatus.

Figure 2 b : plastic tube ( PVC, Plexiglass, Acrylic, ect ) or glass tube with a disc of
Whatmans acid-hardened filter paper or Whatmans glass-fiber filter paper, glued with epoxy
glue or the plastic made soft with a solvent. Make sure you create a good seal between the
plastic tube and the filter paper disc. Acrylic plastic tube placed vertically on a
chloroform soaked filter paper disc and held there, with pressure, until the solvent dries
works well. Place the chloroform soaked filter paper disc on a sheet of glass , not
plastic.

Figure 2 c : same as above, with the plastic tube material or glass tube, but the material
used in the porous diaphragm or membrane can be made of ( 1 ) Fiberfrax ( ceramic fiber )
paper or finely woven cloth, ( 2 ) Fiberglass (glass fiber ) paper or finely woven cloth,
( 3 ) Carbonfiber ( graphite fiber ) paper or finely woven cloth,
( 4 ) Asbestos ( asbestos fiber ) paper or finely woven cloth. The porous diaphragm or
membrane properties can be improved by impregnating the paper or cloth with a
methylcellulose gel. The gel is formed by impregnating the paper or cloth with a hot
solution of methylcellulose in dimethylformamide solvent and allowing it to cool.

Figure 2 d : extraction thimbles as used in the Soxhlet extraction apparatus can be
purchased as glass walled tubes with sintered glass porous frits. Use a fine porous frit.

Finally, potassium hydrogen sulphate ( KHSO4 ) agar gel salt bridge or plugs can be used,
but with great care.
To make the salt agar gel the procedure is : heat 100mls of distilled water in a 250 ml
Erlenmeyer flask just to boil and then place on a steam bath. Add 3.5 grams of agar
powder, stir, and continue to heat until a uniform suspension is formed. Then, add 34
grams of potassium hydrogen sulphate ( KHSO4 ) and stir until it goes into solution. Cool
the mixture to about 40 deg C, this will not allow the agar to gel, but keeps it liquid
for use. The agar gels at room temperature. When making a agar gel salt bridge using a U
shaped tube, try not to get air bubbles in the gelled agar, keep it uniform.
Finally, plugs of this salt agar gel can be made by adding the liquid gel mixture to
Figure 2b & 2c type cell dividers.

Also, you can stretch the condom, as used in Festers procedure over a plastic tube ( PVC,
Plexiglass, Acrylic, ect )
to obtain a more permeable membrane.


CELL DESIGN
Look at file D_1 C1 to C5

Keep the temperature of the electrolyte between 20 to 25 deg C.

C 1: You can purchase cell divided apparatus with a sintered glass frit.

C 2 : Make the cell divider 2 / 3 the diameter of the glass container ( beaker ), this
will keep cell resistance low.

C 3 : Same setup as in C 2 , but the cathode is a copper foil plated with Pd , and wrapped
around the cell divider with gas venting spacers inbetween the cell divider wall and
copper foil. Remember the current density is for the entire copper foil area , and only
expose the Pd plated area to the electrolyte. The copper foil ( clean from oxides and
grease, oil etc) can be plated by placing it in a concentrated solution of palladium
chloride PdCl 2 ,or it an be done at the cathode in the concentrated solution of palladium
chloride electrochemically.

C 4 : Straight forward , look at the diagram.

C 5 : Use a glass walled , fine sintered glass frit cell divider. A large rubber bung with
holes ( red colour ) through the top allowing the cell divider and electrodes into the
cell. The cell must be absolutely sealed and air tight so no hydrogen gas escapes. A
pressure equalization system is setup so the hydrogen pressure does not build up too great
and explode the cell. This is done by filling a large test-tube , 2 / 3 with glycerine and
immersing a glass tube almost to the bottom. See the diagram. The cathode can be suspended
by using a copper wire through a glass tube, and making contact with the Pd ingot fixed to
it by drilling a small hole in the Pd ingot and crimpping the copper wire in the hole and
finally sealing the end by melting the glass . Seal all exposed copper wire with epoxy
resin.


CELL RESISTANCE

Each electrolytic cell constructed with different materials , cell dividers , and
electrolytes has an internal resistance that is different. Using Ohms Law V = IR, you can
determine the maximum resistance at a particular voltage and current. If V = 12 volts and
I = 0.3 amps, then 40 ohms is the maximum cell resistance. This means if you measure the
cell resistance by connecting a multimeter set at low Ohms, on the Pd and Pb electrodes (
disconnecting the power source ) just before beginning the electrocatalytic hydrogenation
, the cell resistance is determined. If it is greater than 40 ohms then a 0.3 amp current
will not flow at that voltage AND heat is generated.

REMEMBER : THE GREATER THE CELL RESISTANCE IS THE LESS CURRENT FLOWS AND MORE HEAT IS
GENERATED.


MULTIPLE PARALLEL CELL ARRANGEMENT

Multiple parallel cell arrangement can be performed from a single power source ( power
pack ) by connection the cells in PARALLEL. This lowers the resistance. DO NOT CONNECT IN
SERIES.


PARALLEL CELL ARRANGEMENT RESISTANCE FORMULA : 1 / R = ( 1 / R 1 ) + ( 1 / R 2 ) + ( 1 / R
3 )

R = the cell resistance

REVISED SUPPLEMENTARY PROCEDURE

THE 1998 FESTER FORMULA: SUPPLEMENTARY PROCEDURE

BY WIZARD X

Electrocatalytic Hydrogenation of Ephedrine, Pseudoephedrine and Phenylpropanolamine

Materials:

One (1) gram of purified ephedrine, pseudoephedrine or phenylpropanolamine.
One troy ounce ingot of palladium
Glacial acetic acid
Concentrated sulfuric acid
Sodium hydroxide
Anhydrous HCl gas source
pH-indicating paper
Toluene
Kling-Tite Naturalamb brand condoms or cell divider in Figure 2
Lead or graphite electrode 1/2-inch wide by 3-4 inches long
Six one-inch alligator clips
Several feet of 16 to 20 gauge insulated copper wire
Variable DC power supply
Ammeter capable of measuring up to 3 amps, with resoloution to 1/10 of an amp
Voltmeter (optional)
thermometer
Apparatus for Cell C 5 construction.


Procedure:

One gram of ephedrine, pseudoephedrine or PPA hydrochloride is
placed in a large test-tube along with 9 mL of glacial acetic acid. The
test tube is heated in a water bath until all the ephedrine (in this case)
hydrochloride is dissolved. Add 1 ml of concentrated sulfuric acid.
Mix it all together and LOOSELY stopper the end of the test tube to
prevent steam from entering. Heat the water bath to just about boiling , and
use it to heat the test tube and its contents for 2 hours. This forms
the acetic ester of the ephedrine, pseudoephedrine or PPA used in the
reaction. The solution should appear clear and water-like, completely
homogenous. Save 3 drops in a small test tube for ester test.
After heating, the reaction mixture can be kept stoppered as is
for a few days, but it's best to use it immediately after it's cooked.

Next, mix up a solution of 10 mL of concentrated sulfuric acid in
200 mL of water. Take a 250 mL beaker, C 5 cell construction
and place it on a magnetic stirrer. Have the cell C 5 constructed
beaker, and place a piece of lead ( Pb ) 1/4 to 1/2 inch in diameter and a 4 inches long
inside the cell divider. On the other side of the beaker, insert the one-ounce
ingot of palladium cathode. Using alligator clips, to make contact with the ingot ,
via the copper wire and with the piece of lead. They are your two electrodes. Next, pour
the
dilute sulfuric acid solution into the cell divider so 1 / 2 to 2 / 3 full. Next , the
dilute sulfuric
acid solution is poured into the beaker so that the solution level is about 2 cm lower
inside
the beaker than the cell divider. The ingot of palladium should be
completely immersed.
The surface of the palladium ingot should be very lightly sanded with very fine sandpaper
prior
to use and washed with methanol. This increases its surface area a little and exposes
fresh, clean
metal. The piece of lead should be scrubbed free of grease and dirt.
Measure the cell resistance with a multimeter.
A DC current meter (ammeter) should be put in series with the wiring.
A good one can be had at Radio Shack for under $50.00.

The wires are first hooked up so that the palladium ingot is connected to the positive
pole (oxidation)
of the DC power supply, and the piece of lead to the negative (reduction).
Use the polarity tester to get the polarities correct.
The typical one- ounce ingot will have a face with an area of about 6-7 square centimeters
immersed
in the solution. Only count the area on the side facing the lead piece.
The back side doesn't count because significant current doesn't reach it.
With this typical ingot apply about 1.5 - 2 amps for 30 seconds to one minute.
Oxygen will bubble freely from the ingot, and
hydrogen from the piece of lead. Blackening will be noted on the edges of
the ingot, where the current is most intense, and a lighter discoloration
on the flat face of the ingot. This pre-treatment is called anodizing. It
has been found that anodizing increases the ability of the palladium ingot
to adsorb hydrogen when the wiring is turned around, and the ingot is made
the cathode.

Next, redo the wiring so that the palladium ingot is attached to
the negative pole (reduction) of the DC power supply, and the piece of lead to the
positive (oxidation). Use the polarity tester to get the polarities correct.
Add 1 / 3 to 1 / 2 grams of the 30 % Pd on carbon catalyst and start magnetic stirring
immediately.
Apply a gentle vacuum to the outlet tube of the pressure equalization test tube so it
sucks out the
air in the reaction beaker.

Turn the juice back on and run between one and two amps of current for about 20 minutes.
At first, the amount of hydrogen generated at the palladium ingot will appear small.
This is because the Pd adsorbs hydrogen so well. After about five minutes of current
passage,
the whole surface of the ingot will freely bubble off hydrogen and the 30 % Pd on carbon
catalyst
is also adsorbing hydrogen. Stop the vacuum after 2 minutes of suction and disconnect from
the
outlet tube.

After the 20 minute charging with hydrogen, add all of the ester reaction mixture from
the large test tube with a syringe. Use two syringes so one plugs the addition port at all
times ,
so the hydrogen gas doesn't escape. Adjust the current flow from the power supply
so that a current of about 50 milliamps per square centimeter of palladium
surface flows. If one has about six square centimeters of the ingot facing
the piece of lead immersed in the solution, a current of about 300
milliamps is called for. This will result in some gassing off of hydrogen
from the edges of the ingot, but over the rest of its surface the hydrogen
will react before it bubbles off. The lead anode will form a brown layer of
lead oxide, and will not dissolve at all in the sulfuric acid solution.
Some surface particles will be kicked off the lead when it's first
charging, but they don't make it through the cell divider. The lead anode can be
replace with a piece of platinum if desired, but lead is a lot cheaper.
Graphite is another possibilty.

Keep the temperature of the cell electrolyte between 20 - 25 deg C.

Keep an eye on the current meter, as the current flow can change
as the reaction progresses if you do not use the current regulator.
Keep the current flow around 300 mA ( 0.3 amp )
for the size ingot given in this example. A Coulomb is
a unit of charge equalling one amp-second. C = A x s
96,500 C = 1 mole of electrons.

Continue at 300 milliamps until 3000 coulombs have passed through the
solution. Let us use the 300 mA current to show an example of these
calculations: At 300 milliamps, 3000 coulombs pass in 10,000
seconds, or two hours, 45 minutes.

3000 coulombs per gram of feed material has been found to give good
yields of a fine product, but by no means consider this number to be
optimal. It may well be that a greater yield would be obtained by passing
more current. It may also be that pseudoephedrine and PPA differ from
ephedrine in their ease of electrocatalytic hydrogenation.
Apply no more than 3 hours at 300 milliamps of current.

During the course of the reduction, the colour slowly changes from
its initially clear color to slightly tinted with yellow. Now that a hydrogen atmosphere
is present the reaction mixture is not in contact with oxygen in the air.
It's a byproduct of the reaction. In any case, it's a remarkably clean
reaction.

When the desired amount of current has passed, the work-up and
isolation of the product is very simple. Save another 3 drops in a second small test tube.
The cell divider is rinsed off into the beaker and removed from the beaker ,
after pulling out the lead electrode first. The anode can be used over and over again.
The palladium cathode is then washed into the beaker and removed.
It too can be reused an INNUMERABLE number of times.
The process of anodizing the palladium will have to be
repeated prior to each run. Some fresh metal may have to be exposed on
occasion by very light sanding of the metal surface. An ingot of palladium
should last for a lifetime.

The reaction mixture should be filtered into a sep funnel, so to collect the Pd/C catalyst
and rinse
both the catalyst and beaker with water. Add a 20 % NaOH solution should be added with
shaking
until the solution is strongly (13 + pH) alkaline to pH paper.
The catalyts is dried at 100 deg C after being rinsed again with water. Store in
desicator.

Extract with two 50 to 100 mL portions of toluene. This should be
plenty for one-gram of product. The toluene extracts are pooled together and dried with
anhydrous magnesium sulphate. Decant in a clean beaker and rinse with tolulene the
anhydrous magnesium sulphate and decant in the same clean beaker.Then bubble with
dry HCl to get the crystalline hydrochloride product. After rinsing them
off with some fresh toluene or ether , they are spread out to dry.

The most pleasantly surprising finding is that crank produced by
this method doesn't give one the body and soul-wrenching hangovers so
typical of the product made by the iodine-red phosphorous method..
If one should wish to produce more than a gram or so at a time, a
larger palladium cathode should be used. Linking together parallel more ingots of
palladium would get pretty expensive, so a more economical alternative will
be detailed. That alternative is electroplating some copper or brass screen
with a thick coating of palladium.

The simplest way to get this section of screen electroplated with
palladium is to go to the yellow pages, look under electroplaters and find
one who plates palladium. Ask for a plate build-up of several thousandths
of an inch, so that enough Pd is deposited to last a while.

The Pd plated screen would then be used exactly like the ingot.
First it must be anodized, then charged up with hydrogen in exactly the
same way. The sole difference is that the greater surface area of the
screen facing the condom-encased anode requires a correspondingly greater
amount of current to be passed. Then, during the course of the reduction,
again 50 milliamps per square centimeter of surface area facing the anode
is used. The total of 3000 or so coulombs per gram of feed material doesn't
change by increasing the size of the electrode.

An alternative to this is plating the screen yourself, anodically
dissolving a portion of the ingot to form a PdCl2 solution .

The lastest word from Fester is a couple of references from Indian
journals on electroplating graphite electrodes with palladium, essentially
giving a Pd black on C catalyst in the cell!


1) Krishnan, Electrochemica Acta, Vol 21, Pg 449-450 (1976)

On the Electrochemical Reduction of Benzyl Cyanide to Phenethylamine with
a Pd/C Electrode (note: The title may not be exact due to the illegibility
of my chickenscratch transcription of my conversation with UF.)

2) Krishnan, Journal of Applied Chemistry, Vol 5, Pg 125-128 (1975)

The greater activity of Pd on C (over straight Pd) results in a shorter
reaction time.



Wizard X
Member posted 10-29-98 06:50 PM Click Here to See the Profile for Wizard X File
D_1 : I must work on so I can post it on this thread. I have sent this entire procedure
with diagrams to BOZ.

E mail : ***@hotmail.com

Wizard X
Member posted 10-29-98 07:26 PM Click Here to See the Profile for Wizard X File
D_1



Wizard X
Member posted 10-29-98 07:30 PM Click Here to See the Profile for Wizard X Tried
posting File D_1 for the diagrams in the procedure, but failed. Any ideas busy bees.

beagle boy
posted 10-30-98 12:06 PM Click Here to See the Profile for beagle boy I
can't stand the fact that this post has been here for half a day and is slipping down the
list without comment. So let me be the first to thank you Wizard for such a remarkable
post. Regarding the diagram file, maybe it could be hosted on OP's site?

I haven't really digested the post yet, so I can't comment on it myself, but I felt that
this tremendous effort deserved acknowledgment. Thanks Wizard!

KrZ
Member posted 10-30-98 12:34 PM Click Here to See the Profile for KrZ I too
would like to congratulate you on this momentous effort. How is the Royer Palladium
Catalyst used? (As seen on SciAlly)

randolph carter
Member posted 10-30-98 12:57 PM Click Here to See the Profile for randolph carter
excellent post .... reads like an abstract but infinitely more subversive... just a couple
of questions senor'... what exactly is the role of the Pd on C in this reaction ??? is it
purely a catalyst to promote the electrolytic reduction or is it "directly " involved in
some intermediary reduction etc ??? also is this based on empirical research or on theory
??? if there is theoretical (i.e. papers papers papers ...)please enlighten the swarm
...... once again good work Wizard X .....

flaskjockey
Member posted 10-30-98 09:37 PM Click Here to See the Profile for flaskjockey
This definitely requires the diagrams. You need a server to host the pictures, then link
to them from your hive post. You can get a quick freebee website for that from tripod or
geocities.

I've got sortof the same question about the role of Pd/C. Sufficient H is carried off in
the electrolyte to load up the Pd/C? Have you tried to determine in some way that is
definitely occuring?

Wizard X
Member posted 10-31-98 10:17 PM Click Here to See the Profile for Wizard X I
have looked and tried all possible ways at posting the diagram file D_1, with no luck. So
if you want this file then E mail me at : ***@hotmail.com And I will send it too you
using "File Attachment", as time permits.
Firstly, let me say thanks to those who appreciated my effort.
This information is from many journal sites, and NOT just theory. Dreams do come true !
Now, let me give you all some insight at the Pd metal cathode. The Pd ingot cathode is
doing two things (1) producing the hydrogen gas and, (2) the Pd metal is acting as the
catalyst. Now, by constructing cell C1 you trap ( more or less ) all the hydrogen gas
produced at this point, the period where it saids. "20 minutes Hydrogen of the Pd ingot "
in the procedure. With the open cell
( Fester's procedure ) mostly all of the hydrogen gas escapes.
The Pd on carbon added at this period where "20 minutes Hydrogen of the Pd ingot "
increases the hydrogenation conditions, so you adsorb more hydrogen. If you want, you can
use cell C1, a graphite cathode electrode to produce the hydrogen gas and the 30% Pd/C
catalyst. However, lower yields are obtained as the hydrogenation conditions are lowered.
Less active catalyst hydrogen adsorbed ratio to time theory.
And yes, you can do this using a hydrogenation bomb, ( stainless steel cylinders) , but
you need an external hydrogen gas source. The cell produces the hydrogen at the cathode
and the Pd ingot and Pd/C adsorbs the hydrogen gas as well as acting as the catalyst. I
included the ester test so you can determine how well the hydrogenation reaction went.
Less reaction time as you increase the hydrogenation conditions when V = 12 volts & I =
0.3 amps, ( if the Pd ingot has a surface area of 6 cm2 ), however I suggest allowing no
more than 3 hours of current to flow when I = 0.3 amps.

randolph carter
Member posted 11-02-98 08:05 AM Click Here to See the Profile for randolph carter
still got my interest .......now if'n you can get those diagrams up somewhere ....or i
would greatly appreciate them "materializing" in my e-mail ....thanx wiz X....

flaskjockey
Member posted 11-03-98 12:53 AM Click Here to See the Profile for flaskjockey
I've put the diagram for this with text on an html page here

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Jose
2005-04-25 20:49:46 UTC
Many have tried as theoretically the introduction of hydrogen just
seems to "want" to make sense
but electro never has been a successful approach

I know of someone that bought a 50 kg drum of ephedra for 2 bills
way back when...from NJ
extracted it and used it in a stainless "bomb"(literally)
apparatus with palladium type catalyst and shot in hydrogen gas
with is c-clamped ghetto regulator
with a "shaker" orbital mechanism attached to avold the old
kaboom--thanks "kraftsman"

and that shit kicked the snot out of anything you could imagine!

long time ago i some very far away land

try getting a tank of hydrogen now since 9-11 though

Jose
R***@Limestine.com
2005-04-26 02:39:13 UTC
nother hive thread

Author Topic: Electrol Reduction
Sky
Member posted 03-23-99 11:30 PM Click Here to See the Profile for Sky Im reading
out of Steven S. Zumdahl Chemistry in the Electo Plating Chapter that The Reduction occurs
at the Cathode, Oxadation Occurs at the anode this contradicts festers method were the
reduction occurs at the negative pole can anybody elaborate on this?

Optimus Prime
Administrator posted 03-24-99 12:54 AM Click Here to See the Profile for Optimus
Prime In electro chem a neg E of cell doesnt mean that the plating will not work it
is just the amount of juice one has to "apply" to the cell to get the reaction to go...
like a car battery...this cell is spontaneous it generates power in the form of the
electrons given off... a neg Ecell would need voltage applied to say chrome plate your
baby buggy bumpers... so Fester isnt neccessarily wrong it would depend on the wanted
reaction... look up some photochem stuff too if you get the chance... thats amazing
chemistry...

OP

dwarfer
Member posted 03-24-99 10:23 AM Click Here to See the Profile for dwarfer +, - .
Electron flow, cathode, anode:

Different ways to describe the polarities that amazingly is not "in common" across all
disciplines.

Sky
Member posted 03-24-99 09:31 PM Click Here to See the Profile for Sky Fester
said pass 3000 coulombs at 0.3 amps in 2Hr-45Mins. If you increase the amps you increase
the Coulombs per second and decrease run time. I in an experiment hooked up a car battery
of course the wire got hot and the solution bubbled . I did this for about 5min and burned
my fingers put it back on for about another 5Min and extracted and got a 50% yield of
excellant product I Know with a little work a person could put out 100% yields fast.

dwarfer
Member posted 03-24-99 10:13 PM Click Here to See the Profile for dwarfer Don't
forget to read the post's instructions in regard to current per square cm of cathode
surface:

If you were using a 12 volt battery, with the resistance being 3 or 4 ohms, the current
was 4 amps or so: if the wire got hot enough to burn your fingers, then the resistance was
probably less than that, or you were using really small gauge wire.

On the other hand, unless you were using a large cathode, your current was too high.

I am surprised that you got 50% yields, but congratulations.

My best results were to keep the current density at about 1/2 what was specified, and to
run the number of coulombs to about 1.25 to 1.5 the specification.

Although my first experiment worked at 6 volts, with current regulated across a pot, to
have an unpressurized machine work at 12 volts at that current is truly interesting.

What was the size of your cathode??

Was it silver??

If so, AbSoLuTeS experiment is re-verified.

Did you prepare the ester??

Thank you,
dwarfer

Sky
Member posted 03-26-99 01:22 AM Click Here to See the Profile for Sky I hooked
silver dollars up to my booster cables the next go around the current pushed hard and fast
it works put I have better dreams with 3V Longer periods of time Say 12 Hour hooked to
multipal setup ran in series its a lot of extracting but the yield is good>

AbSoLuTe
Member posted 03-26-99 02:19 AM Click Here to See the Profile for AbSoLuTe Neh,
nehrne neh re ne.
Told ya Ag works you Dis-believers.
Slow It down a bit,Sky Fester is correct in the slow method,cranking the coulumbs/amps up
seems to waste product.

dwarfer
Member posted 03-26-99 02:32 AM Click Here to See the Profile for dwarfer I
never doubted you, Abbie!!

Why, I can hardly wait to do it my self!

It brings tears to my eyes to see you happily vindicated!

Sky
Member posted 03-26-99 06:33 PM Click Here to See the Profile for Sky Hey
ABSoLuTe You are my Hero! Silver work Great. My dream last night was wierd done everything
exactly by the book made my ester ran 3V through it all night the next day I extracted
with toulene and bubbled with HCL Gas got a pure white product. It looked like snow tested
it with AL foil everything tested posative for Meth. But when I tried it i didnt feel it
very much like I have in past . What went Wrong?

fj
Member posted 03-26-99 09:14 PM Click Here to See the Profile for fj Since most
of the Bombers are here could I ask something? Making an ester with only glacial acetic
and no H2SO4: Has anyone done this and definitely bioassayed a good product at the end?
thanks

Sky
Member posted 03-26-99 10:39 PM Click Here to See the Profile for Sky I have got
a good product both ways but my falure were probable due to other factures. According to
some of the book I'v been reading the ephadrine side chain is joined at the top or 6 H
atom but meth is the next one down or 1 H atom so I'm not sure I'm forming the right
isomer can anyone elaborate?

MetalKiD
Junior Member posted 04-02-99 05:59 PM Click Here to See the Profile for MetalKiD
Hey dwarfer..

I was wondering about your 6v dream..
6v at what amp?? also did u use 1gram psuedo, like the fester book? and... how long was it
run??

all is hypothetical of coarse..


Later,MetalKiD

Weaselknot
Junior Member posted 04-02-99 06:57 PM Click Here to See the Profile for Weaselknot
password check

Weaselknot
Junior Member posted 04-02-99 07:00 PM Click Here to See the Profile for Weaselknot
Sky, In your 12v dream, was your cathode relatively large? How much feedstock did you use?
I've dreamed of Ag w/o Pd catalyst under pressure but was a nightmare. There's something
about the variables involved in this that i am evidently not seeing. thanks in advance.

Weaselknot
Junior Member posted 04-02-99 07:01 PM Click Here to See the Profile for Weaselknot
Sky, In your 12v dream, was your cathode relatively large? How much feedstock did you use?
I've dreamed of Ag w/o Pd catalyst under pressure but was a nightmare. There's something
about the variables involved in this that i am evidently not seeing. thanks in advance.

Sky
Member posted 04-02-99 07:09 PM Click Here to See the Profile for Sky 12V was to
much power all you need is around 3-6V 300ma I'v never used pressure my electodes were
silver dollars. I'v had varying result 12HR get best results pressure under H+ would be
best!good luck

esop
Member posted 04-02-99 07:59 PM Click Here to See the Profile for esop Dwarfer,
sky and all those who have
a positive outcome in experiments:
funny how giving a voltage without
an amperage makes no sense.
Nor does it make any sense
giving both these parameters above
without specifying the catalyst
you used, or the ester process.
I have to give the award to
Absolute who currently is my reference
for this procedure...
all of the other experiments work
I am sure of it, but being exhaustive
in your report is a demonstration
of courtesy for the person
who reads you and seeks thorough
answers on a problem.
(regardless you might give a shit or not)
Not my case since I've got the
problem down to a cinch...
just a kind reminder from an engineer
of a protocol to convey scientific
information :
never assume all other parameters
are all acknowledged by your readers.

Sorry if I offend anybody, I find it
wasteful to see so much *partial*
information posts...

esop

Sky
Member posted 04-02-99 08:20 PM Click Here to See the Profile for Sky Sorry for
not being more clear But for one thing all I did was experimented with ion bridges not
make any hony the amps were 300MA I tried 3,5,13V all at the same ampage this just proves
that other alternatives to condoms can be used remember this is all hypathetical.

Weaselknot
Junior Member posted 04-02-99 08:40 PM Click Here to See the Profile for Weaselknot
I've dreamt Absolute's dream verbatim. Can't get >10% or so. Esop, what is this little
problem that you have gotten down to a cinch? I've perused all relevant posts and have
actually USED the search engine but can't figure out what I'm missing. What is the #1
factor that would cause my dream to fail? Not counting esterization. Should I use Bozak's
power supply?

Sky
Member posted 04-02-99 10:53 PM Click Here to See the Profile for Sky Your
probably not geting your ph high enough after rx don't filter use a 20% lye solution if
you dont have ph paper smell of your rx when ph is high enuogh it smells fishy then use
table salt keep adding salt util no more salt will desolve add solvant and shake pour
through filter to make seperation pepite out solvent only put aside add more lye solution
to mother liquid the ph will drop after first extraction do this 3 times then bubble with
HCL gas if there is anything there you will get it even if your rx does not work you
should at least get back most of your original product

Weaselknot
Junior Member posted 04-02-99 11:11 PM Click Here to See the Profile for Weaselknot
Sky, did you use a variable resistor to change your voltage or what? Variable resistor in
series and blah blah blah... I'm still not getting the variables involved in this dream

Weaselknot
Junior Member posted 04-02-99 11:13 PM Click Here to See the Profile for Weaselknot
Please ignore that last post...

Weaselknot
Junior Member posted 04-02-99 11:26 PM Click Here to See the Profile for Weaselknot
in my dream I get ~10% honey plus a shitload unreacted psuedo I was estimating. a/b
extraction is not my problem. Thank you much for the answer though. My problem is
understanding the actual mechanisms involved in the reduction. Is it really nothing more
than finding the optimum H production at the cathode? How does this really differ from the
pressure- Pd/c catalyst dreams? IS there an acual difference in the mechanism of
reduction? Are these legitimate questions?

esop
Member posted 04-02-99 11:38 PM Click Here to See the Profile for esop amps
between 1.x and 2.5 are
satisfactory.(with x between 4-9)

A voltage between 3-6 volts is
acceptable, with 3.5 being an
average.

It *must* be DC (direct current).
AC is a sinusoid (sine wave) between
positive and negative voltage...
across a period of say 1 second
AC voltage oscillates from , say ,
0 volt ramps up to 6 volts
ramps down to -6 volts and
ramps up to 0. (in 1 second say to give it
a time period)

two silver (Ag) cathode and anode are
hydrogenating the water + catalyst
solution. this reaction is visible.

calculating the resistance of the
cell (in ohms) in essential to
deduce *amperage* adjustments.
Amperage will drop after passing
in the liquid environment.
compensation (up) of amperage is
necessary.
This is best done by voltage increasement.
within the limit stated.

increasing temp of the cell brings about
the third component of the triad of
parameter.
given a cell resistance, a base amperage
and a liquid temp of the cell
a *ideal* amperage comprimising between
these 3 factors is arrived to.
Which is well stated in silver dream
racing.
in other words you should not dissipate
enormous amounts of voltage through
the resistance of the cell.
and raise the reaction temp more
than a 10 C margin.

other than the cell are the obvious
purity of the Pphed extraction.
see LR extraction. a satisfactory
purity is obtained from the method.
It must be a high level of purity.

second is the also obvious end extraction.
which is the *same* as the initial one
with even greater results.
The final product show greater solubility
in toluene than the precursor's one.
first toluene extraction should be
set aside, they are the greater quality
extracts. lesser ones can be combined
and evaporated separately.

I hope this can help you.
it is factual and spacy but
I won't be posting much on this thread
so here goes.
a critic of the comments is invited
in case of a slip mistake on my
part.

esop

esop
Member posted 04-02-99 11:51 PM Click Here to See the Profile for esop By the
way
the base amps are 1.x to 2.5
at the power supply.
I call them base amps because
they are to be adjusted according
to :
1) cell resistance
2) cell temp
and are not meant as final
amperage of the whole system
but as a starting amperage
to be later modified.
(on which to run evaluation
of your own setup)

esop

esop
Member posted 04-03-99 12:00 AM Click Here to See the Profile for esop Oh and as
Dwarfer pointed out
you must approximate the area of surface
*facing* the opposite electrode.
That is a 2d assesment of your
catalyst (be it Pd or Ag).
which influences further the
amount of ampers running at ideal
flow.
please note that cell resistance increases
during reaction.
(ampers are coulombs/sec)
there are good assesment on this site
of how much how fast this must be.

esop

Weaselknot
Junior Member posted 04-03-99 04:20 AM Click Here to See the Profile for Weaselknot
cannot express thanks...

Weaselknot
Junior Member posted 04-03-99 04:24 AM Click Here to See the Profile for Weaselknot
cannot express thanks...

Weaselknot
Junior Member posted 04-03-99 04:27 AM Click Here to See the Profile for Weaselknot
Ahh shit double post

Sky
Member posted 04-03-99 01:24 PM Click Here to See the Profile for Sky This is
only a theory but if the negative cell is giving up H bubbles if you sealed the cell you
would have your H Atmosphere and with a little heat you could increase the pressure in the
cell. then you would not need a H generator or pressurizing device! this is just a
theroy!!!!!!!!

Sky
Member posted 04-03-99 07:20 PM Click Here to See the Profile for Sky I'v got
great results using 12V 300MA pullin through multipupose power suply bought at wal-world
that could be set at 1.5V 3V 6v 9V 12V all at 300MA. I had to set it at 12V to pull 3ohns
using #16 wire with silver dollars as electrodes and a condom for a cell divider it seems
that the voltage gives it a little more push but the amps is what generates the heat that
burns the product so you can use higher voltage as long as the ampage is low. this might
help:+(

dwarfer
Member posted 04-05-99 05:14 PM Click Here to See the Profile for dwarfer On the
first experiments I did that worked, at 6 volts, I was trimming the current with a 50 ohm
variable resistor, and cutting the current down to about 1/4 amp if I recall. (This is
from memory: I know that the current DENSITY on the silver cathode was only 1/2 of what
was specified as the maximum. )

Since I was EDUCATED about excess voltage and got a power supply, I have done a couple of
"interesting" euphoria runz and have noted that 500 MA takes about 2 volts to start with
through a D-III, rising to about 3.5 V later in the reaction.

ESOP, why does the resistance increase: I have wondered if this is not an "indicator" of a
change in the cell chemistry: I thought maybe it happened when the electrolytes were fully
saturated or something, but that ain't it.

I have intuited that you think I'm trying to hold something back; which is not true. (If
my guess is accurate.)

I'll try to get the pics this week.

I'm coy about what I do and how I fix and what I run and other dreams: I will "speak"
readily about the machine, and operating parameters.

Sky, I'm amazed at your results at 12 volts!! Super easy and fast.

I think that a concern with excess voltage is that it may give rise to other modifications
to the molecule other than the desired one.

I wouldn't want to suggest a change if your results are optimal, but you may try and see
if you get even better results from your 300 MA power supply at 1.5 or the next lowest
voltage setting. (Sorry: I just reread a "higher up" post and you already agreed that the
3 V was a bit more efficient.)

You had to set it a 12V to pull 3 ohms?????

dwarfer

esop
Member posted 04-06-99 12:07 AM Click Here to See the Profile for esop Dwarfer :

You're back!
That's exactly what you had to say
to get ya back in my agenda's
"to do" list, dudy!

Oh the resistance increase because
the damn thing loses conductivity
over time. (free base is not a salt)
but nothing major probably the least
of my problems...

esop

dwarfer
Member posted 04-06-99 03:58 PM Click Here to See the Profile for dwarfer Well,
glad to be on the same wavelenght, esop!

My observation of the conductivity/resistance/voltage changes that occur while running is
that they are not linear: like it runs at 500MA for a long while at 2 volts: then 15
minutes later suddenly it takes 3 volts.

This could be lack of careful observation, but i think I'm right.

dwarfer

corrodium
Member posted 04-06-99 09:20 PM Click Here to See the Profile for corrodium A
cell containing H20 only and no sulfuric fails to register current flow. Add sulphuric and
up go the needles! Could this current drop signal a decomposition or neutralization of the
above added component and could more be added to compensate and raise the current flow to
precalculated levels? Higher amps seem to shorten the time it takes for the current drop
to occur. 4v,2amps,2hrs,12v would not correct current drop...spicemines

corrodium
Member posted 04-06-99 09:21 PM Click Here to See the Profile for corrodium A
cell containing H20 only and no sulfuric fails to register current flow. Add sulphuric and
up go the needles! Could this current drop signal a decomposition or neutralization of the
above added component and could more be added to compensate and raise the current flow to
precalculated levels? Higher amps seem to shorten the time it takes for the current drop
to occur. 4v,2amps,2hrs,12v would not correct current drop...spicemines

corrodium
Member posted 04-06-99 09:21 PM Click Here to See the Profile for corrodium A
cell containing H20 only and no sulfuric fails to register current flow. Add sulphuric and
up go the needles! Could this current drop signal a decomposition or neutralization of the
above added component and could more be added to compensate and raise the current flow to
precalculated levels? Higher amps seem to shorten the time it takes for the current drop
to occur. 4v,2amps,2hrs,12v would not correct current drop...spicemines

MetalKiD
Junior Member posted 04-07-99 04:43 AM Click Here to See the Profile for MetalKiD
hmm.. do you HAVE to esterize the ephed or can you get by with pure ephed..yields would
suffer i bet.. any thoughts???
Any idea's on a 'salt bridge'??? I saw that in a chem book. It says its a paper soaked in
KN03(saltpeter,potassium nitrate) and that it distrubtes current to both cells.. wouldn't
the kn03 interfere with the reaction? thats what i though.. and.. how does one link up the
cells?


questions.questions.questions..=answers

Cheapskate
Member posted 04-08-99 03:03 PM Click Here to See the Profile for Cheapskate
Help!! One of these procedures has been tried by a monkey down the street and he had
rather good results, but.... He can't tell the leftover Pfed from the desired product and
both apparently separated out. Else he got like a 90% yield. How should this monkey
separate the precursor from the product??

fj
Member posted 04-08-99 04:17 PM Click Here to See the Profile for fj First,
which procedure did the monkey try? Dumping in the pfed without esterfication?

Cheapskate
Member posted 04-09-99 02:27 PM Click Here to See the Profile for Cheapskate
Yes, there was no esterfication. The idea was to try the simplest procedure possible. So
the silver dollars (actually it was silver bracelets) were hooked to a highpowered battery
charger with a huge capacitor to level the voltage and keep voltage spikes out. This is
similar to the battery setup that Sky used. Ran this at a reasonable bubble rate while
paying attention and not allowing it to get too hot. Couldn't tell the current because the
meter didn't go down that low.

Did the usual basify and extract and evaporate...wait, meth freebase is an oil!!! The
monkey got crystals!! Shit it didn't work.

jimwig
Member posted 04-09-99 03:35 PM Click Here to See the Profile for jimwig To vary
voltage the traditional way one uses a device that does not distort the sine wave. Meaning
phase control (wall dimmer Fred) which does not vary voltage. Just an rms fascimile. Chop
it up and the load says "yeah we going real slow now". Dumb load.

These a variable transformers or autotransformers.

AKA a variac or powerstat.

I have several of these used in a variety of wattages. (Watts=Voltage x Current {DC})
but for our poiposes {AC} good enough formula.

I am sellling these wonderful devices for about $35 and up. Depends on the unit. Plus
shipping. I have about six of them. Most are the standard chem lab type (around 7 - 8
amps) with cord, fuse, knob for varying, case and a handy dandy receptacle. And of course
they are in lab blue. Some of you might recognize the m.o.

Although used they look (and perform) well.

Also several industrial strenght units that go 20 amps but less ergonomic. 120vac

And some baby types (some new in box) good for about 180 watts without case, cord and
plug. For the do it yourself types.

***@hotmail.com

Sky
Member posted 04-09-99 07:29 PM Click Here to See the Profile for Sky No
Esterfication No RX. I'VE tried every way to get around the esterfication and can't! It
take about as long to form the ester as it does to do the whole RX but it is very
important for a successful reduction!

esop
Member posted 04-10-99 05:33 AM Click Here to See the Profile for esop That's
right Sky...
Tell'em (teehee)

I don't even know how this
came to existence...
but you do have to follow
the holy "damned" ester thingy...

esop

spiderwire
Member posted 04-10-99 06:24 AM Click Here to See the Profile for spiderwire
jimwig, you're the man.
You're always like, 'hey, I know how that tool works.' And its explained and thats it.
Then you're like, 'and by the way I have some cool used ones for hella cheap.'

So cool

Sky - Zumdahl can be very explanatory if you have the time to read thoroghly. Very useful
equations too

fj
Member posted 04-10-99 05:11 PM Click Here to See the Profile for fj Are you
doing the Holy Esterfication for a Catechism in unpressured battery acid?

With reference to the new meth page that Rhodium just put up on his page, I'd like to know
the contents of that narc dood's "personal communication" (ref 1) which pertains to a
direct reduction of the benzyl alco with Pd/C. I guess that's why it was restricted
circulation.

Sky
Member posted 04-10-99 06:41 PM Click Here to See the Profile for Sky MY last
experiment went 100% I didnt weigh it but visually it looked like 100% It went like the
usual festerfication doing the ester thang for 3HRs using the same silver dollars I've
used 15 times now they look a little hairy but it seems like there working better with
age. I dont think that silver will last an infanitly but if they last for 20 RX you get
your monies worth. anyway the product has a slight yellow tint tast like shit and make
your skin crawl the last kept me up for three days. it great if you like to loose sleep
after the first night I've had enough you can have that shit I like my sleep to much I
think I'll start working on that lude resipe on roads page or something well here I am
rambling again sweet dreams

corrodium
Member posted 04-10-99 09:03 PM Click Here to See the Profile for corrodium What
I think is somebody did not get shit and they are only here to fuck people up the way
antisocial did. Otherwise they would say how so it could be verified.

Sky
Member posted 04-10-99 09:27 PM Click Here to See the Profile for Sky Do the RX
and verify it your self!


Optimus Prime
Administrator posted 04-10-99 09:52 PM Click Here to See the Profile for Optimus
Prime Sky: Please e-mail...

***@hotmail.com

OP

corrodium
Member posted 04-10-99 11:14 PM Click Here to See the Profile for corrodium
Thang-thing,monies-money's,tast-taste,it-it's,to-too,lude-quaalude,resipe-recipe,Roads-Rhodium's,infanitly-infinitely,your
self-yourself...Liquid Fire won't go clear?

Backdoor469
Member posted 04-11-99 01:15 AM Click Here to See the Profile for Backdoor469
Sky:

Just curious as to which power supply you obtained at wally-world. Is it the "wall unit"
with the 4 different attachments?

Worlock
Member posted 04-19-99 08:10 PM Click Here to See the Profile for Worlock
Suppose
acetic acid + ephed + eth-OH<>ester + H20
To drive reaction to right remove water.


If refluxed in presence of toluene & H2SO4.
The lowest boiling component would be an azeotrope of water, ethanol, and toluene (b.p. 75
degrees)
ethanol (b.p.78.3 degrees)
as fast as water is made it is removed by distillation.

The ephed is slow to form ester.
but could result in high yield of eph-ester

Worlock
Member posted 04-25-99 11:38 AM Click Here to See the Profile for Worlock Gas
Electrodes

The at the cathodeof ephedrine is reduced(gain of electrons).

With a platinum or Standard hydrogen electrode, hydrogen gas is bubbled across the surface
of the platinum in a continuous sream, so the solution and gas are always contact the
electrode.

The primary electron transfer to ephedrine then, involves the hydrogen gas, by a two step
process.
H2(gas) < > H2 (sat'd soln)

H2(sat'd soln) < > 2H + 2e

This is in contrast to electroplating or producing a solid for gravitonmetric evaluation.
In Electroplating the production of H2 gas is avoided, because you wish the electron
transfer to take place at the surface of the electrode and not at the surface of the gas.

In this dream we want the H2 gas production.
H2 gas is produced by higher Voltages, and by an increase in Hydrogen ion concentration.

The reaction between Ephedrine and H2 is then the transfer of electrons from H2 to
Ephedrine, and ephedrine releases the ester side chain with the oxygen.

One side reaction occurring is Cl- ion
Cl2 < > 2Cl- + 2e
Note the smell of Chlorine at the end of the process.

Some of the ephedrine HCl must be replaced by HSO4- ion or SO4--(ionic with 2 ephedrines),
or ethamphetamine.

The only other dominant negative ion is the Acetate ion
ACet-

So I would like to apologise to Dwarfer for assuminbg his use of high voltages was
incorrect. You should have a voltage strong enough to produce a stream of H2 gas under
pressure. I was wrongly under the impression that this was similar to electroplating.

Worlock
Member posted 04-25-99 11:57 AM Click Here to See the Profile for Worlock
Pre-conditioning of your salt bridge, condom, electrodes, or clay pot, reaction chamber.

As you might imagine, these items will become dry if not immersed in solution.
Depending on the porosity and ability to absorb atmospheric water, this can be a
detriment.

Glass electrodes require many hours to re-hydrate if they dry out. Stainless steal
electrodes also absorb some of the solution if left to dry.

The most serious would be the clay pot, due to its porosity it can absorb lots of solution
and therefore ephedrine.

Doing a run with a small sample may result in zero return, as up a gram or more of
ephedrine may be absorbed into any of the surfaces.

It seems a good plan to either store your equipment in solution, or to pre-condition
everything before inserting pre-honey.

A clay pot left out will absorb lots of water, and may need to be baked until dry then pre
conditioned with the solution.

Pre conditioning under pressure, and under H2 load would be a logical progression in
thought.

During the ephedrine preparation, load the elecrolytic cell with everything except
pre-honey and crank up the pressure, turn on the juice for several hours, this will force
solution and H2 into the equipment.

All will then be well solvated and hydrogenated prior to adding the goodies,
aiding the reaction and preventing major loss of precursers.


quick1
Member posted 04-26-99 01:02 AM Click Here to See the Profile for quick1 sky,
what is the power supply that got at wally world? you said that it could bee set for 3v at
300MA. i did not see what you were talking about but i found a charger rated 6V at 1A.

dwarfer
Member posted 04-26-99 07:47 PM Click Here to See the Profile for dwarfer
Warlock, I don't even remember the criticsm: the highest V I've used is 6, which worked:
others have used 12 and have reported super results and hot wires.

The V should be the minimum to attain the current you want, although it works as mentioned
at 6 V, (direct experience); and 12V (testimony of others.)

In another thread you referenced a reversible reaction to the ester in aqueous solution
and planned to run in GAA as the electolyte. ( I think it was you but if not, whomever.)

In my opinion, and this is from a dynamics perspective rather than chemical, I do not
believe that the ester, once formed through the somewhat rigorous process excluding water,
including H2SO4 as an accellerant or catalyst, and pure GAA, is going to reverse in water.
The energy available to transmogrify the ester to a more palatable form will be found only
at the electrical interface which you so aptly described above.

If I'm correct, don't waste your GAA.

If I'm wrong, then it is quite curious how the process has worked so well for some.

The clay is held together by strong ionic bonds before firing: I think some of the silica
fuses, but I am not sure.

The pore size in the fired red pottery is suspect: that's why using it as a "back up" for
the 'skin is appealing.

As someone posted before, unglazed fine white china would be preferable, as it is more
consistent and with a finer pore size.


as regards pre treatment, you may wanna soak the clay pot in water first: but under any
circumstance the absorption will be a small noise factor (in re production efficencys)
compared to the much larger concerns of extraction and other processing inaccuracies.

Quick one, your 6 volt will work but you need a 50 OHM variable resistor and a cheap
multimeter.

regards,
dwarfer

quick1
Member posted 04-27-99 12:30 AM Click Here to See the Profile for quick1 ok
dwarfer, i found a telephone power supply.
output: DC 12V 250mA
is this close enough? what would the rxn time bee with 12V?

Worlock
Member posted 04-27-99 03:20 AM Click Here to See the Profile for Worlock
The reversablity of the reaction involving the esters is from,
Organic Chemistry, Morrison and Boyd 3rd edition; pg 658-665.

They compare rates of esterfication in acid and alkaline solution, involving primary,
secondary, and tertiary amines. The tertiary being the more difficult to react.

They say it is a one step reversable reaction, "when heated".

The increased pressure perhaps is similar to heating?

The adding of a water molecule separating the ester is more common in acidic and alkaline
than in neutral solutions.

quote: alkaline solutions provide hydroxide ion, which acts as a strongly nucleophilic
reagent; acid provides the hydrogen ion, which attaches itself to carbonyl oxygen and thus
renders the molecule vulnerable to attack by the weakly nucleophilic, water.

My last run with the glacial was actually quite shitty, The esterfied solution was added
to the bomb, while still hot.

An un-noticed wax showed up
after the esterfication process. The clay pots have the disadvantage of "possibly"
becoming plugged after multiple uses.
and of carrying contaminents to the next batch.

I'm preparing the open beaker test.

After a prior run the pot was allowed to air dry slowly, as it dried it became coated with
a large amount of white powder.
a mix of primarily Sodium acetate, various salts, meth, ephedrine.

So the clay is quite permiable to organic salts of low molecular weight.
I wonder about the different types of clays and possible interference by unknown
substances.

I have never had a great result, 50%-60% chicken feed to honey is about tops.
The honey is awesome but the chicken scat ain't too sweet.

I had hoped to be in the 80%-90% by now.

dwarfer
Member posted 04-27-99 03:23 PM Click Here to See the Profile for dwarfer My
experience is that the water addition after esterification is not damaging to the further
processing, and does not cause change to the ester.

My opinion on this besides experience, was originally derived from the dude from whom I
got some technical info in re safety and other concerns, who is a Dr. in chem: and I had
had a dialogue wiht him also in re esterification, water's effect in the formation of
such, and specifically asked him why water was not a problem after the ester was formed
and he was the one who told me there was not a problem after the ester was formed because
it was then stable.

As usual, my knowledge is derivitory of others input: I certainly do not claim to qualify
your extracts from the chemistry text which you quote, which seem applicable on their
face; but can specifically experientially stipulate that my experience does not, in the
experiments I have done, indicated that the ester we are discussing reverses in moderately
acidic aqueous solution.

Having said this, which I believe in fact, I must state that my lack of accurate scale
precludes proving it. However, in estimates of my best run, if I did not get 80% yield,
[+] , I'll eat the porcelain Buchner funnel in which the precipitate was collected.

My next time I'll use the precise measurements on the ester formation which seem to be the
bugaboo of most of us, as described by Wizard: 7 (or was it 9?) ML GAA, and 1 ML conc
H2SO4, per gram; 60 degrees C for the first hour and watch the second hour and remove when
brown begins.

I'm irritated that a 6 gram run should take 42 ML GAA. That seems excessive to me, but
I'll follow instructions first and whine later if'n it don't work.

That's my story and I'm stickin' to it: unless I change my mind.


dwarfer

fj
Member posted 04-27-99 07:14 PM Click Here to See the Profile for fj An
improvement to ester yields may be in adding a silica dehydrant to the brew, to lock up
h2o as it's formed. That's something students do sometimes, given that extra H2SO4 can't
be used for that here. It's just something I remember reading, I don't have exper or
specifics. I assume it's the stuff put in paper packets to keep products dry.

fj
Member posted 04-27-99 07:15 PM Click Here to See the Profile for fj An
improvement to ester yields may be in adding a silica dehydrant to the brew, to lock up
h2o as it's formed. That's something students do sometimes, given that extra H2SO4 can't
be used for that here. It's just something I remember reading, I don't have exper or
specifics. I assume it's the stuff put in paper packets to keep products dry.

Wizard X
Member posted 04-27-99 11:50 PM Click Here to See the Profile for Wizard X GAA
by itself is a poor electrolyte. Even a dilute solution of GAA will not allow the
magnitude flow of current as a H2SO4 solution. This is due to ionization constants.

Because the hydroxy is a secondary alcohol, greater reaction conditions are required to
force the reaction to the right.
Acetic anhydride and acetyl chloride reacts with Eph, 100%, but also on the acidic
hydrogen on the nitrogen.

C6H5-CH(OAc)-CH(NAcCH3)-CH3

Esters are hydrolyzed back to there initial components, but not spontaneously.

Dilute acidic or alkaline solutions are required and heat.

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Crystal Meth
Electrolytic reduction

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Author Topic: Electrolytic reduction
Blackbird
posted 07-21-98 10:40 PM Click Here to See the Profile for Blackbird Can
anyone share in the hypothetical, any info on if and how ER (pfed & mercury?) works in the
production of meth. Is this the meth-od that I recently heard about on the news which only
takes 45 minutes, or does such an efficient method even exist?

BB

KrZ
Member posted 07-21-98 11:55 PM Click Here to See the Profile for KrZ Nobody's
going to answer your ? because no one knows. Until UF's advanced tech. comes out.

I was at the library looking over principles of electrolytic reduction today, the fire
alarm sounded before I could lookup journal ref's specific to ephedrine. I was thinking
something with a voltmeter, and a model train DC transformer wire the transformer up to
the Carbon rod, and the paladium (Perhaps in the form of that highly reusable mesh that
SciAli sells?) coin. Then I could get one of those glass ion bridge tubes with the
membranes in them, link the two beakers and run it at whatever the reduction potential of
ephedrine is for 12 hours or so... should yield pretty well I suppose.... Extract and
recrystalize..

Blackbird
posted 07-22-98 12:00 AM Click Here to See the Profile for Blackbird Have
you heard of this "45 minute" miracle process then?

BB

KrZ
Member posted 07-23-98 07:08 PM Click Here to See the Profile for KrZ Try and
start an intelligent conversation and this is what you get.... Electrolytic reduction can
be done for 45 minutes but if you just leave it on for 12 hours you'll get 97-99%
yields... Anybody got any ref.s at all? This is what the nazis did until the russians cut
off their palladium supply...

Blackbird
posted 07-23-98 07:49 PM Click Here to See the Profile for Blackbird So
this is the infamous "Nazi Method"?!? Hey, I think I could handle hanging around for the
extra few hours it takes to get those kinds of yields. More info greatly appreciated if
anyone can satisfy my thirst for knowledge about this meth-od (shit, I'll even kiss your
preverbial ass if need be).

Thx,
BB

Draeno
posted 07-23-98 08:01 PM Click Here to See the Profile for Draeno Any
ref's on this method?

Optimus Prime
Moderator posted 07-23-98 09:17 PM Click Here to See the Profile for Optimus
Prime KrZ: I dont suppose the type of salt bridge used would matter would it as long
as the e flow was continuous... is this correct or is the membrane needed...

OP

BookwormII
posted 07-24-98 02:48 PM Click Here to See the Profile for BookwormII
Gads; run though dejanews on Elc. of ephedrine. Yes It works well on the ester of
ephedrine (pusedo too). a dived cell is best for yeilds, take a cermic class to make you
own lab ware, just dont glaze the seporater. PB (lead) anodes, and cathodes work just
fine, lead wire pounded flat is best. the trick is to have enough amps per sq. cm one the
anode best is over kill, IE 20 amps on a 5 cm anode. Last stiring helps as keeping temp
down, yeilds are about 45 to 75.
now was'nt that hard?

KrZ
Member posted 07-27-98 07:00 PM Click Here to See the Profile for KrZ Wasn't
that hard?
Don't be so snide you have given us NOTHING

Draeno
posted 07-27-98 11:07 PM Click Here to See the Profile for Draeno Gads; I
still am visualising all this crap- vessels and anodes and paladium and flattened lead
wire and carbon rods- floating in space. I mean, hey, I am a freaking e.e./c.s. weenie for
Bob's sake! If I thought deja news was a reasonable resource I woulda checked, BWll.

If I wanted the crass response my posting would have looked like this:
Hi. Could you please belittle me because I haven't read enough info on this subject to
visualise the equipment configuration? Thank you in advance for your punishment.

anyhow... thanx
cheers, D.

Lone Ranger
posted 07-28-98 12:58 AM Click Here to See the Profile for Lone Ranger
One piece of informtion lacking in all the electrolytic wrte ups are details on the
current or voltage required. Some say you must use a battery. That provides constant
voltage, the current changes as a function of the effective resistance. The same text
might say that a constant current of 9 amps is neeed. To do that the voltage must change,
and so a battery cannot be used!!

Which is it? Constant current, or constant voltage?

flamethrower
posted 07-28-98 01:03 AM Click Here to See the Profile for flamethrower I
DREAMT OF A MOD OF RATIO OF RED P AND I THAT PRODUCES IN ONE HOUR. IN THIS DREAM HUMAN
TESTING FOUND THE PRODUCT WAS QUITE EXCEPTABLE AS FAR AS QUALITY AND CONVERSION RATE. IF
THE WET DREAM IS RECALLED CORRECTLY I BELIEVE IT WAS 2X I
1/3 P 1E . THE MAIN CHARACTER OF THIS DREAM CURRENTLY RESIDES IN FED WORLD, BE CAREFUL.

Piglet
Member posted 07-28-98 04:57 AM Click Here to See the Profile for Piglet The
overview of Fester's electrolytic reduction that I read was indeed using the acetyl ester.
This makes sense to me since ALL the other reductions use some sort intermediate, almost
always an ester. Fester suggests H2SO4 and glacial acetic acid in a single cell with
platinum electrodes. One thought I had was that many labware companies sell palladium
labware such as crucibles. The lid of one of these might well make a nice electrode...
I suggest that other esters may well work for this process.
The overview suggests that the H2SO4 is needed to make the acetic acid acidic enough to
form an acetic ester. H2SO4 alone should form an ester anyway...

Also, anyone thought of adding I2 to ephedrine to form the iodo intermediate and then
using palladium+hydrogen to reduce it? Just an analogue of Festers chloro intermediate,
but easier to do...

flaskjockey
Member posted 07-28-98 08:07 PM Click Here to See the Profile for flaskjockey
Damn, ephed->iodo->Pd\H does look very interesting, hypotheticaly speaking. rdx of that
intermediate works in pots of HI all the time. Is there a some advantage over UF's acetyl
ester, I don't know. Both easy to acquire and easy to do. Maybe I2 coming back into the
solution on rdx would make a handy color indicator - When it stops getting redder, shut
her down.

KrZ
Member posted 07-28-98 10:30 PM Click Here to See the Profile for KrZ What about
the amp for an electrophoresis kit?

A couple of weeks ago, while shopping for a computer so that I could be
kind of a regular visitor to this newsgroup, I came across an article
titled Electrolytic Meth. This is my commentary. There are several
electrolytic methods for reducing ephedrine, pseudo- ephedrine and PPA to
meth or amphetamine, but I doubt that this one will work. The proof of
course is in the trying, so perhaps it does. More weird things have
worked in the past. I'll start with a critique of the construction of
the cell. The sub- mitter uses a clay pot to separate the anolyte from
the catholyte. This produces a huge amount of resistance which generates
a lot of heat. I see no mention of cooling in the recipe. It would be a
lot simpler if a Trojan Extra Sensitive condom was used as a diaphragm
for the anolyte. It only takes about 6 volts to break the insulation on
these condoms, allowing the use of a toy train DC transformer or battery
charger as power source. Meth in dilute solution as the salt doesn't have
the rubber dissolving power of the free base, so the condom should hold
up. If not, try one of those new polyurethane rubbers. The submitter
specifies the use of dilute sulfuric or hydrochloric acid as anolyte.
Hydrochloric acid in the anolyte would lead to quick dis- solution of the
lead anode, forming PbCl2. Only dilute sulfuric acid would be acceptable
for use with lead. The submitter makes no mention of effective stirring
of the catholyte. This is a huge ommission. Very effective agitation must
be present to bring fresh substrate to the surface of the mercury for
reduction. The submitter specifies 4 amp current without quantifiying the
mercury surface area. There are two choices of control of an electric
reduction, voltage or current density. Neither are specified. Now to a
critique of the chemistry. My search of the lit shows that benzyl
alcohols aren't reducable by this method. See Org. Syn. Collective Vol 3
page 60 titled aminobenzyl alcohol. In a nearly identicle setup, the
benzyl alcohols formed wasn't further reducable. The article states that
the method is general, so no benzyl alcohols should reduce under these
conditions. For methods that do work, see Tet letters p2157-60(1979) and
J Org Chem p. 1604-6(1970) and J Electrochem Soc.(1959)No 4 p 325-7. The
Tet Letters procedure could be improved by using a palladium cathode
charged up with hydrogen in a manner similar to the hydrogen charging of
the Raney nickel cathode used in Tet Letters Vol 25 p. 5347-50(1984), and
also by using the sulfuric acid ester rather than the more exotic meth-
anesulfonate. The quaternary ammonium used in the articles might be
replaced with the quaternary salt found in waterbed conditioner. Maybe
even sulfuric acid with the Pd cathode reducing the sulfate ester. Think
hydrogenation. As another electrolytic route to amphetamines, the
lithium metal found in lithium batteries can be continuously cycled back
in liquid ammonia using Pt anode and cathode in an undivided cell. See
Topics in Current Chemistry p. 149-219(1987) All this and much more is
going to be covered in my upcoming book, "Advanced techniques..."

KrZ
Member posted 07-28-98 11:14 PM Click Here to See the Profile for KrZ Thats
festers post btw.

Can't wait to get those ref.'s

KrZ
Member posted 07-31-98 12:02 AM Click Here to See the Profile for KrZ God damn,
UF is a cunt.
All those ref.'s were absolute *crap*
Jackass....

Lone Ranger
posted 07-31-98 12:39 AM Click Here to See the Profile for Lone Ranger
There are many references that detail working catalytic reductions of benzyl compounds. To
reduce an alcohol in such a fashion might work well with a few CCs of H2SO4 added per gram
of alcohol. The ester can now be reduced catalyticaly (for sure) or electrolyticly (I'd
have to read more, but likely). The new book Strike mention's in the general discusion
(see Mmonster Book on Ampetamines" thread) is a must for anyone toying with these methods.

Now, is it constant voltage or constant currenr for best results?? Or (horrors!) even
constant power accros the cell?? There are ways of suppling the proper
current/voltage/power that is required, but this is a detail that no one seems to know.

BookwormII
posted 08-01-98 02:30 PM Click Here to See the Profile for BookwormII
current is what dose the the trick, you must have at least 2amps per sq cm of eltrode.
voltage just seems to heat the batch up. I found a lovely supply at a elctronic salvage
shop 5volts at 50amps for 10 bucks.

Lone Ranger
posted 08-02-98 12:22 PM Click Here to See the Profile for Lone Ranger
Bookworm II feels that:

"current is what dose the the trick, you must have at least 2amps per sq cm of eltrode. Voltage just seems to heat the batch up. I found a lovely supply at a elctronic salvage shop 5volts at 50amps for 10 bucks."

This power supply will be useless. If the resistance starts at only .5 ohm, your 5 volt PS
will deliver only 10 amps. If the resistance is 5 ohms, only 1 amp will flow. This power
supply (5V, 50A)is a constant voltage power supply, probably appropriate, but the output
voltage must be adjustable (in the 10-20 volt area)so that the current can be set to the
desired density. The current will then change as the reaction proceeds (and the resistance
changes). Current = voltage/resistance.

Articles I have just looked at say to set the voltage so that the desired current density
is achived. Then the voltage is left at that point, even though the current will change
with time. So the answer to my question is that a constant voltage power supply is called
for, one whose output is adjustable.

The good news is that a battery is just such a device. Series up motorcycle batteries
until the current flow is correct. Use a 30A fuse to protect your ass if resistance goes
low (membrane rupture, conductive bridging of electrodes, ect). Up to 3 batteris will be
needed (18 volts)

rubberneck
posted 08-03-98 05:00 AM Click Here to See the Profile for rubberneck
Remembering way back, I learned somethings on reduction potentials. Metals could be
selectively reduced from complex solutions depending exclusively on potential. Potential
is the important thing here (volts) as this is what causes the reaction to happen, this is
the driving force, the energy chasm which the reaction gets pushed over. Amperage would
only control the rate as this is how many electrons go into the system. The important
information is what potential to drive the reaction at rather than amperage (that factor
could be made up with time duration). ie you could put 100A through an acidic water
solution but it wont electrolyse (just get hot) if the voltage is not high enough.
Reduction potentials are what drive any reduction so this is the important thing. (sorry
about trying to drill this point in but I reakon that its a basic concept thats being
ignored here)

Best of luck to whoever gets this bitch to work!

rubberneck

monkey
posted 08-04-98 06:23 AM Click Here to See the Profile for monkey Well,
I'll tell ya... there's probably some genius out there doing it right now... but monkey
will believe "battery and flowerpot" fairytales when he sees it; three decades ago he
wasted many monkey-months and a lot of raw materials trying, and would love to know of a
resounding success. Who knows, maybe with exactly the right solvent and exactly the right
voltage, the whispered-about kitchen magic does work.

Once upon a time, in a galaxy long ago and far away, some limited success was attained,
lore has it, using a reactor resembling K-O 3rd Vol. 8 p.700 Fig. 1(b).

The power supply, say the Druids, was a constant-voltage type, 5-30VDC and 30 amps max
output capacity, taken from a projects reference, name forgotten. If monkeymemory serves
it was by the editors of "73" magazine. Heavy duty heat sinks cooled with either
high-velocity air or cold tapwater were needed on all transistors, FWBR's, and especially
the drawdown resistors. Voltages employed were low, comparable to those typically used
with mercury cathodes. Voltages lower than 5VDC were obtained with use of a 200-watt
0-4-ohm variable resistor (a _big_ sucker) in series with the electrovessel. BookwormII's
5VDC 50 amp power supply just might work, with such a resistor.

Amperage per sq. cm. was not a crucial factor, in fact amperage throughput at any moment
was never more than 20, but contact time (needed: not too short, not too long) and
temperature (needed: not too low, not too high) were. Electrolytes which worked were
dilute, slightly acid aqueous solutions of metal salts with what were then thought of as
"plating buffer compounds", but today's electroplating (and perhaps other) PTC's would
probably work as well or better.

The PS was easily built from a cannibalized and rearranged guitar amp, but design of the
reaction vessel required integral calculus involving flow rates and thermal transfer. It
took several hours of 1970's mainframe computer time and a _lot_ of FORTRAN cardpunching.
Its construction required about ten dozen tries and professional machine shop services to
get right.

The Goldilocks electrode material was a trial-and-error-found,
repetitiously-plated-then-sintered surface of Pd-plus-Pt-on-80/15 nichrome with rare earth
(monkeymemory is dim, he suspects cerium) oxidation-protective component the rest, not
simple auto-battery Pb (Cheeeez-us Priced Almighty...). This surface was an outright
woolly bitch to make --it took several weeks with round-the-clock monitoring by four
trained personnel, using professional Detroit plating equipment, but only (alas)
garage-built vacuum laser sintering equipment, to deposit it cleanly enough to work.

The results were interesting in that both reductive aminations and olefin oxidations could
be made to happen, by wiring active surface as cathode or anode, but the only interesting
thing was that it worked at all; yields were disappointing. But perhaps if the
investigators hadn't run out of time, might've improved. Modern metal finishing technology
is light-years ahead of what existed then, so today its manufacture might for all monkey
knows take only a few hours of simple sputtering.

But monkey would suggest bees only pursue organic electrochemistry if bees have a lot of
time and money and plenty of raw materials to spare, plus a good machine shop, and have
intimate knowledge of such a computer package as Mathematica. Still, Strike's small army
of full-time x consultants may want to look into it, because if an economical route to x
is ever found from eugenol, it will most likely involve electrochemistry. Monkey has seen
it done, albeit in very low yield.

rgds,
monkey

BookwormII
posted 08-04-98 03:55 PM Click Here to See the Profile for BookwormII OK,
cutting the spam,
Current density, is what turns the trck from what I read. Regaurdless the point in getting
the amp needed is based on the load resistance of the cell a power supply can pump out a
shit load of power (voltage and amps) and not do the trick. Ohms's law states that amps
(current)=voltage/resistances,so in creating the right current densisty (.02-.05per cm2,
minum need for reduction) you have two chocices ethier change the volatage as labrat has
stated or change the resistances of the cell. with a fixed voltage supply the only choice
is to change the resitance of the cell, this is done by either the increase the condutivy
by adding more acid to the electrolytes or by changing the thickness of the seperateor (in
the case of clay seperateor sanding works well), to increas the resistance of the is to
use a reostat in a series ciruct current is the same at any point, only voltage changes.
The way to find out the resisitance needed in a cell is r=v/I,or with a 5volt 50amp power
supply a cell with the total resistance of .01 would draw the max current that the supply
produces. Can be done and works well.

monkey
posted 08-05-98 03:44 PM Click Here to See the Profile for monkey I don't
think so. You _might_ be able to use mercury and a
flowerpot to reduce P2P and ring-substituted P2P's (Synthesis
November 1987 p.1005), but not ephedrines, and mercury is useless
for electrolytic oxidations and isomerizations of olefins.
The Fujisawa method of meth from chloroephedrine (CA 46:2432a)
is pure crap.

Prove me wrong. Post a working recipe.

rgds,
monkey

Lone Ranger
posted 08-09-98 12:48 AM Click Here to See the Profile for Lone Ranger
Monkey - I am with you on this one.
Bookworm II - I say that 5V, 50 amp is not useful because .01ohms through the circuit and
solution is very unrealistic! Try it - I cannot even get into this ballpark! My
electrolysis experiments require 10 volts to even draw 5 amps!

Joe uGly
Member posted 08-10-98 08:44 AM Click Here to See the Profile for Joe uGly I
heard that in Fester's new method, the psudo needs to be changed into an ester before
processing with electric current. Are there more than one kinds of ester??
How would you go about the rxn for this?

Joe

monkey
posted 08-10-98 11:00 AM Click Here to See the Profile for monkey A
simple recipe for sulfuric acid ester:

1. Pseudoephedrine freebase, 20g (works OK too with hydrochloride.
Phenylpropanolamine works too.).

2. H2SO4, 85% concentration, 60ml (103g).

3. 250 or 500ml Ehrlenmeyer flask with 1-hole stopper, 3 ft of tube.

4. Tube leads from stopper down your drain and around the U-trap.

5. Chipped-icewater bath for the flask.

6. Chill ingredients #1 and #2 in freezer first.

7. 75 ml Jose Cuervo La Rojena Tequila or 40% EtOH, similarly chilled.

8. 75 ml 99%+ isopropanol, similarly chilled.

9. 250ml graduated cylinder which will take a stopper and fit in your freezer.

10. Funnel so you can pour into grad cylinder from flask.

11. Bucket of cold water with a few tablespoons of baking soda.

With tube in place, stopper ready to go, flask in icebath,
put pseudoephedrine in flask, add H2SO4, quickly stopper.

Sulfuric acid will proceed to slowly dissolve pseudoephedrine, with
evolution of nasty fumes which go down your drain. Run a little
water from your faucet down the drain to entrain and carry fumes
into your septic tank. Swirl flask a bit, to get pseudoephedrine
which foams up above top level of liquid.

Keep flask ice-cold. Digestion is complete in approx. 30 minutes.

Unstopper flask. Fumes are not too bad, but better do it by the
window with fan blowing out. Quickly add tequila. Then add isopropanol.

Pour this mixture into the grad cylinder. Stopper. Put in freezer.
Take tube out of sink and drop into bucket of soda water. Clean
stopper and tube. Wash and put away flask. Wait two weeks.

The white stuff which precipitates out at the bottom of the grad cylinder in your freezer
is your ester. Pipette clear liquid off, mechanically rinse white stuff out with cold
isopropanol. Can be cleaned of excess H2SO4 by rinsing with cold iso-p on _very fine_
filter paper. Coffee filters will work, but some product gets through.

Monkey will bet you his Nolan Ryan autographed baseball, you can't reduce it
electrolytically in a flowerpot.

rgds,
monkey

Joe uGly
Member posted 08-10-98 12:28 PM Click Here to See the Profile for Joe uGly Hey
Monkey,

I believe Festers method uses a naturalamb condom (unlubricated), with the lead anode
inserted (tee-hee). It then uses a palladium bar or screen for the cathode in a 500ml
beaker. The palladium generates hydrogen that drives the reaction.

Your comments are appreciates!

Joe

monkey
posted 08-10-98 02:25 PM Click Here to See the Profile for monkey Sounds
to monkey like a waste of the best condom on the market. Will look into it. Any details as
to electrolytes, concentrations, voltage, current passed, etc.?

rgds,
monkey

BTW if any Real Chemists want, monkey will post the "real" way to make the ester.

Sharp
Member posted 08-10-98 02:57 PM Click Here to See the Profile for Sharp Monkey,
on the old board UF mentioned that the Pd cathode needed to be anodized(sp?) first. Any
posted on that would be greatly appreciatied.

Joe uGly
Member posted 08-10-98 03:27 PM Click Here to See the Profile for Joe uGly I
would like to know the real way to make the ester. I don't have any more info on this
reduction. Will have to wait for fester's book. Should be out by Nov/Dec from what I last
heard.

Joe

Lone Ranger
posted 08-10-98 04:30 PM Click Here to See the Profile for Lone Ranger
"Monkey will bet you his Nolan Ryan autographed baseball, you can't reduce it
electrolytically in a flowerpot"

Maybe not, but I'll bet 100grams of 2,5 dimethoxybenzaldehyde that Pd/C or Pd/BaSO4 in a
sodium acetate buffered solution and hydrogen atmospere will make short work of that
ester, at room temp and pressure. Using this ester is likely the easiest way of doing
catalytic reduction.

monkey
posted 08-10-98 07:55 PM Click Here to See the Profile for monkey Sharp:
m will check into it and get back to you. Did Fester provide any hints of either the Pd
alloy manufacturer/number, or else how this anodization was accomplished?

Joe and LR: Well, perhaps monkey has made a glaring error. But you might lose your
aldehyde too, LR.

Let's all take a close look at Helvetica Chimica Acta, 1929. Author, Hermann Emde. You and
monkey have talked about this before, LR.

Experimental (Here's what you want, Joe). (+)-Pseudo-ephedrin-O-sulfuric-acid-ester from
(-)-Ephedrin. p.402, translation from the German by monkey:

"Into 100g ice-cold conc. H2SO4 one adds 20g natural (-)-ephedrine hydrochloride in about 40 portions within 10 minutes. Thereupon vigorously develops hydrogen chloride. One shakes under ice-cooling, until it all has dissolved, rinses the residue from the walls into the bottom with 10 cm3 conc. H2SO4, takes from the ice and leaves to stand 15 minutes at 15 deg C. Thereupon one pours under stirring onto 200g crushed ice, whereupon one also cools from the outside with ice, and adds 300 cm3 absolute ethanol. Thereby precipitates the (+)-Pseudo-ephedrin-O-sulfuric-acid-ester in beautiful white crystal needles. One filters through a Buchner funnel (the original reads "nutscht durch einen Glastiegel ab", which literally means "filters (or sucks) off from, through a glass crucible"; m thinks his translation as "filters through a Buchner funnel" is a fair assumption), washes with water and obtains about 10g (+)-Pseudo-ephedrin-O-sulfuric-acid-ester."

Emde, in the same four-part article, disclosed that he did _almost_ exactly what you say,
Chemo Sabe, but not on the ester; he used Pd/BaSO4 in a sodium acetate buffered solution
and hydrogen atmosphere to obtain the arrrrgh-dust formerly known as desoxyephedrine,
specifically he reported 3.27g of its hydrochloride salt starting from 3.89g of
(+)-chlor-pseudoephedrine hydrochloride (pp.373-374).

Then, further down on p.374, he casually tosses off the claim that "I have furthermore
prepared (+)-Desoxyephedrin also through a catalytic reduction of
(+)-Pseudo-ephedrin-O-sulfuric-acid-ester. In this case buffering of the reduction-mixture
is unnecessary, the calculated quantity of hydrogen becomes taken up within the
limits-of-error-of-measurement, and upon steam-distillation no di-desoxyephedrin remains
behind (monkeynote: this dimer formed during reduction of the chloro intermediate was
Emde's chief theoretical focus at the moment --or so he would have posterity believe
;-D)."

Emde concludes the paragraph with: "However, the smell of phenylpropylene enters in here
also, therefore here also are side-reactions, if only in quite insignificant quantity,
because the yield of (+)-Desoxyephedrin fulfills about 95% of the theory."

95% yield ...and that is all he wrote. Monkey looked a long time, back circa 1970, for
anything further written by Emde or anyone else, anywhere, ever, on the reduction of the
ester and never found anything which told further details. He says he did it without
sodium acetate buffering; in what solvent? In water, as with the chloro- compound? In
methanol, glacial HOAc, in huckleberry juice, horse piss, or what? It seems one of the
great mysteries of the ages. The hell of it is, monkey in his childhood, circa 1962, knew
a local pharmacy owner who was a contemporary of and studied with Emde. But, that was then
and this is now.

Monkey way back when tried every sort of PdCl2/Pd-BaSO4/Pd-C reduction, in water, in weak
HOAc, in glacial HOAc, in methanol, and probably in others, and never could get it to work
on any ester --even when exactly duplicating Emde's procedure for production of the ester,
from _ephedrine_. Nor from pseudo, nor PPA.

One thing monkey didn't try, though, was doing the hydrogenation under _pressure_. Maybe
that's the key. Son-of-a-bitch, looking closely at Emde's procedure, he says room
temperature, but nowhere does he mention pressure. That's gotta be it. So, you'd lose, LR.
Even though you said, in a post elsewhere, that you thought Pd + H2 + pressure would turn
the trick on the ester (though monkey erroneously called it "sulfonic acid" ester). I'll
bet you were right after all --the first time.

And the glaring error which the monkey formerly known as a chemist _may_ have made, of
course, though maybe it wouldn't result in failure, was starting in his posted simple
recipe from pseudoephedrine.

Phenylpropanolamine shouldn't make any difference in chirality, though. And even the ester
from ephedrine, the Emde way, didn't work.

So it was pressure. It was the only thing monkey forgot to consider, in his callous
arrogant youth. Got to be the key. Try starting at 3 atm and gage by uptake as measured by
drop. In gram quantities you could do it with a MHG (monkey hydrogen generator), running
via an inflatable pool animal or whatever, through a 12-volt car tire compressor, into an
SRV or KRV, a little water, a little HOAc, a little Pd-on-lithopone, your ester, some
shaking at RT e.g. hang it on a fishing pole off the back of your Land Rover and go for a
drive up a logging road, and voila, all-dextro crank with a lot less mess than the red P/I
route, no need for SOCl2 like the Gero route, and an exceedingly favorable
acquisition-and-smells profile.

Friends, as far as the biker crowd is concerned, it looks like we may be about to win
their war for 'em. Got to think about this. Would pseudoephedrine work. Damn. Monkey
wishes he had his old sticks-and-balls kit. Do they even sell those, anymore?

Let Me Know If You Dream This, LR.

rgds,
monkey

PS Hypothetically, if one had 2kg of aspartame, how might one derive phenylalanine
therefrom?

Lone Ranger
posted 08-10-98 10:02 PM Click Here to See the Profile for Lone Ranger
Monkey - I doubt aspartame can be changed into phenylalanine without a lot of trouble
(like protection). Easier to start with D,L phenylalanine from Twin Labs at your drug
store. The L kind is no good.

For all reductive methods pseudoephedrine is identical to ephedrine. The "right" ephedrine
is 1R,2S)-(-)-Ephedrine, as in cold pills. The "right" pseudo is
1R,2R-(-)-Pseudoephedrine. The other isomers, with the Nitrogen flipped instead of just
the soon-to-be-gone hydroxyl flipped, are not OTC.

I am not too impressed with this electrolytic method - I was saying that the ester might
be wonderful for catalytic reductions. Much better than OH, better than C, as good as B -
as in bromoephedrine - which reduces easily to you-know-what in just 2 hours at RT (under
H2).

I have been in touch with my Grandma, who is researching the reduction of the acid
chloride of R-phenylalanine. No real news yet - see "Novel Synths"

I have burnt my substrate attempting to make this sulfonic ester in the past, and asked -
but not gotten - help. I am in your debt for this last posting.

Lone Ranger
posted 08-10-98 10:10 PM Click Here to See the Profile for Lone Ranger
Well it's noe officially mislabeled as the "Sulfonic ester"!!

This method will work, I am certain. My Grandma has had success with the bromo and chloro
variations. Why did it fail you? Well, I have found that the catalyst must be reduced
before hand, and not all my Pd/C works. The 10% Pd on charcoal from Fischer is the best,
but this could be just that one batch. I have 3 other Pd catalysts that fail constantly,
and no hydrogen is consumed.

Hydrogenate your catalyst at elevated temperatures prior to use, to stand a chance.

Lone Ranger
posted 08-10-98 10:18 PM Click Here to See the Profile for Lone Ranger
One more thing. I had no results until I hooked up a flask clamp to a floor sander, as a
shaker. Stirring and hand shaking do not cut it. This sander SHAKES like hell, and things
started to look up.

Lone Ranger
posted 08-10-98 10:26 PM Click Here to See the Profile for Lone Ranger
Paeudoepedrine would form ephedrine-O-sulfuric acid ester. The ester appartently is
created opposite the original hydroxyl position. This should make no difference.

monkey
posted 08-11-98 03:37 AM Click Here to See the Profile for monkey Have
your grandma try monkey's method too, LR. Compare the yields. Post her results.

Sharp
Member posted 08-11-98 08:16 AM Click Here to See the Profile for Sharp Monkey &
LR, I hate to even post such trival info after such exchange of brilliance and chemical
savvy. But I was asked a question.
The Pd in question was what I believe to be an ordinary Pd 1oz ingot that can be purchased
at any coin dealer. As far as the anodization, UF mentioned that the surface of the ingot
must be oxidized I assume to be able to do what ever Pd does in this rxn(sounded good till
the end). How this process is done it was not mentioned, just that it must be done.
LR, Are esters required fo all Pd/H/pressure reductions.
LR,

Joe uGly
Member posted 08-11-98 12:54 PM Click Here to See the Profile for Joe uGly I
love this place!
Joe

Joe uGly
Member posted 08-11-98 03:24 PM Click Here to See the Profile for Joe uGly Hey
LR,
Is POPeye's home Hydrogenation similar to your dream? Will his version work?
Thanks man,
Joe

Lone Ranger
posted 08-11-98 04:43 PM Click Here to See the Profile for Lone Ranger I
do not know if POPeye's Acetic acid/H2SO4 method works or not. I have a ref saying that a
few drops of H2SO4 in water with Pd/C will reduce ephedrin at 50deg and 45-60psig of H2.

I am more familiar with room temp and pressure reductions, which require the bromo or
chloro compound. The H2 is usually in a balloon, but sometimes an inverted graduated
cylinder is used, so the H2 uptake can be measured.

Going through the Monkey Ester may require slight pressure(2 or 3 atmosperes) and temps.

The catalyst must be reduced right before use, and the agitation must be extreme.

I have had no luck with any reductions in Acetic acid - Ethanol is my first choice,
methanol should be fine. I like these primary alcohols because the catalytic reduction of
a secondary alcohol is easier. Primary alcohols can be reduced slowly in this manner, but
all the starting material would be reduced before this happens.

Sharp - I do not know enough about electrolytic reductions to comment on the use of Pd
electrodes. The new Amphetamine syth book shows a cell using lead and carbon electrodes.
Get the carbon rod from a large "F" drycell. It even has a stud and nut to connect your
wire to!

monkey
posted 08-13-98 04:59 AM Click Here to See the Profile for monkey
BookwormII: your humble supplicant monkey knows the feeling well, of having a piece of
knowledge which others lack, and the superior feeling which said exclusivity may endow one
with. He also is well aware that, --in fact, you have just seen an example of how--
sometimes, even the most advanced and widely praised investigator can actually be
not-in-possession of the true leading-edge.

If you can bring yourself to regard us, from your uniquely-high vantage point, as in
however small way worthy of such condescension on your part, though we are by no means
your equals, and have doubted you in the past... we now offer our sincerest and most
penitent apologies and obeisances. Graciously hearken, O Thee Of The Dazzling
Effulgence... to our sincerest, most earnest requests as sightless, lost and confused
beggars,... and kindly bestow upon us such Welcome Guidance as we may be Fit To Receive.

Respectfully,
monkey

LR: it is an honor and a privilege, to have been of some small service to The Masked Rider
Of The Plains.

Sharp: monkey thinks he will keep his yap shut, until he sees this book. You have m's
word, if he's trying to baffle us, m now can and will bust him --fast and hard. But m will
supply no further clues to help him try. On the other hand, if he's even halfway in the
ballpark, and on solid ground, m suspects he can take it the rest of the way.

Caution to all: if you try it, all the shielding you can think of, ten feet or so at all
times between you and the running apparatus, and a particle counter with its face(s)
positioned closely, so as to catch planarized emissions near the corners of the palladium
electrode, might not be a bad idea. Also check temperature of electrolyte. You will be
duplicating certain aspects of Pons/Fleischmann-type experiments. Monkey could say more on
this, but, not yet.

rgds,
monkey

Joe uGly
Member posted 08-13-98 12:07 PM Click Here to See the Profile for Joe uGly What
the hell are planarized emissions?? Are these toxic or cancer causing?
Joe

Lone Ranger
posted 08-13-98 04:08 PM Click Here to See the Profile for Lone Ranger
Monkey says:

Caution to all: if you try it, all the shielding you can think of, ten feet or so at
all times between you and the running apparatus, and a particle counter...
...............small cut............
You will be duplicating certain aspects of Pons/Fleischmann-type

Yes, you will be duplicating the work of Pons and Fleischmann in some respects (although
they felt thet the Pd should be deuterated). For those that do not recall, these are the
"cold fusion" guys. However there is no need to worry, they were victims of "pathological
science". There is no cold fusion, no particles will be emitted.

I have personally been involved with several experiments aimed at verifing "cold fusion".
All were failures (and your tax dollars at work). Small scale fusion events were observed
when 10 MILLION volts were used to bombard a Pd target that was tridium or deuteron
enriched. Even with this extreme high voltage, radiation was minimal. There was never a
chance of achiving the "break even" point, of course. Input power was kilowatts, output
power was nanowatts! Since the home cells will not exceed 12 volts or so, there is no
cause for concern.

The similarity of a Pd reduction cell to the "cold fusion" cell is an astute obsevation,
however.

Invest in a fume hood, not in shielding.

Joe uGly
Member posted 08-18-98 02:07 PM Click Here to See the Profile for Joe uGly
Anodize
: to subject (a metal) to electrolytic action as the anode of a cell in order to coat with
a protective or decorative film
- an·od·iza·tion /"a-"nO-d&-'zA-sh&n, "a-n&-/ noun

You must need to do this before you use the pallidium as a cathode?
Joe

FMAN
Member posted 12-19-98 04:02 AM Click Here to See the Profile for FMAN Config
this. A tire, with two check valves. Plexi mounted where the hub should be. A whisper fish
pump. A regulator to fill and exhaust gasses at the portals. A window that opens outward,
in case of explosion and an enterance for the hand, that opens inward. A pressure gradiant
is invoked to vent O2 gas from the Anode side of the reaction vessel as it is formed.
Pursuant to safe and applied home technique. Place this configeration behind a window or
other mount as you desire increassing saftey margins.

Bozakium
Member posted 12-21-98 12:48 AM Click Here to See the Profile for Bozakium KrZ,
whaddya mean thats Fester's post? It has your name on it.
ANYHOO, It seems to me that by so many of the questions being on very basic things covered
in the original method, that maybe it got lost. I know no one likes being told "just
search for it" so I'm gonna repost it here for all y'all.
As for voltage and current, any power supply capable of enough voltage to pass the
required current will be OK, but unless one has a current-regulated supply(rare), one will
have to hook an ammeter in series with the cell and adjust the voltage to keep the current
constant as the cell's resistance changes. A good idea is to graph current vs voltage, as
one slowly raises the voltage. At a certain voltage, the curve will flatten out. This is
where the reaction is taking place, as the current is being absorbed in the reaction. If
one goes too high,the curve will climb again. Some systems, such as the electric
production of meth from phenylacetone and methylamine in Festers new book, will have other
reactions that take place(causing curve flattening) at higher voltages, so plotting the
graph is important to be sure the proper potentials are used.
When my sabbatical is over, I'll look up a nice current reg supply for y'all.
As for all the substitutions of esters and dividers and electrodes, why not attempt the
reaction AS GIVEN in the original work before trying substitutions? Thats the way real
scientists do stuff.
I have heard from a reliable source that, as is, this method does work.
There's a reason lamb condoms, NOT rubber ones, are used. Ditto for the ACETYL ester, and
the Palladium electrode.
Current/voltage curves are given in Advanced techniques.., which is at Loompanics now.
Please dont dis Fester till' ya try the method as given. Hypothetically of course.

DISCLAIMER: THE FOLLOWING INFORMATION IS FOR INFORMATIONAL PURPOSES OR ACADEMIC STUDY
ONLY. CHECK YOUR LOCAL, STATE AND FEDERAL LAWS, AND PROCURE THE NECESSARY PERMITS BEFORE
UNDERTAKING ANY OF THE REACTIONS DESCRIBED BELOW. NEITHER BOZAKIUM NOR UNCLE FESTER SHALL
BE HELD LIABLE FOR USE, MISUSE,
INJURY, DEATH, IMPRISIONMENT OR FELLATION DUE TO THE APPLICATION OF THIS INFORMATION.

"Festerlytic Hydrogenation''

Preface:
As those of you who have been following the chem scene this year know, the new
book from Uncle Fester has been promised and promised by Loompanics since March or
so of this year, with the release date continually being pushed back, despite the word
that it was "at the printer's" in June. I have been privy to the manuscript of a very,dare
I say,revoloutionary chapter of this book since much earlier this year, and out of respect
for the author's need to make a living, not divulged any "trade secrets" though I have
told of said formula's most vital element, and teased of the simplicity this new Fester
Method. Now several months later, and nearly a year since the book was written it is still
not available and we are now told by 'Panics to expect it in September sometime.Yeah,
right (sarcasm here folks). Anyway, while discussing this with Fester, I mentioned how I
had teased the swarm with hints of the new method , but hadn't divulged any "trade
secrets". The embittered Fester, pissed at the gravelly hand-job Loompanics has been
giving him(allegedly due to management changes or something) defiantly trumpeted: "Divulge
Trade Secrets!" I nearly busted at nut with both excitement and relief that I could now
share this breakthrough with you, the scientific world. My shit-eating grin still aglow,
Uncle excitedly gave me two new references which promise to significantly shorten reaction
time. It is now my great honor to share this knowlege in the interest of the furtherment
of science. Enjoy.
--Bozakium 1998


THE 1998 FESTER FORMULA:
Electrocatalytic Hydrogenation of Ephedrine, Pseudoephedrine And Phenylpropanolamine

Absract:
Reduction of the hydroxyl group of various 1-phenyl, 2-amino propanols and their
substituted amino variants are easily and efficiently carried out by electrocatalytic
hydrogenation of their respective acetic esters at a palladium or palladium-plated
electrode in a divided electrolytic cell. Use of a lamb's skin prophylactic as an
inexpensive yet effective cell divider is also demonstrated in this experiment.

Materials:
-One (1) gram of purified ephedrine, pseudoephedrine or phenylpropanolamine.
-One troy ounce ingot of palladium
- glacial acetic acid
- concentrated sulfuric acid
-sodium hydroxide
-anhydrous HCl gas source
- pH-indicating paper
-toluene
-Kling-Tite Naturalamb brand condoms
-lead or graphite electrode 1/2-inch wide by five inches long
-six one-inch alligator clips
- several feet of 16 to 20 gauge insulated copper wire
- variable DC power supply
- ammeter capable of measuring up to three amps, with resoloution to the tenth of an amp
-voltmeter(optional)

Procedure:
One gram of ephedrine, pseudoephedrine or PPA hydrochloride is placed in a large test-
tube along with 5-7 mL of glacial acetic acid. The test tube is heated in a water bath
until all the ephedrine(in this case) hydrochloride is dissolved. A few drops of
concentrated sulfuric acid are added. Mix it all together and LOOSELY stopper the end of
the test tube to prevent steam from entering. Heat the water bath to just about boiling,
and use it to heat the test tube and its contents for a few hours. This forms the acetic
ester of the ephedrine, pseudoephedrine or PPA used in the reaction. The solution should
appear clear and water-like, completely homogenous. After heating,the reaction mixture can
be kept stoppered as is for a few days, but it's best to use it immediately after it's
cooked.
Next, mix up a solution of 5 mL of concentrated sulfuric acid in 100 mL of water. Take a
250 mL beaker, and place it on a magnetic stirrer. Clip a well-scrubbed Kling-Tite
Naturalamb condom in one side of the beaker, and place a piece of lead 1/2 inch in
diameter and a few iches long inside the condom. On the other side of the beaker,
stand up a one-ounce ingot of palladium. Using alligator clips, make contact with the
ingot, and wth the piece of lead. They are your two electrodes.
Next, pour most of the dilute sulfuric acid solution into the beaker. Save enough that
some can be poured into the condom so that the solution levels are about equal inside the
condom and the beaker. The ingot of palladium should be almost completely immersed. The
alligator clip should be up out of the solution, and there should be enough space left to
add the ester reaction mixture from the test tube to te beaker without causing the
solution level to reach the alligator clip. The surface of the palladium ingot should be
lightly sanded prior to use. This increases its surface area a little and exposes fresh,
clean metal. The piece of lead should be scrubbed free of grease and dirt. The wire lead
to the Palladium ingot can be clipped to the side of the beaker with a clothes pin or
paper clip to prevent the ingot from falling over during the course of the reaction.
A DC current meter (ammeter) should be put in series with the wiring. A good one can be
had at Radio Shack for under $50.00.
The wires are first hooked up so that the palladium ingot is connected to the positive
pole of the DC power supply, and the piece of lead to the negative. The typical one- ounce
ingot will have a face with an area of about six square centimeters immersed in the
solution and one square centimeter up out of the solutuion. Only count the area on the
side facing the lead piece. The back side doesn't count because significant current
doesn't reach it. With this typical ingot apply about two amps for 30 seconds to one
minute. Oxygen will bubble freely from the ingot, and hydrogen from the piece of lead.
Blackening will be noted on the edges of the ingot, where the current is most intense, and
a lighter discoloration on the flat face of the ingot. This pre-treatment is called
anodizing. It has been found that anodizing increases the ability of the palladium ingot
to adsorb hydrogen when the wiring is turned around, and the ingot is made the cathode.
Next, redo the wiring so that the palladium ingot is attached to the negative pole of
the DC power supply, and the piece of lead to the positive. Turn the juice back on and run
between one and two amps of current for about 20 minutes. At first, the amount of
hydrogen generated at the palladium ingot will appear small. This is because the Pd
adsorbs hydrogen so well. After about five minutes of current passage, the whole
surface of the ingot will freely bubble off hydrogen. After the 20 minute charging with
hydrogen, begin magnetic stirring of the solution, and pour in about half of the ester
reaction mixture from the large test tube. Adjust the current flow from the variable power
supply so that a current of about 50 milliamps per square centimeter of palladium surface
flows. If one has about six square centimeters of the ingot facing the piece of lead
immersed in the solution, a current of about 300 milliamps is called for. This will result
in some gassing off of hydrogen from the edges of the ingot, but over the rest of its
surface the hydrogen will react before it bubbles off. The lead anode will form a brown
layer of lead oxide, and will not dissolve at all in the sulfuric acid solution.
Some surface particles will be kicked off the lead when it's first charging, but they
don't make it through the condom. The lead anode can be replace with a piece of platinum
if desired, but lead is a lot cheaper. Graphite is amother possibilty.
Keep an eye on the current meter, as the current flow can change as the reaction
progresses. Keep the current flow around 300 mA (0.3 amp) for the size ingot given in
this example. When 1000 coulombs ( a coulomb is a unit of charge equalling one amp-second)
have passed into the solution, add the other half of the ester reaction mixture from the
test-tube., and continue at 300 milliamps until 3000 coulombs have passed through the
solution. Let us use the 300 mA current to show an example of these calculations: At 300
milliamps, 1000 coulombs pass in 1000 / 0.3 Amps = 3333 seconds, or a little under one
hour. 3000 coulombs pass in 10,000 seconds, or two hours, 45 minutes. 3000 coulombs per
gram of feed material has been found to give good yields of a fine product, but by no
means consider this number to be optimal. It may well be that a greater yield would be
obtained by passing more current. It may also be that pseudoephedrine and PPA differ from
ephedrine in their ease of electrocatalytid hydrogenation. I don't think that
any harm can come from passing more current, within reasonable limits, so by all means
experiment with the amount of current passed.During the course of thi reduction, the color
slowly changes from its initially clear color to slightly tinted with yellow. It's not
known whether this color change is due to some of the condom soaking out, or if it's a
byproduct of the reaction. In any case, it's a remarkably clean reaction.
When the desired amount of current has passed, the work-up and isolation of the
product is very simple. The Kling-Tite condom is removed from the beaker. after pulling
out (no pun intended) the lead electrode, the jimmy hat is, as is custom in some parts,
flushed down the toilet. The anode can be used over and over. The palladium cathode is
then rmoved and rinsed off. It too can be reused an INNUMERABLE (Bozakium's emphasis)
number of times. The process of anodizing the palladium will have to be repeated prior to
each run. Some fresh metal may have to be exposed on occasion by
light sanding of the metal surface. An ingot of palladium should last for a lifetime.
The reaction mixture should be poured into a sep funnel, and a 20 % NaOH solution should
be added with shaking until the solution is strongly (13 + pH) alkaline to pH paper.
Extract with two 50 to 100 mL portions of toluene. This should be plenty for one-gram
of product. THe toluene extracts are then bubbled with dry HCl to get the crystalline
hydrochloride product. After rinsing them off with some fresh toluene, they are spread
out to dry. The most pleasantly surprising finding is that crank produced by this method
doesn't give one the body and soul-wrenching hangovers so typical of the product made by
the iodine-red phosphorous method.. This is a highly desirable way to keep one's own party
rocking and rolling.
If one should wish to produce more than a gram or so at a time, a larger palladium
cathode should be used. Linking together more ingots of palladium would get pretty
expensive, so a more economical alternative will be detailed. That alternative is
electroplating some copper or brass screen with a thick coating of palladium.
The simplest way to get this section of screen electroplated with palladium is to go to
the yellow pages, look under electroplaters and find one who plates palladium. Ask for a
plate build-up of several thousandths of an inch, so that enough Pd is deposited to last
awhile..
The Pd plated screen would then be used exactly like the ingot. First it must be
anodized, then charged up with hydrogen in exactly the same way. The sole difference is
that the greater surface area of the screen facing the condom-encased anode requires a
correspondingly greater amount of current to be passed. Then, during the course of
the reduction, again 50 milliamps per square centimeter of surface area facing the anode
is used. The total of 3000 or so coulombs per gram of feed material doesn't change by
increasing the size of the electrode.
An alternative to this is plating the screen yourself, anodically dissolving a portion of
the ingot to form a PdCl2 solution then..... sorry folks, this all of the manuscript I
have, but I'm sure palladium plating is no national secret (yet). There is a company that
sells an electroplating kit consisitin of a power supply, metal solution and a 'pen'
electrode. As soon as I find their paperwork among my rubble I will post it. The lastest
word from Fester is a couple of references from Indian journals on electroplating graphite
electrodes with palladium, essentially giving a Pd black on C
catalyst in the cell!

1) Electrochemica Acta 1976 Vol. 21 Pg.449-450 Krishnan(author) On the
Electrochemical Reduction of Benzyl Cyanide to Phenethylamine with a Pd/C Electrode
(note: The title may not be exact due to the illegibility of my chickenscratch
transcription of my conversation with UF.)


2) Journal of Applied Chemistry 1975 Vol. 5 Pg.125-128 Krishnan(author)

The greater actiivity of Pd on C (over straight Pd) results in a shorter reaction time.

If anyone manages to find these references, please post them at the hive.
I'd also be happy to answer anyone'e electrical questions, as long as you are not doing
anything illegal of course. Please keep me abreast of your dreams & enjoy.
------Bozakium

KrZ
Member posted 12-21-98 02:59 AM Click Here to See the Profile for KrZ I copied
it from UF's post on the newsgroups. Thats what I mean.

Beaker Babe
Junior Member posted 12-21-98 08:34 AM Click Here to See the Profile for Beaker Babe
Boz, thank you for the reposting. I believe most people would agree that the secret is in
the ester, which seems to be the problem. Lets assume that one has the purified feedstock
to begin with, via a/b extraction. Here are two a hypothetical reactions with results:
Both use the following- 4grms eph(not psed)feedstock, 40mmx50mm reaction area on flattened
pd ingot, pt in lambskin, 200ml dh20 with 10ml h2so4 electrolite, 6 hours at .8 amp
w/stirring. Let assume procedure follows above except all ester is added at once, per
festers book. Theoretical results with two different ester production techniques.
1. 7ml gaa with 3-5 drops h2so4 results in slightly cloudy yellowish ester(not really an
ester?), turns electrolite cloudy white upon pouring in, turns clear has reaction
precedes(slighly yellow). A/B extract yeilds easily gased out non-reduced eph.
2. 9ml gaa with 1ml h2so4 results in clear brownish ester(an ester?) which is oil like
when poured in and electrolite lightens in color has reaction precedes. A/B extract yeilds
nothing but a little oil on bottom when gased. When oil is precepated with acetone seems
to have a little kick, but disappointing.
These two theoretical rxns may have results some bees are getting and these problems need
to BE discussed, please! You wanted details there you go!

Bozakium
Member posted 12-21-98 02:41 PM Click Here to See the Profile for Bozakium
KrZee: Thanx I knew that post sounded familiar. It Is really old though.

BeakerBabe:, thankx for the details, I'll ask around among the penguins. One possibility
for now is to hypothetically try only 1 gm of feedstock. I have recieved correspondence
stating that this is a small-scale synth only, perhaps there is a problem with upping it
400%. I guess you dont have an IR spectrophotometer handy, huh?

Bozakium
Member posted 12-21-98 02:45 PM Click Here to See the Profile for Bozakium
KrZee: Thanx I knew that post sounded familiar. It Is really old though.

BeakerBabe:, thankx for the details, I'll ask around among the penguins. One possibility
for now is to hypothetically try only 1 gm of feedstock. I have recieved correspondence
stating that this is a small-scale synth only, perhaps there is a problem with upping it
400%. I guess you dont have an IR spectrophotometer handy, huh?
I'm glad ya appreciated reposting the technique, I wasn't sure if I should've done it or
not, bandwidth being slim and all. If I was moderator of this forum, I would've edited the
procedure out and just put up the link to it on Rhodium's site. The formatting is much
better there anyway.

Bozakium
Member posted 12-21-98 02:49 PM Click Here to See the Profile for Bozakium Damn
double-posting. I thought I hit the stop button in time. Sorry, folks. I guess I'd nix
that one, too.

Beaker Babe
Junior Member posted 12-21-98 06:06 PM Click Here to See the Profile for Beaker Babe
Boz, hope the penguins have some good ideas! Certain nationwide hobbie electroic supply
stores in malls have a little catalog for sale that have several current regulating units
for sale to the public(up to 2amps self regulating) $200 bucks and up. Some bees may get a
little agressive with so much invested (ingots,stirrer,powersupply,etc.) just to get a 1/2
grm by the time it's all over that would be gobbled up in minutes, not to mention the
effort involved in the rxn itself, is tuff to justifiy. But ones love for chemistry keeps
us trugging onward!

Bozakium
Member posted 12-22-98 01:47 AM Click Here to See the Profile for Bozakium I
think the key to larger amounts may bee a multiple-cell setup, combined with a higher
current and carbon(Pd on C) electrodes. In a few weeks I'll post an under 50 bux current
regulated power supply plans from TV Shed.

Beaker Babe
Junior Member posted 12-22-98 05:34 PM Click Here to See the Profile for Beaker Babe
Thanks Boz, as you stated above maybe a return to the basics is in order. I'am sure most
bees would just like to have this elusive ester formula puzzle solved. Please!, may the
penguins see the misery we suffer and bestow on us the knowledge we seek!

Wizard X
Member posted 12-22-98 08:28 PM Click Here to See the Profile for Wizard X All
of you busy bees let me tell you something, electrochemical reductive cleaverage of an
acetic ester or a hydroxy group works well only if the group is :

-CH(OH)-COOH or -CH(acetic ester)-COOH
or
-CH(OH)-CN or -CH(acetic ester)-CN
at 3.0 - 4.5 volts
Acetic ester or hydroxy group reduction works well with Pd/C : H2 hydrogenation.
Now Boz, I know the answer to this question, but I want to hear your reply! What is the
Polarography wave ( voltage/current curve) of the reaction.

Beaker Babe
Junior Member posted 12-23-98 08:26 AM Click Here to See the Profile for Beaker Babe
Come on Boz one more post before you leave! It would bee a wonderful Xmas present if this
puzzle could answered for the many bees that will be busy working in there hives this 4
day weekend!

Nefertiti
Member posted 12-23-98 10:26 AM Click Here to See the Profile for Nefertiti
Someone_who_is_not_me also got a black/red tint solution while making the acetic ester.
They used 100ml Kodak Glacial Acetic Acid, 12g of pfed, 24 drops pHdown heated on medium
heat ~75C for 3 hours. Any explanations?

Nefertiti

Bugs Bunny
Junior Member posted 12-26-98 04:47 PM Click Here to See the Profile for Bugs Bunny
Ive finally aquired all things necc to attempt electrochemical reduction. Poverty has
decided that I use Ag instead of Pd. If all goes well on 1g Im hoping to scall up 4x by
doubling the beaker diameter and using 4 cathodes placed 90 deg apart from each other with
the anode in the middle. Also as research funds become more available am planning to try
Wizard X's ideas as she/he seems to have a damn good grasp on this. Today a beginner who
knows maybe tomorrow the Nobel Prize for electrochemical reduction of x.

Now for the stupid newbee questions.

Some posting suggest that "a lot" of hydrogen is produced from this exper. What is the
cheapest way to get rid of it? Would a fan pulling it into a plumbing vent stack work or
would the sparks from the fan blow me and my nieghbors up? The same questions for toluene.
Assuming both are lighter than air they should go right up the stack and join the rest of
the pollution my town gets to breath. If Im wrong then give me hell. As all my roomies are
away for the holidays now is a good time for me to play with this. I will await an answer
before becomin a newpaper article.

Many thanks in advance.

------------------

fj
Member posted 12-26-98 05:07 PM Click Here to See the Profile for fj Back when I
was hot on this method I got a more-or-less clear ester solution, a lot of other people
did too. That's how it should appear. The process is too simple to mess up really, unless
you allow moisture or condensation into it. So the problem, it seems to me, must be impure
starting materials. There are about 10 zillion ways to extract ephedrine, and I don't
doubt that some of them bring over dissolved adds from all the pill formulations.

The Fester method needs pretty good purity from start to finish, that was my experience.
If you aren't doing a good A/B extraction on the ephed, you don't know that you're
bringing over just alkaloid material. That's my opinion, as shaky as ever.

Wizard X
Member posted 12-26-98 08:34 PM Click Here to See the Profile for Wizard X Bugs,
just don,t let the hydrogen gas or the tolulene vapour concentraction build up or the fan
motor spark could set it off. Have good ventalation and you'll be fine.

Nefertiti
Member posted 12-26-98 09:09 PM Click Here to See the Profile for Nefertiti If
it is that the starting base is impure - is there a bee out there that is wise enough to
be able to figure out what product is getting formed from a base of pseudoephedrine and
triprolidine with Fester's method of obtaining the O-Acetyl Ester? I understand that the
best way is A/B - but someone not me has already ruined it seems 20g and is wondering if
there is a way to salvage or use as long as the byproduct is not chemically active or
poisonous......
Nefertiti

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Author Topic: Ester Q...
Backdoor469
Member posted 04-08-99 10:27 AM Click Here to See the Profile for Backdoor469 In
making the hypothetical ester of pfed can one use the common photo 28% acetic acid with
success and if so does the quantity of acid need to be increased from the 10ml/6g ratio?

dwarfer
Member posted 04-08-99 12:58 PM Click Here to See the Profile for dwarfer No, it
must be glacial because otherwise the water interferes with the desired end.

I have a question which has not been answered about the process, however: is the addition
of the small quantity of H2SO4 also to the GAA to act as a dryer, or is it actually a
catalyst for the reaction??

Thank you
dwarfer

Crissp
Member posted 04-09-99 01:38 PM Click Here to See the Profile for Crissp Just
yesterday in O chem lab, we esterized cotton(which is a poly saccharide, it has three OH
groups per monosaccharide unit). We used GAA, acetic anhydride, and H2SO4. Anyhow, the
teacher said that the H2SO4 was a catalyst. I'm not sure exactly how this functions. He
never mentioned anything about how water would interfere, but I'm sure he doesn't even
think about it knowing we're using reagent grade stuff at school. Esterizing cotton(only 2
out of 3 groups are effected) is how they make the plastic used in overhead sheets.
Dwarfer,
now then can you tell me how long you usually leave the tupperware on the boiling water?
And how do you reclaim your esterized crystals. Just a regular acid base extraction or
evaporate GAA or what. Those questions would really help me out. Thanks a bunch

Free Radical
Member posted 04-10-99 12:01 AM Click Here to See the Profile for Free Radical
Dwarfer,
Where does one acquire glacial?
Photo supply for *stop bath*?
Are there other sources readily available?

Thanks


FR

esop
Member posted 04-10-99 04:26 AM Click Here to See the Profile for esop hey guys
:

stop bath is *not* 28% acetic acid

a brand :
Hilford *concentrated* stop bath
is to be diluted...
a 10(GAA) : 1 (H2O) ratio
to make *print* stop bath
for B&W print developing
process.
( your standard B&W process...)

hope this helps

esop

Dreamer Envy
Member posted 04-10-99 02:35 PM Click Here to See the Profile for Dreamer Envy
Acetic Acid, Glacial 99%
Would there be any benefit to running
this through a drying agent? Thanks DE

corrodium
Member posted 04-10-99 02:47 PM Click Here to See the Profile for corrodium If
someone had a hard time with the ester step, I would not want to be around them if they
attempted to butter toast or steam a hotdog!

Free Radical
Member posted 04-10-99 06:38 PM Click Here to See the Profile for Free Radical
esop,

I found this at a Photo supply website.

If *stop bath* is not 28%,then why are they making this claim?

EK6031 28% ACETIC ACID STOP BATH*** $5.39

Just curious?


FR

corrodium
Member posted 04-10-99 08:49 PM Click Here to See the Profile for corrodium Any
professional photographers supply that carries Kodak film developing solutions has pure
glacial acetic acid that is supposed to be diluted 8 parts water/3 parts GAA to get 28%,
which is what film developers want. Kodak has gallons for $28 I think.

Stik E. Fingers
Member posted 04-10-99 11:51 PM Click Here to See the Profile for Stik E. Fingers
Photo supply centre redirected me to chem supply house with seeming (paranioa?) disgust
when I asked for glacial acetic acid, stating that it was a chemical and hence not
available here (!?). As I went with full straight, business~/family man conservative
bearing, looks, etc, and had researched GAA's photographic uses, it was a shock. My
questions now are:
Is CAA (or Kodak procces referred to in thread) only available in USA?
Is vineger simply acetic acid in water or does it contain expected, other, but lesser
products of acetic fermentation?
Attempts at contact drying with MgSO4 suggest acetic combines with Epson salt much better
than water (can't even regenerate). What other (contact or non contact)dessicants can be
used.
Thanks kindly again. Fingers

Free Radical
Member posted 04-11-99 01:34 AM Click Here to See the Profile for Free Radical
Corrodium,
Your price on the pure form is real close.
I found the dilute 28% for $5.39 and the pure for about the same price you mentioned.
One site I was at noted it as hazardous and wanted to charge an additional $12.00 on
shipping.
So I just went on to the next few sites,none of theme even mentioned the hazard thing!
I think that one site was just tryin to squeeze another $12.00 out!

Stik E,
Just type *Darkroom suppliers*,or "Photography supplies"
into your favorite search engine and start weedin em out!
I had more luck with "Darkroom supplies".

Don't even try searching *stopbath*,you will probably get nowhere fast.
I didn't try that,but I could only imagine!

FR

Dreamer Envy
Member posted 04-11-99 02:20 AM Click Here to See the Profile for Dreamer Envy
Corrodium

Lighten up on the Caffeine, you hit enter 3 times : )

corrodium
Member posted 04-11-99 07:50 AM Click Here to See the Profile for corrodium
Sorry,honestly I only click "submit reply" one time. If this posts three times then
something is wrong with my computer!Here goes...plastic baby food syringes for milliliters

Crissp
Member posted 04-11-99 04:35 PM Click Here to See the Profile for Crissp Great
then corrodium,
I butter toast(if peanut butter counts) every day, then it would be that easy for you to
email me with your exact process and you'd think nothing of it. I'd trade toast anyday.
Let's get down to business, enough talk. ***@hotmail.com

Crissp
Member posted 04-11-99 04:37 PM Click Here to See the Profile for Crissp Free
radical, you email me and I will email you back with a mail order place with GAA for 9
dollars a pint. Peace

corrodium
Member posted 04-11-99 05:34 PM Click Here to See the Profile for corrodium I
have only read this at:Bozakium post 01/25/99,Absolute post 03/03/99 and plus the Wizardx
post somewhere here. But all 3 are at www.villageidiot.webjump.com/index2.html the last
time I looked.

dwarfer
Member posted 04-12-99 04:22 PM Click Here to See the Profile for dwarfer The
esterified feedstock does not crytallize out at this step. It starts as an exceptionally
biting strong acrid dissolved salt, and changes it's biting characteristic as the reaction
progreses.

I have let it cook for up to 4 hours , with 5 to 8 grms of feedstock dried powder, before
commencing with the additon of the 5% H2SO to comprise the catholyte.

If you add too much H2SO4, you will wind up with a black "over oxidised??" mixture that
will reduce the yields.

Jut put in a few drops of H2SO4: not over 1ML has worked for me.


dwarfer

corrodium
Member posted 04-12-99 07:10 PM Click Here to See the Profile for corrodium When
ignited,H2 gas combines w/ o2 gas explosively in proportions ranging from 4.1% to 71.5%
H2. Ignition temp is 580C to 590C...Ref.Shakhashiri,Bassam Z. Chemical Demonstrations Vol.
1 Univesity of Wisconsin Press 1983 W/out details-Half Blind
Sailor-Pd/c/stock/glacial/sulfuric in SS pressure vessel sealed-introduce tanked H2,hold
to 38C w/ heat blanket,wait,filter etc.-or-Popeye's-Catalysts/stock,etc in vessel/add
hydrogen to 40lbs. then slowly release pressure-repeat 3 times to purge tank/pipe to
60lbs./shake or spin vessel and do not stop{very important}/when pressure drops to 20lbs
add H2/do this 3 times/"when H2 uptake stops-reaction is finished"/extract w/methanol-must
see these/no electrics/are these real anyBee?

Optimus Prime
Administrator posted 04-12-99 07:57 PM Click Here to See the Profile for Optimus
Prime man corrodium you gotta get that button fixed...

OP

corrodium
Member posted 04-12-99 10:42 PM Click Here to See the Profile for corrodium
Logitech First Mouse Plus/$31.93 at Walmart.The correct water temp is when the baby food
jar stops surfing around in the pot of water,I would say.Tec-America has Radio-Shack
electronics, for sale ,on it's shelves, in their stores!HHHMMMMMMMMMMMMM clic

chencho
Junior Member posted 04-12-99 11:22 PM Click Here to See the Profile for chencho
FYI, although it is not GAA, Kodak Indicator Stop Bath has a stronger percentage of acetic
acid than the 28% I have heard mentioned here.

http://www.holycross.edu/departments/publicsafety/website/msds/INDICATS.HTM
Kodak Indicator Stop Bath
ACETIC ACID, 85-90%
WATER, 10-15%
BROMOCRESOL PURPLE, < 0.1%

Raavin
Member posted 04-22-99 06:36 PM Click Here to See the Profile for Raavin I would
be interested to see if the esterification mentioned in SOMM4 under the Pd black/ hydrogen
method would work.

I've already posted a rundown at

http://hive.lycaeum.org/ubb_board/Forum6/HTML/000806.html

so if someone would like to try it we could have something.

good luck

Raavin

Raavin
Member posted 04-22-99 06:39 PM Click Here to See the Profile for Raavin OP also
mentioned something about bubbling HCl through either Methyl or Ethyl alcohol to get the
coeresponding ester of phenylaniline but didn,t elaborate. Nows your chance OP.

Pleeeeeeeez

Raavin

Optimus Prime
Administrator posted 04-23-99 05:51 AM Click Here to See the Profile for Optimus
Prime members.tripod.com/Optimus_4/esters.htm

OP

[Note: This message has been edited by Optimus Prime]

quick1
Member posted 04-23-99 02:15 PM Click Here to See the Profile for quick1 is it
ok to use the kodak stop bath instead of glacial? nobody around here has even heard of
glacial! they are like huh, what is that used for. next is sulfuric. don't you need a
permit for this kind of acid? what are some ways to pick up this stuff. i have not seen
any otc drain cleaners with it, so can anyone help

Wizard X
Member posted 04-24-99 12:27 AM Click Here to See the Profile for Wizard X BUSY
BEES : The heating of the reaction mixture is also important. If you heat a reaction
mixture at boiling water temperature for say 2 hours and you get a brown to dark brown to
black final reaction mixture then this is excessive.

That is why I gave you all a ester test so you can all monitor the ester synthesis
progress.

quick1
Member posted 04-24-99 07:35 PM Click Here to See the Profile for quick1 if you
run the kodak through a drying agent, would you have glacial? crissp, is the place you
talk of for individuals. if so could you let me in on your secret?

Commodium
Member posted 04-24-99 07:48 PM Click Here to See the Profile for Commodium No
need to be coy about where to get GAA. They can never put the pinch on this stuff.

http://www.photoformulary.com/BULK-PRC1.html

$8.95 per liter.

Smoothe
Member posted 04-25-99 12:33 PM Click Here to See the Profile for Smoothe test

Smoothe
Member posted 04-25-99 12:35 PM Click Here to See the Profile for Smoothe WIZ:
What have you found to be the optimal time and temp for the ester formation? I have only
dreamed of this reaction once and the final ester product obtained was a brown semi-solid
"gunk". Too much heat? Or was it too long of a reaction time? Thanks for all input!!!
Smoothe

Smoothe
Member posted 04-25-99 10:37 PM Click Here to See the Profile for Smoothe WIZ X:
Could you please post a link or tell me where the "ester test" is posted? I have look via
the search featuer but cannot find the message you are refering to... Thanks!!! Smoothe

Wizard X
Member posted 04-25-99 11:33 PM Click Here to See the Profile for Wizard X
Smoothe : Yes too much heat and reaction time. If you use my ratio of 9 mls of GAA and 1
ml of Con.Sulphuric acid to 1 gram of Eph, the 50 - 60 deg C for the first hour, and
monitoring throughout the second hour. That is if the solution starts turning brown and
the ester test confirms ester presents, then stop and remove from heating, and allow to
come to room temp.

ESTER TEST : Hydroxamic acid test for esters.
By comparing the colour of two samples produced before the hydrogenation and after, you
can determine the amount of ester reduced ( hydrogenated ).

Pre - test : To 1 drop of the Ephedrine acetic ester mixture in a small test tube before
the hydrogenation, add 1ml of 95% ethanol and 1ml of 1N HCl. Then add 1 drops of 5 % iron
( III ) chloride solution. If a violet , blue , red or orange colour develops, then the
test below can not be used as something ( contamination ) else is reacting with the iron (
III ) chloride.

[ 1 ] Place 3 drops of the Ephedrine acetic ester in a small test tube before the
hydrogenation. Place another 3 drops in a second small test tube after the
electrocatalytic hydrogenation is complete. Now add to both test tubes 3 drops of a
saturated solution of Hydroxylamine hydrochloride in methanol ( or 1ml of a 6 % solution
of Hydroxylamine hydrochloride in methanol to both test tubes ).
[ 2 ] Add to both test tubes 6 drops of saturated Potassium hydroxide in methanol
solution, or until distinctly alkaline to litmus. Remember add to both test tubes equal
amounts. Heat the mixture gentle just to boil, the cool to room temperature.
[ 3 ] Acidify both test tubes with equal amounts of dilute HCl ( 2N ) and then add to both
test tubes 2 drops of 5 % iron ( III ) chloride solution. A reddish ( burgundy ) or violet
( magenta ) colour will indicated the presents of ester.
Sample taken before hydrogenation is the control, assuming 100% Ephedrine converted into
the acetic ester.
The second test tube having the sample after the electrocatalytic hydrogenation will
indicate the amount of ester not hydrogenated.

Optimus Prime
Administrator posted 04-26-99 02:15 AM Click Here to See the Profile for Optimus
Prime Damn he's good.... Wiz if you dont mind Id like to put that on my site...

OP

(Lloyd)
Junior Member posted 04-26-99 08:24 PM Click Here to See the Profile for (Lloyd)
Hell, I've been overheating the stuff at first.

Wiz, is that stoichiometric?? How did you figure that. ??

I've had better results since I lessened the H2SO4 below the 2CC I put in with approx 2.5
to 3 gms feedstock. Maybe the crap i got was because of overheating??

I put the double boiler on and went and watched TV for a couple of hours.

So start at "hot water" for an hour: then to "boilin" for an hour: watching the second
hour for signs of "browning".

May I presume that the times do not change for larger inputs: just the quantity of
reagents? (stupid question)

Lloyd


Wizard X
Member posted 04-26-99 10:23 PM Click Here to See the Profile for Wizard X OP :
Sure it's OK by me.

Lloyd : Heat at 50-60 deg C for the 1st hour, then take a small sample of your reaction
mixture (max 3 drops) and test for ester. I ester is present then turn the heat off and
allow to cool back to room temp. If ester is not present then continue heating at 50-60
deg C keeping an eye out for signs of browning. Heat for another 1/2 Hour, then take a
small sample of your reaction mixture (max 3 drops) and test for ester.

Because the hydroxy is a secondary alcohol, greater reaction conditions are required to
force the reaction to the right.
Acetic anhydride and acetyl chloride reacts with Eph 100%, but also on the acidic hydrogen
on the nitrogen.

C6H5-CH(OAc)-CH(NAcCH3)-CH3

chencho
Junior Member posted 04-27-99 11:22 PM Click Here to See the Profile for chencho
Thanks Wizard X for all your wisdom

I'm wondering if one tried the ester process with free pseudo instead on pseudo HCL and
got brown liquid if that person would have produced pseudo acetate, which could be
recovered with NaOH.

Is pseudo HCL needed or can it be free pseudo?

Has anyone tested this brown stuff to see what it really is?

Now, I must locate Ferric Chloride OTC or check out rock shops for molycite.

Wizard X
Member posted 04-28-99 12:07 AM Click Here to See the Profile for Wizard X
chencho : both can be used.

One side reaction is dehydration of the Ephedrine acetic ester.

C6H5-CH(OAc)-CH(NHCH3)-CH3 == heat ===>>

C6H5-CH=CH(NHCH3)-CH3 + HAc

HAc is acetic acid. Because a double bond now exhists, polymerization can occur and the
acids are polymerization initiators.

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