Author Topic: Intermediate Studies on the Sub-Oz Birch  (Read 25041 times)

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  • Guest
Intermediate Studies on the Sub-Oz Birch
« on: November 03, 2004, 04:09:00 PM »
Note: The following is intended for those individuals who have totally familarized themselves with, and have taken appropriate mitigation measures from; the serious hazards
related to liquid ammonia.

Although not exhaustive in scope, personal protective equipment should include

1.  appropriate impermeable gloves with some insulative

2.  a face shield.

3.  Long sleeves, preferably under a vinyl covering.

4.  Engineering controls such as a fume hood, or strategically placed fans to keep vapors from the operator.

5.  One hand always on the delivery valve.


November 3, 2004
Intermediate Studies on the Sub-Oz Birch

With all due respect to Ms. Jadeness
and Mssr. Organicumness: ;)

and with unrecognized respect to the resources
from which I draw the following suggestions,
for I would never try it myself...

I proceed.

1.  Hook up the supply in such a way
as to draw from the liquid phase
and conduct it to a heavy walled flask
such as a vacuum suction filter flask
through a vinyl hose
and thence thru a  tube (thru a one hole stopper) 
whose end is about at the level
of how much you want to collect. .

The heavy walled flask
should have had a magnetic stir-bar dropped in it first:
or a couple of large glass marbles:
before adding cold smelly.

2.  hook up the suction fitting on the filter flask
to another vinyl hose long enough
to go through the handle of the plastic milk carton
or bleach container or similarly formed container
whose handle of molded plastic is hollow,
which you have arranged adjacent.

The plastic hollow handled throw- away container
should be filled with water or dilute HCl. 
The handle will hold and direct the tube appropriately
to the bottom of the container,
and you will have no worries about the weight slipping.

trust me, you do not want the weight slipping.

3.  Arranging your receiver for the smelly,
you will also provide for your subsequent usage
some gardening shears of the anvil type,
or other guaranteed quick
slice- through- the- really- dirt-cheap- vinyl- hose cutting device, (Linesmen's Dikes, wire clippers, etc..)
as otherwise the frozen no- longer- very- plastic- hose
 will comprise a removal problem associated with a hazard
 whose failure mode consequences
are unpleasant to contemplate,
let alone experience.  :(

This is called “Job Hazard Analysis..”

3.  As the collection of the smelly
approaches the level of the bottom of the tube,
splashing will be seen to eventuate,
even though you cannot see the level
because of the frost
which has rendered the container translucent.
(Or opaque, depending on local humidity..)

4.  at this juncture, turn off the supply valve,
wait 5 seconds, cut the fume control line
4 inches from the glass fitting it surrounds,
cut the delivery line 1 inch from the entry tube,
pick up your flask of smelly,
and convey it to your preferred location.

5.  At your next location
(which may be the same as your collection location)
you will now connect up your aspirator
to the vacuum fitting, to control fugitive emissions
to the non-detect level.

However, if you have added either your metal
or your reducible species to the flask
afore running in the smelly on top of it,
the fumes arising from adding the second one
will not be nearly as bad
as adding them both at this point.

In fact, for those who care to walk the bleeding edge,
sodium can be added (as described below)
to the prepared reducible species
(as described below)
just prior to collecting the smelly on top of both of them:
thus taking care of some large % of the fuming
at the collector point fume control device.

According to what I have heard,
this has been proven effective for sodium processes,
which does not assure that it will work
without over-reduction, with lithium.

6.  Replace the one-holed stopper, delivery tube,
and vinyl hose stub with a large plastic or glass funnel:
large hole preferred.

Also, assure that you have a 1" synthetic bristled
clean paint brush handy.

Obtain from your local supermarket
one of those cheese graters
used at snobbish upscale restaurants
by waiters who hold the device over your soup,
ask you if you want cheese,
and then who upon hearing a “yes”,
rotate the handle, causing the circular grater
to grate the cheese into your soup:
on your salad:
or in your lap. 
We’ll call this your “sodium grinder.” 
It’s use, hidden now I’m ever SO sure,
will be explicated following. 

Battery breakers are SOL: sorry. :(

7.  Reducible species preparation:
(the section following relates to Na metal:
Li metal effectiveness theoretically would be raised
by cognate salt, LiCl) {or other halogen-based salt..)

take your fake salt and estimate it’s volume.

Take 1/3 to 1/4 times it’s volume of straight table salt,
NaCl, and dry the hell out of it in your microwave.
(note: take a NaCl weight   = to the weight to your fake salt as the guidline,
since volume of the fake salt can vary significantly,
depending on preparation.. )
(Note: although there is little water complexed with NaCl,
about a 5 to 10% reduction in weight can be realized..)

Mix the hot dried NaCl  with your fake salt,
and regrind the hell out of it
in your coffee bean expresso 
super-whizzer grinder.

Any signs of any dampness whatsoever
should entail a re-visit of it all to the micro,
where you heat, stir, heat, stir,
until you see your first wisp of smoke,
which is a bit of fake going up in smoke,
likely because of an attached polyampholyte,
the nature of which is such
as to be very interceptive of microwave energy.

(This could be an opportunity to segue’
into how to clean GUP’s by cooking the poly’s:
but enough:
suffice it to say that the fine dry salt
confuses some amendments
which may still be present, raises your yields,
enhances extraction, and de-clumps your materiel...)

8.  OK: back to the program:
your funnel sits atop your flask:
your flask is cold and happy:
fumes are entrained in the side water
connected to the aspirator. 
You may have a blue metal solution:
or a whitish-clear solution
to which the previously described
fake salt and salt powder has been added..

And it may be circulating because of the mag stir,
or you may have to pick it up
and gently rotate the marbles
to assure that mixing is proceeding
in accord with your expectations..
(not so vigorously  as to coat the side
with reactants which will be out of reach
of the main process, however...)

You have placed your fake salt and salt fines
in a

<wait for it>

salt shaker:
preferably one of those with the flip-top
plastic sealer lid commonly associated with picnic baskets,
 and sex on a blankie ‘neath a large oak tree
in late spring,
after the grass is dry
and the ticks have already fallen off. 
(Nothing like a tick buried
in one of the cheeks of your butt,
unnoticed until after the festivities are concluded
and you go to scratch your butt
like you have a million times before and
!!!!!!SON of a BitCH!!!!!!..)

Anyway, enlarge the holes in the plastic a bit if you like:
 but if its truly dry it will run out like a liquid...

And, it won’t clump uselessly
presenting only it’s surface area for reaction.

As for the cheese grater
now used as a sodium grater,
the guy who discovered it’s efficacity in this endeavor
 should be regarded as a genius of his time,
comparable only to the guy who invented the
“vinyl hose thru the hollow handle” fume control. 
Wait: they are the same guy. 
OK OK I guess he’s in a class by himself.. 
::) demented ::)

The paintbrush is used
to shoo the crumbs of sodium or fake salt and salt
down the chute.

8. OI vey: <do you vey at the moon??>  
fait accompli:
everything is blue:
no additives left to add.

Quench?  If you feel the urge, don’t use water. 
Put in an ice cube.  Mo betah, safer.

 True sodium right-wing Birchers can add dry alcohol:
 may as well put the remaining metal to mop-up duty.
(This will not over reduce with Na:
but may with Li: be warned,
ye battery manglers..) :P

Also, alcohol, (dry, mixed, $8 gal)
 can be used to extend a reaction going dry:
up to around 20 to 25% alcohol
 will still retain solvated e-:
I think if the alkie is dry-ice cold
even a higher % may be used.

If you have some reactants glomming
 onto the side of the reaction vessel,
wash them down intothe mix with a squirt bottle
filled with the dry alcohol..

9.  Put the abandoned delivery one-hole stopper
and glass tube back in:
now the aspirator is sucking relatively warm air in
and directing it to the stuff you now want dried..

After it appears dry,
seal the glass delivery tube,
providing a further vacuum drying effect...

Once room temperature has invaded
the entirety of the flask,
you can proceed to your favorite extraction technique..

<burp> 8)
1.  First mod 4 Nov specifying salt
more accurately and adding safety warning.


  • Guest
eating,smoking, & nosing crap:
« Reply #1 on: November 12, 2004, 02:27:00 PM »
Here is a fine example of someone taking a good result,
extrapolating from it,
drawing conclusions,
and giving half-baked advice
whose effect would be destructive,
as regards the goal.

It was tempting to let this drift into the past without comment:
or ask Lugh to wipe it out:
‘twould be fine with me
if that was to happen,
I sure don’t want it in my legacy..
Oh well... :-[

Here’s 2 mistakes corrected:


as regards the NaCl:

if you have noticed incomplete reactions,
with unreduced material:

add somewhere around 10% NaCl in a Birch (Na) reaction,
or the same % (or so) of some salt of Li in that reducing system:
it will push things in the right direction next time.
(A web resource authority for this will be obtained if needed)

As regards using dry alcohol to “quench”:

if you are using a NP based separation system,
this will complicate your life
unless you evap to complete dryness
before accomplishing same:
alcohol will carry a lot of crap
into the NP,
and they when you gas,
you get  :P
Yum. >:(

Of course, if you distill-separate,
it ain’t no thang,
but it should be noted.

Now the net effect of combining two errors,
pushing the reaction to completion
with a HUGE and untried excess of NaCl:
plus quenching unreacted Na with alcohol??

And then unthinkingly doing a NP
without assuring it being all dry of alkie
afore time?

And then filtering and gassing?

you get
"PiecesofCrap. HCl"

I know of no market, local or distant,
for the chloride salt of  "PiecesofCrap."

If you know of one, please advise.

Oh well: the cheese grater is pimp..