Author Topic: Nitro route using ultra thick foil  (Read 2322 times)

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lab_bitch

  • Guest
Re: When it comes to Al/Hg Os' is da man.
« Reply #20 on: October 07, 2002, 06:08:00 AM »

When it comes to Al/Hg Os' is da man. This Bee knows Jack 'bout the nitro variation, but I had thought of a variation to Os's variation which involved pie tins cut into long strips then bent into W or even M shapes. They would be evenly spread in the flask/PP garden sprayer (hint) and so stirring may not be needed (stuff fizzes). An excess of Al would not harm the outcome because it won't all be reduced to Al oxide. And 'cause stirring may not be ness. this could be done in a sealed system (pressure). What do you think?




The purpose of stirring is not to evenly distribute the foil, but to increase the Reynolds Number, thus increasing the mass transfer coefficient of the reactants to the metal surface, thus increasing the rate of reaction, thus increasing yields. ;)   This probably makes no sense to anyone who is not an engineer, but trust me on this one.  Basically, stirring increases the rate that the reactants can diffuse to the metal surface.


lab_bitch

  • Guest
Re: And while you guys fire up your 20 L flasks ...
« Reply #21 on: October 07, 2002, 06:12:00 AM »

And while you guys fire up your 20 L flasks to process a mole of ketone, true believers in the way of Os do that reaction in a 2L flask, and don't care if it runs a overnight or even a whole day.




I got a better one:
ketone + MeAm + Pd/C + KHCOO
Catalytic Transfer Hydrogenation
Aluminum not required


Diggity

  • Guest
I have pulled my hair out..
« Reply #22 on: October 07, 2002, 06:18:00 AM »
litterally, trying to get this fuckin rxn down pat. It appears, one really needs to spend 24 hours amalgamating the sheet.. every hour, manually swirling the flask.. every 6 hours, pouring off the meoh/hg, adding more.. rinse, lather, repeat!!!

ARG!! I refuse to fill a 5L flask with little squares of metal and fuck a flask up. However, he will gladly do it with a 2L flask. Have yet to try as he is letting the AL amalgamte for 2 days now.. no rush, just experimenting with 27g, at MM's scale using nitro.

It's really a bitch to remove all the al203! Even went to the extreeme of using 400mg of hg per wash,  to speed up the process. Last time it was checked up on, 90% of the al had turned dull.. but some shine was still visual.  :(  

Os, how long does it take normally to remove this layer?! Swim is using AL Flange.. maybe thats the problem.. should he just use a fuckin coke can?! This is all so frustrating.. and is really causing serious health problems with his hands. I feel like arthritis is setting in from balling up foil. [pain]

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.   
 

Osmium

  • Guest
> It appears, one really needs to spend 24 ...
« Reply #23 on: October 07, 2002, 11:34:00 AM »
> It appears, one really needs to spend 24 hours
> amalgamating the sheet.. every hour, manually swirling
> the flask.. every 6 hours, pouring off the meoh/hg,
> adding more.. rinse, lather, repeat!!!

WTF are you doing there again Diggity? Why make it any more complicated than it is?
Cover the Al with  alcohol, add some HgCl2, wait for 30 mins while swirling the flask occasionally or stirring it and you're done!
No need to wash and keep adding more HgCl2. Once these 30 mins are over add the other reagents and that's it.

> Last time it was checked up on, 90% of the al had turned
> dull.. but some shine was still visual.

What do you think an amalgamated Al surface looks like?
shiny and silvery...DOH!


I'm not fat just horizontally disproportionate.

Diggity

  • Guest
Im starting to think the "flange" isn't the right
« Reply #24 on: October 07, 2002, 11:51:00 AM »
Im starting to think the "flange" isn't the right type then. Theres no way it would of taken 30 minutes. At first it was stirred every 5 minutes or so.. swirled around manually. Maybe using dh2o instead of solvent to amalgamate? Maybe find another source of Al also..

Pop cans sound more usable. And from what Ive read many people seem to have issues with this Al Flange. Maybe thats the problem..

What do you think an amalgamated Al surface looks like?

Dull? Dull grey?

[edit] Shiny?! WHat? I thought it would be the same as foil.. kinda greyish blue.. dull. The shiny layer is the al203? no?

& I'm, somethin of a phenom, no need for da cron, I'm un-stopable.