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Author: Subject: high pressure and heat resistance beaker
ruxx
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[*] posted on 20-12-2012 at 13:02
high pressure and heat resistance beaker


wher can i find beaker/flask etc that can be sealed and withstand
heat and high pressure?
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Hexavalent
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[*] posted on 20-12-2012 at 13:10


How hot does it need to be, and what pressures does it need to hold?

What do you need such an item for? A Buchner flask would be an initial idea, depending on the details.




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blogfast25
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[*] posted on 20-12-2012 at 13:11


What's your purpose for this vessel?



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Vargouille
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[*] posted on 20-12-2012 at 14:46


I'll quote directly from Organometallic Syntheses, Volume I:

Quote:
Autoclaves made of stainless steel are indispensable in transition-metal organometallic chemistry for preparing metal carbonyl derivatives requiring the use of carbon monoxide under pressures sufficiently high to exclude use of Hoke bombs or Carius tubes. [...]

Stainless-steel Hoke bombs (Fig. 10) are particularly suitable for reactions requiring gases conveniently charged from a vacuum system. The Hoke bomb fittings are also readily adaptable for connection to a high-pressure system for introduction of carbon monoxide under pressure. However, it must be borne in mind that the maximum safe operating pressure of a Hoke bomb is around 100 atmospheres. This and the difficulty of stirring of shaking reactions mixtures in Hoke bombs make them less desirable than autoclaves for reactions with carbon monoxide under pressure. The use of Hoke bombs for simply carrying out reactions with liquids above their boiling points [...] should be pointed out. [...]

The final alternative for pressure reactions is a sealed thick-walled glass Carius tube (Fig. 11). The maximum safe working pressure for a Carius tube depends on the skill of the operator in sealing the tube but in any case it is less than that of a Hoke bomb. Explosions are therefore more frequent when using Carius tubes than when using Hoke bombs. [...] An obvious advantage of Carius tubes over Hoke bombs is the ability to observe the reaction mixture while the reaction is taking place.


As for where to find these contraptions, I can't say. A quick Google search with their names should give you more information. With "autoclave", you tend to get the more relevant results by specifying "chemical autoclave".
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kristofvagyok
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[*] posted on 20-12-2012 at 15:15


Carius tube rocks, the only problem is that it could explode if it is not properly sealed(:





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ruxx
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[*] posted on 20-12-2012 at 17:04


Quote: Originally posted by Hexavalent  
How hot does it need to be, and what pressures does it need to hold?

What do you need such an item for? A Buchner flask would be an initial idea, depending on the details.

its for the reaction i talk about in the "phosphorus from phosphoric acid" it has temperature of 540 °C .
dose the autoclave can withstand that? how i can cool down the materials inside after that?.
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kristofvagyok
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[*] posted on 20-12-2012 at 17:16


Forget it, autoclaves are expensive as hell and they are attacked by mineral acids at elevated temperatures.

Get a quartz tube and try it out.




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Poppy
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[*] posted on 20-12-2012 at 18:38


Sure a beaker free of any bubbles of defects would be best suitable, at least until it melts I'd think. A microscope should be proper enough for scanning micro bubbles that could cause cracks at high pressures.
Once you have a nicely built bunker you could put the steel pressure resistant vessel in, and be able close-open it from outisde, its then worth experimenting for sure!
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kavu
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[*] posted on 21-12-2012 at 00:24


Not that suitable in this particular case, but useful anyhow are the ace pressure tubes. I have been using these when preparing wittig salts. Just load with starting materials, screw the top on and clamp into an oil bath. http://www.sigmaaldrich.com/catalog/product/aldrich/Z181099u
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