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Author: Subject: Lab scale industrial processes
lolcat
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[*] posted on 6-12-2012 at 16:25


I am a bit confused about the combustion tube. Is there a flame in direct contact with the material being combusted, like is there a hole in the combustion tube? Or does the flame just heat up the glass? Which doesn't really make sense, because then how would it combust.

plante1999, do you remember where you bought your borosillicate combustion tube? I found one at, http://www.perkinelmer.com/Catalog/Product/ID/N2411300 , but it seems rather expensive.

Also, in your Bibliography, you mention Ullmann, F. Ullmann’s Encyclopedia of industrial chemistry, 5th ed.; John Wiley & Sons, 1999, I was curious as to how you had access to this source.

[Edited on 7-12-2012 by lolcat]
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[*] posted on 7-12-2012 at 02:15


The flame just heats up the glass. It combusts because there is an external air stream done up with glass tubing. But it is an interesting point, because I had brought up earlier that I wasn't sure if combustion was necessary, as I recalled an anecdote where mercury was freed from cinnabar simply by heating, leading sulfur in the vessel.
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plante1999
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[*] posted on 7-12-2012 at 03:46


The cinnabar need external heating to combust in air, without air it will only sublime.

For the tube I simply bought a 18mm by 150 borosilicate test tube and I cut the bottom to get a really cheap tube.

Well, I have "some" book in the PDF format...




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[*] posted on 7-12-2012 at 11:26


The cinnabar will sublime? As far as I am aware, cinnabar does not sublime to any considerable extent, only convert to the black mercury sulfide at around 344C, which melts at 850C. At least, that's what the CRC says, and it does not mention any sublimation. Incidentally, this casts aspersions on my recollection that cinnabar forms mercury and sulfur when heated in absence of air. Perhaps I'm losing my memory prematurely.
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[*] posted on 7-12-2012 at 12:16


plante1999 - If you have any pdf's from Ullmanns Encyclopedia of Industrial Chemistry that cover the extraction of mercury from cinnabar, I would be very grateful if you could post it, I would like to read up some more on the whole process.
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[*] posted on 7-12-2012 at 14:24


Quote: Originally posted by lolcat  
plante1999 - If you have any pdf's from Ullmanns Encyclopedia of Industrial Chemistry that cover the extraction of mercury from cinnabar, I would be very grateful if you could post it, I would like to read up some more on the whole process.

Here is the chapter on mercury from Ullmann's, extracted from the whole book kindly provided by solo in the References section.

Attachment: Mercury - Ullmanns Encyclopedia of Industrial Chemistry p. 781-812.pdf (262kB)
This file has been downloaded 2468 times





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[*] posted on 7-12-2012 at 15:42


Oh! thanks, I didn't know that Ullmanns Encyclopedia was in the resource section, I guess I will need to ask for permission to that forum.
A few questions on plante1999's diagram.
What is the reason for the air pump going through an empty glass bottle before entering the combustion chamber. My only thought is that this might prevent unwanted back flow into the pump itself.
Why is the glass bottle that is directly connected to the combustion chamber in an HCL ice bath, I understand why it is in an ice bath, but why a hydrochloric acid ice bath?
Could a Liebig condenser be attached directly to the combustion tube, and cold water run through the condenser, instead of the glass bottle acting as the condenser? The mercury would still fall into a glass flask and glass tubing would carry away the SO2 to the next bottle.
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plante1999
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[*] posted on 7-12-2012 at 17:28


You got it wrigth for the first bottle. The ice/HCl bath cool down to minus 30 degree celcius instead of 0 for normal ice bath, you can use CaCl2 too. A liebig condenser would be hard to clean up, the dirty mercury contain mercury ashs. Mercury ashes is cinnabar dust with 60% + elemental mercury in it. This ash would restrict the mercury flow. This ash can be distilled to get the mercury out of it.

What cinnabar will you use?

If you have any questions, please ask.

[Edited on 8-12-2012 by plante1999]




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[*] posted on 7-12-2012 at 17:48


http://cgi.ebay.com/ws/eBayISAPI.dll?ViewItem&item=20033...

That makes sense as why not to use the liebig condenser.
2 questions concerning the HCL/ice bath. Will the ice/HCl bath actually go below zero, to minus 30 degrees as you say?

And why would you want it that cold if that is the case? Sulfur dioxide condenses at -10 degrees and mercury condenses at 356 degrees. So wouldn't there be a fear of the SO2 condensing as well?
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plante1999
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[*] posted on 7-12-2012 at 18:02


I didn't saw sulphur dioxide problem, because the gas are extremely hot. Because gas are extremely hot, extremely low cooling is needed to get room temp. in the chamber.

That's good cinnabar.




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[*] posted on 7-12-2012 at 20:58


Attached is a rough draft of the procedure I will follow, pretty much an adaptation of your plate1999's work. The Erlenmeyer Flasks in the picture are 125 mL each. Its not in the picture, but I think I might place the last glass tube into a beaker of water, to see if any SO2 is leaving the sodium carbonate beaker. Any comments will be appreciated.

Attachment: Mercury from Cinnabar1.pdf (372kB)
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[*] posted on 8-12-2012 at 14:14


It should go alright. But for heating, like I said, you may need something stronger. Time to time I used a propane torch to get to the wright temperature. You may see blue flame in the tube if you heat enough.

Good luck.




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[*] posted on 15-1-2013 at 19:32


Look at what I just found:

http://ebookbrowse.com/lab-scale-industrial-process-for-chem...

And I didn't put it there, it seams my pdf are shared without any reference to my website! I'm glad I put a link on the top of the first page!

Any thoughts on this?




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[*] posted on 16-1-2013 at 01:28


Well, link's broken, so it's not a problem.

On topic, it is an odd thing to happen. From what I gather, someone who saw your pdf linked it to e-Book Browse. I can't really think of an innocuous reason to do so, considering that the downloads on your site are free.
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[*] posted on 17-1-2013 at 04:57


Yea, thats what I wanted to show, there is many link to my PDF on other page than my website.
I guess there is sort of reward for people who put PDF...




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[*] posted on 17-1-2013 at 04:57


Yea, thats what I wanted to show, there is many link to my PDF on other page than my website.
I guess there is sort of reward for people who put PDF...




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