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TheNaKLaB
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[*] posted on 27-10-2011 at 16:57
Nickel and Titanium complexes


I have some Nickel and Titanium metal that I recently bought. Both are 99.9% purity.

I was wondering if I can make some easy complexes with these metals? if any?

eg. Reacting Titanium or Nickel salts with an organic compound.

[Edited on 19-09-2011 by TheNaKLaB]




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[*] posted on 27-10-2011 at 17:00


Please use available search engines or a library before posting.

Titanocene and Nickelocene are two examples of Ti and Ni organometallics which would show up in a simple Google search. It's hard <em>not</em> to find published synthesis of these and more. Please put a little effort in yourself before asking to be spoon fed.

[Edited on 10/28/11 by bfesser]




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TheNaKLaB
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[*] posted on 27-10-2011 at 17:59


I have actually been looking for some 'easy' ones for a while. I can't seem to find any..
What I mean by easy is 'easy to synthesize'. Would you have any ideas?

[Edited on 19-09-2011 by TheNaKLaB]




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[*] posted on 27-10-2011 at 20:03


ammonia sometimes forms complexes with metal solutions (Nickel II Chloride + Ammonia = [Ni(NH<sub>3</sub>;)<sub>6</sub>]Cl<sub>2</sub>



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TheNaKLaB
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[*] posted on 27-10-2011 at 22:03


Yeah that could work. I think I might try that and film it for a video. I've been looking for some Titanium complexes, still yet to find some..



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[*] posted on 28-10-2011 at 03:47


Quote: Originally posted by TheNaKLaB  
Yeah that could work. I think I might try that and film it for a video. I've been looking for some Titanium complexes, still yet to find some..


Titanium most famously forms a Ti (IV) peroxo complex, deep red in colour. Search for it here at SM. Or at woelen's place.

Dissolve some titanium in strong HCl (it dissolves slowly but noticeably in it - faster at BP), that gives you a blue/purple TiCl3 (Ti [+III]) solution. Add peroxide solution (strength of no great importance). Bob's your complex.

It also forms (NH4)3TiF6 (Ti [+III]) but that's much harder to make.




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TheNaKLaB
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[*] posted on 28-10-2011 at 17:57


I like the sound of the Ti (IV) peroxo complex. I might try and make some. A few questions about the Titanium complex, would crystals (if any) precipitate out? And what would be the chemical formula for the complex. Thank you for your help!



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[*] posted on 28-10-2011 at 18:58


Test them to see if either forms a complex with 2-acetoxybenzoate.



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[*] posted on 29-10-2011 at 09:28


Quote: Originally posted by TheNaKLaB  
I like the sound of the Ti (IV) peroxo complex. I might try and make some. A few questions about the Titanium complex, would crystals (if any) precipitate out? And what would be the chemical formula for the complex. Thank you for your help!


http://woelen.homescience.net/science/chem/exps/titanium/ind...

Whether it can be obtained as a solid I don't know...




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TheNaKLaB
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[*] posted on 29-10-2011 at 15:02


I read up on it, would the formula be [Ti(O2)(OH)]2Cl2 you think?



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[*] posted on 30-10-2011 at 03:51


Yes.



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[*] posted on 30-10-2011 at 08:46


Hi,

Titanium forms some remarkable complexes. I don't know what reagants you have but here is a list of some complexes I have made over the years:

Starting material was Ti powder dissolved in 20% HCl (Left for about two days to form deep red-purple Ti 3+ chloro species) then diluted.

Potassium Ferrocyanide: Heavy deep amber precipitate.
Potassium Ferricyanide: Heavy pea-green precipitate.
Potassium Thiocyanate: Intense clear, purple complex.
Sodium Nitrite: Colour fades to clear as nitrite probably oxidizes the Ti3+.
Catechol: Bright orange and clear, turns hazy.
Dimethylglyoxime: Black then white then salmon pink!
L-Cysteine: Pale tan precipitate
Oxalate: Deep orange-red and clear
Ammonium Pyrrolidine Dithiocarbamate: Tan-orange precipitate.
EDTA: Intense violet and clear.
Glycine: Olive green, clear liquid.
8-Hydroxyquinoline: Green precipitate.

If you add some sodium hydroxide to the catechol complex then the orange colour turns green from the top down as aeriel oxidation sets in!

The 8HQ complex dissolves in acid to give a lemon yellow complex!

I was really surprised how colourful this element could be.



[Edited on 30-10-2011 by strontiumred]
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[*] posted on 30-10-2011 at 11:28


Strontiumred, may I ask how you prepare the dmg,8-hydroxoquinoline and EDTA solutions? As I understand, only the protonated species create the complexes.

[Edited on 30-10-2011 by Mixell]

[Edited on 30-10-2011 by Mixell]
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[*] posted on 31-10-2011 at 06:17


Hi Mixell,

The dmg was dissolved in 3% sodium hydroxide to form a pale yellow liquid - It hardly dissolves in neutral conditions. Wikipedia says that it is the conjugate base, not dmgH2 itself, that forms the complexes - So I deprotonated it with hydroxide.

The EDTA was the tetra sodium salt just dissolved in water.

The 8hq was dissolved in 2% sodium hydroxide. When the initial green pct was later acidified it produced a yellow complex. Looking at some of my other results with this ligand complexes were only produced with added acid, Cobalt II is a good example. Alkaline produced a yellow preciptate, adding sulfuric acid caused a clear orange-red complex to form.

I'll probably revisit some of these and look at varying the pH.

(My initial Ti solution contained quite some HCl don't forget).



[Edited on 31-10-2011 by strontiumred]
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[*] posted on 31-10-2011 at 07:07


Did the amount of the hydroxide solution was according to the molar amount of the dmg (1 mole of hydroxide for every mole of dmg, so that the dmg2H2- (2 units of dmgH-) macro-cyclic ligand will form.
The above question also applies for 8hq.
I only have the disodium salt, so I'll just add it to a molar equivalent of sodium hydroxide solution. What was the molar concentration of the solution of your tetrasodium EDTA?

Also, I plan to make a nice amount of those solutions and keep them for further experimenting, do you know if they degrade? Or they are stable in solution?
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[*] posted on 31-10-2011 at 09:01


Looking at my notes there there was a slight excess of alkali used. The molarity of the EDTA was 0.11.

I've always made the solutions when needed so I'm afraid I don't know about their stability over time.



[Edited on 31-10-2011 by strontiumred]
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