                              HOME HYDROGENATION

 This is not an article on how to hydrogenate your home.  For that
information you would want to consult alt.elemental.architecture,
alt.explosions,die.die.die, etc.

 I am speaking within a very narrowly defined range here.  This outlines a
specific type of catalytic hydrogenation: the one I know about...don't
extrapolate any of this info toward broader chemical theory if
yaKnowhatImean. Coincidentally, this process can be utilized in the
manufacture of drugs like Methamphetamine and other home remedies.

 Hydrogenation is a chemical process which involves introducing elemental
hydrogen gas to a liquid solution  containing a catalyst.  The catalyst
latches onto the H atoms then gives them up, to bond with the molecules in
solution.


                         ~ Elements of Hydrogenation~

CATALYST-
 The catalyst consists of a metal in powder form which has been sifted into
a buffer like Carbon, it is all very fine powder, black and nasty,
shouldn't be inhaled and gets all over everything if you're not careful,
leaving your fingerprints for all to see.  Catalysts come in different
concentrations.  For example: 10% Palladium on Carbon would be 90% carbon
and 10% Palladium by mass, and is expressed: <10% Pd/C>. This procedure
describes the use of Pd/C as the catalyst.   Other catalysts are used in
hydrogenation but I am unfamiliar with them.

The catalyst is always settled and filtered out after the process, it is
then washed with distilled water, dried, and is reusable up to around 20
times.  With this in mind, it's not too expensive.

HYDROGEN GAS-
 The hydrogen is supplied from a pressure tank. A fresh Hydrogen tank
contains extreme pressure.  For this reason, a pressure regulater is
required , fitting a simple valve to the tank is potentially catastrophic.
Even pressuring a Parr shaker requires a regulated or low pressure feed.

 A regulator for a cutting torch is the obvious and best choice.  You have
to use the regulator and gauge set from the oxygen side of the torch
set-up, since it is designed for high pressures.  Once you have used a
regulator and hoses for hydrogen, NEVER use them for anything else,
hydrogen is absorbed into  materials and this limits their safe usage with
other gases.
Smaller gas containers can be obtained from scientific supply houses, they
are referred to as 'those little tank things' or 'watchamacallits' and may
require different hook-ups. I am unfamiliar with these, but I'm sure it's
all worked out.

Hydrogen gas is easy to produce yourself, but I have no experience or
recommendations in this area.

I guess everyone knows that Hindenburgers are char-broiled, or is at least
familiar with ledZeppellin album covers...hydrogen is very flammable,
doggone explosive, even.

 POPEYE perceives hydrogen line configurations as two types: fixed hose or
detatchable hose.


Fixed hose configuration:

                                  Exhaust valve->exhaust hose
                                        |
Reaction vessel<->Hose<->T fitting<->T-fitting <-Regulater <-H tank
                            |
                         psi gauge



Detatchable hose configuration:
                                                       -> exhaust hose
                                                    /
Reaction vessel<->T-fitting<->valve<->quick connect
                                                    \
                     |                                <-hose <-regulater<-H
tank
                 psi gauge

IMPORTANT: OTHER THAN THE REGULATOR, THERE ARE NO BRASS FITTINGS ALLOWED
HERE. THIS PREVENTS PRODUCTION OF WIERD CUPRIC TOXINS..Stainless or
specialized plastic, teflon, etc. must be utilized. Hose must be psi rated
and neoprene is best.


PRESSURE REACTION VESSEL-
        Where the gas and liquid get together with the catalyst.  It must
be able to contain (for our purposes) 60 psi, capable of a gas supply hose
connection, and an access opening at least the size of a quarter; silver
dollar or larger is better, any opening larger than 4" and I would do alot
of dry run pressure testing before using, to make sure it will hold.

        Stainless Steel is the only thing I would use. It's a snob thing.
                 Examples of SS containers which are easily converted:
                        Stove top milk steamer devices as used in home
Cappicinno synthesis as well as some types of stove top expresso makers.
There are as many varieties of these as there are Yuppies.  They have cool
little SS valves already configured in.
                        Soda fountain equipment. For larger batches, or
mandatory life sentence quantities,  the refillable containers that soda
fountain syrup comes in are excellent (they're about 6 gals), also the tank
on the CO2 maker.  These systems are phasing out right now commercially and
components are surplus everywhere.  Can also be ripped off from the little
fenced in area behind the local convenience store.


        Glass is used commonly, but I don't like it.  There is no advantage
in transparancy for this application. You have to be able to wire or clamp
a stopper and design a hose barb that won't pop out and guess at the psi
capacity. There is Sci-glass spec'ed for this.


        Chemical resistent polymer constructed pump garden sprayers aren't
bad and almost ready to go like they are. Come in all sizes, psi rated.
Very economical,  I always worry about polymers in the presence of benzene,
diethyl ether, etc., but haven't actually had any bad experiences. Polymer
gasoline containers are also used, but hose connection takes some
doing...not preferred.


SHAKER-
The Pressure Reaction Vessel is fastened to this mechanical
device...imagine a paint shaker...the paint can is your pressure reaction
vessel...that's it.  There are as many home hydrogenator designs as there
are ambitious speedfreaks. Some are brilliant, others are pretty damn
funny, still others are unintended amateur militia ordinance or automatic
911 dialers.  In deciding on, or tweaking out your own shaker device, there
are a few things you should know.

 As mentioned, the contents of your reaction vessel are a liquid solution,
which is flammable, and a solid catalyst in powder form.  The catalyst is
wha-chaCall PYROGLYPHIC (SP), implying potentially EXPLOSIVE. Into this you
are preparing to pump in HYDROGEN and fucking shake it ?!!
 Proper understanding of handling the catalyst is required.  The catalyst
is dangerous when dry and floating around in the air like dust, especially
around oxygen...see grain elevater explosions-Texas City Disaster.  Keeping
the catalyst wet throughout the entire procedure is key to survival.  This
is also why the Pressure reaction Martini is 'shaken not stirred' (kudos
jamesBond).  Those of you who have utilized mechanical or magnetic stirs,
know that the liquid occasionally sloshes up pretty high on the inside of
the vessel, the catalyst could easily slosh up there, dry out, then
dust...you know the rest.  With an effective shaker, the whole inside of
the vessel is constantly washed with solution so this cannot happen.
Therefore,this is the minimum level of activity required to prevent
incident.  Shakers also create the most desirable exposure of catalyst
surface area to the gas, increasing efficiency and uniformity of the
reaction.


Here are some approaches to shaker devices

Straightforward approach-go out and buy a paint shaker then design a
reaction vessel to fit it.  (fixed or detachable hose config.)

Bizarre approach- The Milwaukee Skateboard-> You will need: A variable
speed SAWZALL, a skateboard, a C-clamp, four 1x4's 12" long, A workbench
with a sturdy vice, electricity.
Place the body of a Sawzall in a vice so that it is parallel to the bench
and turned sideways, put two blades in the Sawzall by stacking them (short
blades).
C-clamp the blade tips to the stern of the skateboard which rides on the
benchtop.  Nail the 1x4's together so as to imitate two lengths of angle
iron each a foot long. Lay the wooden angle pieces on the bench on the port
and starboard sides of the skateboard and parallel and not so snugly so as
to prevent travel.  Tack them to the bench.  You now have a little
bobsledTunnel sortaThing for the skateboard to run back and forth within.
Attach the reaction vessel (a cylinder) to the skateboard by laying down on
it's side and duct taping it on.  Set the sawzall speed then use the
trigger lock.
(detachable hose config.)


The aerobic approach- Fasten a rope to the pressure vessel, hang it from
the ceiling, shake it back & forth by hand on the dangle...tiring, need
partner for shift work, not recommended.
(fixed or detachable hose config.)

The high dollar approach-  Buy a Parr shaker. For about three grand.  I
held onto one of these for an ex-partner/friend who took a mandatory
retirement in Folsum for 3 to 5...and had some occasion to try it out.
They're bullet proof, precision machined, over built.
  These are designed for mini-yield experimentation, not production.
  The model I'm familiar with had a meager 1L capacity yet weighed approx
200 lbs. and took up 42"x27" of floor space.  The bottle clamp was not
tweakable to greater capacity...the motor was NOT sparkless, the exhaust
valve seat was way too small and clogged with catalyst every single time.
Before returning it to the owner, I had to change all the  bolts from
carbon to stainless myself, after minimal acidic exposure rusted them out.
Totally unimpressed...not POPEYE approved.
(fixed hose config.)

POPEYE's bathtub Sailorman approach:
        I thought this one up myself, it is fairly intuitive so I'm sure
others have too.
        Buy a bunch of those suction cup rubber mats and stick them on the
sides and bottom of a bathtub.  Fill the tub.  After pressuring the
reaction vessel, detach the hose, orient the cylindrical vessel
horizontally, float it, then spin it, rocking end to end slightly.
        POPEYE recommends this method because if there are any leaks, they
are evident from bubbles in tub.
(detachable hose config.)


                    ~Standard hydrogenation methodology~

1. First combine ingredients of reaction mixture in safe container.
2. In a seperate beaker, carefully add dry catalyst, them moisten with a
non-reactive solvent, Hexane is common.
3. Introduce 1/3rd reaction mixture to catalyst 'paste', stir briskly,
quickly transfer to pressure vessel. Repeat. Repeat.  Pressure vessel
should never exceed 2/3rds full to allow for sloshAbout.
4. Seal pressure container, afix hydrogen feed line, and pressurize
container to 40psi.  Now realign valves and release the pressure into a
safe exhaust.  This is called 'purging',  and is done three times.
5. Now pressurize to 60psi, cut off H feed then shake (or spin)
6. Continuously monitor the pressure gauge and when the pressure within the
vessel falls below 20psi, repressurize to 60psi.  When uptake of hydrogen
ceases (after 3x's is average) reacton is finished.
7. Remove pressure vessel from shaker and orient in a vertical position,
let rest about 15 minutes, then slowly release pressure into safe
exhaust...it is not unusual for the contents of the container to aerosol
out with the gas resulting in loss of product and temper, for this reason,
POPEYE recommends you design a simple liquid trap (aspirator) which is
afixed along the exhaust line at this point.

   ->exhaust HOSE->->->->   ->->->exhaust
                         | |
                         v ^
                        _|_|_
                       \     /
                        \   /    <-two holed rubber stopper

                        GLASS
                        BOTTLE
                       G LA S S
                      B O T T L E
                     G  L  A  S  S
                     B  O T T L  E
                     G  L  A  S  S
                     B  O T T L  E
                     G  L  A  S  S
                     B  O T T L  E

Troubleshooting:

The hydrogen is not being taken up.
        Not using enough catalyst, check recipe.
        Catalyst is old or no good.
        Your recipe is no good or you've goofed the chemistry.
        Have you cut off hydrogen feed b-4 shaking as mentioned in step 5?
        Your psi gauge is malfunctioning or is fouled with catalyst.
        Line or valve is fouled with catalyst.

The hydrogen is endlessly being taken up.
        You have a leak!


                   Filtering Catalyst From Reaction Mixture

 Methanol is used as a solvent/carrier in this description...appropriate
substitution where necessary.
 Combine contents of aspirator and pressure container into a  glass vessel
which can be stoppered. Rinse containers with methanol and add.  The
holding vessel should then be filled to the top with methanol to purge the
air and prevent any wierd oxidation catastrophes, then stoppered.

 Let sit for halfAday until Pd/C settles out.  Carefully suction out the
reaction mixture without disturbing Pd/C sedimentation.  To increase yield,
refill container with methanol and repeat last step. Now, filter solution
until it is free of catalyst, adding more methanol to carry solution
through filtercake as necessary. Vaccuum or distill off Methanol leaving
product.
 Wash catalyst w/ distilled H2O and air dry for re-use.



                        *final disclaimer*
I am not 'in the business', I have grown weary of 'the business' and
worrying about the cops.  It is interesting to note that the existence of
one is very much dependent upon the health of the other.   You would do
good to avoid both. If you think about it, that is where the real value of
this Newsgroup lies.
  -Peace


                                -POPEYE


-----------------------------------------------------------------------------
Subject:      the holy hydrogenator

   Combine 100 gms L-ephedrine  and 890 mls. glacial Acetic Acid in a 5L
ehrlemeyer on a stir plate and begin stirring.  Slowly add 66.56mls
Sulphuric Acid at a rate which will keep the temperature below 71C. 
   In a pressure container, a paste is made up of 65 gms. Pd/C and enough
glacial acetic to moisten, the contents of the ehrlemeyer are then added.
The container is sealed and heat blanketed so that the temperature can be
held at 38C.
   The dieties are called upon,  the sacred valves are gently fondled, and
a  holy purge is brought about.  The vessel is annointed with the most
elemental of all gasses.  Now the sacramental hydrogenation ceremony is
carried forth. The straining of the catalyst shall follow and all that was
before, will be no longer, and in its place shall be born anew, and it is
good, and it is freebased, so that the primordial  elements and acids be
torn asunder that they shall be cast aside.  And the oil is extracted, and
the oil is acidified, and from the oil shall the pure white crystals
emerge.

   And it was done.  Yea, though it was done in ancient times, it did come
to pass.  And those who witnessed, were heard to say, "These are not the
promised  yields!" and doubt was cast even upon the virtue of the chosen
few crystals which came about amidst a gnashing of teeth, wringing of
hands and a great burning of the eyes.
   And lo, the time did pass, until one day, he who did cometh from the
sea, though he be not a fisher of Men, but a Half Blind Sailor, turned to
his brethren in the holy land of INTERNET and cried out, "Hear me, Ye
ministers of the Elements,  have my sins and faltering ways wrought these
fallow fields of hollow crystal, or was I led astray by false scripture
unto a fool's quest, wherein no man could but cast his ephedrine into the
sea and harvest only wind.
     What say Ye?...for I know not where to lay my faith, or place my
trust.  Is this a travesty of the cheministry, a fuming trial of Meth
oozala's children..or have I but mine ownself to blame for worshipping not
even at the high school alter of the organics and handling the Glass of
Ware not in the traditions of the elders, but like a tamer of scooters who
shuns his own somnabulistic ritual.

You may testify by E-Mail or before the flock.  

When you plant ice
You're gonna harvest
wind                                                                                                                                                                                                                                                                                                                                                                                     

           
                   -Half Blind Sailor  

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

Subject:      Home hydrogenation-precusors
Date:         1995/07/19

My anonymous Net Pal asked me to post this for information purposes only.
                                                           -oLIVEoIL

                        *standard disclaimer*
 It should be obvious that I am not a chemist. Merely a chemHacker
experienced in certain chemical processes/techniques.
 This describes illegal activity, this is posted cross-eyed and double
blind anonymous, I could be making this up, I have already been publicly
denounced, don't try this in Tupperware...  I have hereby disclaimed, you
have been warned....be careful in realTime, remember to keep your mouth
shut.
 All responses expounding ethical and/or moral pretences will be mutilated
for entertainment purposes and your addressing circulated amongst low-life
scooter-trash.

                          *disclaimer over*



 Whenever I've purchased supplies from commercial distributers, I forged a
Purchase Order (using a different boxy bold font for the PO number, so it
looks like automatic consecutive printing)  fake company (related to
purchase) fake address on a fictitious street, space for phone number left
blank (sorry not hookedUp yet).
 A PO facillitates filling the order and the lack of one is a red flag
indicating that you are not a business in the legitimate taxpaying sense.
Since we all have computers, formatting a PO is worth the trouble.
 Supplying a PO also helps you to tell the difference between clerks who
may need info just to fill out in-house paperwork for banal reasons, and
nosey, brainwashed, gung-ho, bootlicking, snitchPrick targetheads who will
invariably ask for verification or ID.  If the Bullshit on the PO ain't
good enough, fuck'em, walk out.  And while you're at it, tell them that  a
legitimate businessperson, such as yourself, has no interest in being
shitlisted with Jack-booted government thugs just because a bunch of slimy
dope fiends can't control themselves and everybody else refuses to mind
their own fucking business.  POPEYE never slinks out like a common
criminal.

 In the interest of bandwidth preservation, I will not belabor common sense
variables such as flagrant display of auto liscence plates, paying with
personal checks,  stomping in on DocMartins clad in raunchy crankOil
stinking leathers with your Jolly Roger headband and studded chain mail
riding gloves,  taking direct routes to/from suppliers and labs and/or
customers, selling 1/4 grams directly from a fully stocked lab out in the
garage of your family home, a virtually endless list of possible no-brainer
fumbles that will cost you everything.

Pd/C catalyst:
        Purchasing- I will leave it up to others to decide just how
"watched" we all are, but will say that I have purchased 100 gm bottles
Pd/C from chem supply houses without being asked to sign anything or
produce ID, that may have been the 90's, organic memory is partially
chemErased, could be different now,  call and ask, use a pay phone.

        Stealing/Bribing- Since POPEYE actually IS a common criminal,
behold: petroChem plants and many oil refineries use this in cracking
towers by the ton. It comes in bags like concrete in bulk.  Plants have
security against industrial sabotage and politico-terrorist corporate
paranoid delusional contingencies so it's best to hit railroad cars en
route (obviously while they are stopped somewhere) or bribe truck drivers
or plant workers to steal it for you.  Good product can be much more
persuasive than money, since these folks are well paid but overworked.


Hydrogen Gas:
        As mentioned this can be acquired at chem supply houses but I don't
know if you must sign for it or if they put little bugs or homing devices
or detonators in them,  or follow you home in a helicopter.
        A well stocked welding supply house.  It is used in specialized
welding, glass blowing, neon sign art, sci glass and any application that
requires a totally clean burn but not extreme temperature.  Whether you are
leasing a tank from the supplier, or purchasing one, you will be required
to register it.  This is a theft discouraging thing that all welding supply
houses engage in.  A letterhead may suffice.  POPEYE is a Biker and always
knows lots of welders, I had someone get one for me, on pay or barter, when
I was into this sort of thing.

         Stealing/bribing-too much trouble to steal, never steal something
you can't run with, huh?   Who me?  What hydrogen tank?


              Give Me Liberty
                    or
                Give Me Meth
                                        -POPEYE

