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Author: Subject: Madness to the extreme, nickel teracarbonyl
plante1999
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[*] posted on 4-5-2013 at 08:18
Madness to the extreme, nickel teracarbonyl


I dessided to try to make nickel tetracarbonyl today. I used a equimolar supply of CO2 and CO from sulphuric acid dehydratation of oxalic acid. the nickel was from 5 cent (canadian 99.9% Ni). I got something, but I'm not sure it is the desired compound, I think I may need to dissolve the nickel, pyrolise the nitrate to the oxide and use it as a source of nickel, finer nickel.

I had an hoose going very, very far away, and the experiment was done outside.








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[*] posted on 4-5-2013 at 08:55


Wow, very nice setup. But powdered Ni would be much better. Just be careful not to poison yourself. Or make iron pentacarbonyl instead.



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[*] posted on 4-5-2013 at 09:14


That's not going to work. You need a very pure carbon monoxide stream and freshly reduced nickel powder.
The carbon monoxide should be made from formic acid and sulfuric acid and dried. The nickel is produced by heating its oxide in a stream of hydrogen and the gas stream then switched to CO.
Nickel tetracarbonyl vapors produce an intensely luminescent flame when fed into the air intake of a bunsen burner with non-luminescent flame. That's the best way to detect its presence in a gas stream and simultaneously destroy the offgas from the synthesis.
And of course it deposits a nickel mirror when passed through a strongly heated glass tube.




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plante1999
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[*] posted on 4-5-2013 at 10:49


10g of freshly made Nickel oxide, ready for reduction. I will keep you all updated.


EDIT
I reduced the nickel oxide with large carbon piece with water vapor (to make water gas). It gave me a light gray powder, which I guess is nickel.



[Edited on 4-5-2013 by plante1999]




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[*] posted on 4-5-2013 at 13:35


Quote: Originally posted by plante1999  
I reduced the nickel oxide with large carbon piece with water vapor (to make water gas). It gave me a light gray powder, which I guess is nickel.



Explain that bit a little more?




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[*] posted on 4-5-2013 at 13:42


Well, the purer the nickel, the better. Careful, you don't want to get near nicker tetracarbonyl... take obvious precautions and burn off any flaw.



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plante1999
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[*] posted on 4-5-2013 at 14:04


Quote: Originally posted by blogfast25  
Quote: Originally posted by plante1999  
I reduced the nickel oxide with large carbon piece with water vapor (to make water gas). It gave me a light gray powder, which I guess is nickel.



Explain that bit a little more?


Well, nickel oxide, and quite large (one cm to two round pieces). Were heated to about 600 C in a tube, and water vapor passed over it. After cooling, the carbon pieces where sieved and the nickel put aside to make the carbonyl.




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[*] posted on 4-5-2013 at 20:02


Why not decompose the tetracarbonyl at 200*C and generate nickel crystals in a continuous process?

One quantity of CO, an amount of nickel in the 'warm' end (to generate 50*C to 130*C), and a hotter top end to decompose the carbonyl (to Ni and CO at 180*C+) in a cycle.

Also, this way, you can cease forming carbonyl at the 'warm' side, and continue decomposing it at the hot side, anbd then purge the device hot and release nothing but CO in a 'safe' way.

Basically, the Mond process. I have a to-do list including this.
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