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Author: Subject: Titanium Tetra-chloride Bottling
ger.wat
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[*] posted on 25-1-2018 at 10:50
Titanium Tetra-chloride Bottling


My employer used to make a device for testing air movement that used Titanium Tetra-chloride in 10ml snap top vials with a long narrow neck for hermetic sealing. 20 yrs ago we were able to get it easily and it became harder as time went on. The guy that did the job at our original supplier retired and we were never able to find anyone else that would do it more than once. I did it myself a few times and stopping fumes long enough to melt the glass on the end of the neck was always very difficult.

FYI: TiCl4 is Titanium dissolved in pure hydrochloric acid. It reacts with humidity to make beautiful dense white "smoke." When trying to seal vials, the titanium in the fumes contaminates the glass surface so the melted glass won't stick to itself.

So here's my question: how do I stop the fuming while still being able to hermetically seal the neck of the vial? Ideas?

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PirateDocBrown
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[*] posted on 25-1-2018 at 16:24


Stick in a small tube with an argon bleed to purge the air inside the ampoule. Heat the ampoule neck till it's soft enough to crimp. Pull out the argon line, then crimp.

Alternatively, melt the neck electrically, inside an inert gas dry box.




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[*] posted on 26-1-2018 at 04:49


Freeze the sample in the ampoule using a dry ice-acetone bath, vac/purge the headspace with argon, then seal as normal (whilst still being cooled in the bath)
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[*] posted on 26-1-2018 at 09:49


These guys seem to sell a refill kit of the Titanium tetrachloride ampoules-

http://www.airflowdirection.com/smokeproducts.htm

Unless that's YOUR company and stock is depleted?:P



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[Edited on 26-1-2018 by Bert]




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[*] posted on 26-1-2018 at 11:02


Quote: Originally posted by ger.wat  

FYI: TiCl4 is Titanium dissolved in pure hydrochloric acid.

No it isn't.
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[*] posted on 26-1-2018 at 13:56


That would form TiCl3, which doesn't fume.



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Nicodem
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27-1-2018 at 10:48
ger.wat
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[*] posted on 29-1-2018 at 16:03


Fine, Titanium dissolved in Chlorine then. Nevertheless it forms HCl when it reacts with water.

I am familiar with airflowdirection.com. Our works similar, more of a Cadillac version.

Thanks for the ideas, I can make this work.
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[*] posted on 29-1-2018 at 21:59


Hydrochloric acid AND Titanium dioxide are formed, the wonderful stuff that helps makes your white paint opaque.

Between the acid condensing droplets of water and the very fine solid TiO2, it makes a wonderfully opaque fog for the weight required. As I recall, it even screws up infrared imaging to some extent. Need to check my references from Pyrotechnics on smoke again, most of my uses require REDUCING smoke, not enhancing.




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2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.

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