plante1999
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unknow titanium compond
Long time ago ive made something that i dont know wath is it , when i made this , in all my document about titanium chemistery , none wrigh about
titanium carbonate so i tried to make the carbonateand it make this result, take note that i re-tried more and more to chec if it wasnt an error:
lab temp: 5degree C
First take an solution of TiCl3 and ad hydrogen peroxide to get the peroxo complex. Take the peroxo complex and ad sodium hydrogen carbonate to it
first it product carbon dioxide , after a certain amont of time a greenish gas that the odor corespond to chlorine is produce. Finaly a blue
precipitate of crystal is produce.
Blue precipitate proprety:
very vey hard, like zirconium metal.(mohs harness more than 7)
complety insolube in water and common solvan including chloroform and acetone.
1-can you explain wath this substance is?
2-If anyone have the material can you try to make it please , for comparing with my experiment.
thanks!!
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blogfast25
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Yes, that is strange. I might want to try and reproduce that.
At first the chorine would seem to point to this: assuming there was small excess of H2O2 left in the solution and that on alkalising this oxidised
some Cl- to Cl2:
2Cl-Cl2(g) + 2e ….. E = - 1.36 V (oxidation)
H2O2 + 2H+ + 2e 2H2O ….. E = + 1.78 V (reduction)
Cell pot. = Ered + Eox = - 1.36 + 1.78 > 0
(Source: http://web.archive.org/web/20070518092613/http://www.northla...)
But note that the reduction of H2O2 calls for acid conditions and your conditions are alkaline. Still, it seems the only way to explain the chlorine
evolution.
The blue colour does seem to point to Ti [+III], not Ti [+IV] but how did you get from the Ti[+IV] peroxo complex to Ti[+III]???
You claim the blue product is ‘hard like zirconium metal’: how did you verify this?
Whether or not this could be a Ti[III] carbonate (or bicarbonate, or a basic carbonate - Ti(OH)CO3) depends on the relative solubilities: in a sodium
carbonate solution there’s plenty OH-, beside CO3 (2-). If the solubility product of the ‘Ti carbonate’ is lower than the solubility product of
the oxide/hydroxide, then the carbonate will generally precipitate. That’s the case for Fe2+ (FeCO3) and Mn2+ (MnCO3). But in the case of Al, no
carbonate precipitates, only plain old hydrated alumina…
I’ll check this out myself…
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plante1999
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remenber i have on my hand zirconium metal....
if it is a carbonate , it is very hard and crystaline , not like other carbonate , and it is blue!!
also peroxo ligant temb to be stable with titanium , it is why i use the peroxo complex.
also im sur that it doesn disolve in acidic condition! this matter makes me think of a polymer...... this mater is wird.
[Edited on 7-4-2011 by plante1999]
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blogfast25
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Nope, I didn’t manage to replicate your result.
I dissolved a small amount of thermite Ti into strong, hot HCl and then cooled and filtered the solution:
About 6 or 7 drops of H2O2 9% were then added drop by drop from a plastic drop pipette: the solution first cleared up (oxidation of Ti [+III] to Ti
[+IV]), then takes on that typical red-amber colour of the Ti [+IV] peroxo complex (as per usual):
To this solution was then added drop wise saturated Na2CO3 solution. I checked for Cl2 but didn’t find any. As I added more and more soda and got
closer and closer to the point where all the HCl was neutralised I noticed a white precipitate formimg which then, right up to the very end,
redissolved in the remaining acid reserve. Here’s the end situation:
Middle: fully neutralised solution. All red-amber gone and quite a bit of white precipitate, presumably fresh TiO(OH)2, formed.
Right: a bit of the middle suspension was transferred to that test tube and strong HCl was added. The precipitate dissolves and the
amber colour is restored.
Left: this is sort of half way through the neutralisation: bubbles of CO2 can be seen.
Plante, you’ll have to try and replicate this yourself, with photos.
I might want to try again with NaHCO3 but I can’t see this make any difference…
[Edited on 7-4-2011 by blogfast25]
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Mumbles
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I agree that the color points to an oxidation state less than +4. I've been trying to look into various titanium oxychlorides, or chloride hydroxide
complexes, but can't find any sort of color. I've seen references to TiOCl2, but it clearly mentions a colorless solution, something not consistent
with the compound. If it is Ti +4, it is going to need some pretty strongly donating ligands.
Is this hard blue solid something that you have been able to repeat?
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hyperkinetic
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What about a Ti compound which is Cl free? Some species of HTiO are apparently blue, insoluble and crystalline.
http://www.springerlink.com/content/115707386071rl71/
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plante1999
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from wath i read from this document , it seem to have same proprety , i will try to reflux TiCl3 with urea to see if my product is the same as i
already have.
thanks!
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hyperkinetic
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Any updates?
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plante1999
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not at this time , i need to buy 50gram of 99.99% Titanium piece....
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hyperkinetic
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Sounds good, in the mean time was the original TiCl3 produced from Titanium metal or titanium oxide? Any idea of the purity of the starting Ti source?
Do you still have the crystals? It would be a shame if they were the result of an unidentified impurity and were unable to form without it. What a
neat sounding compound.
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