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Author: Subject: TiCL3 made at home?
watson.fawkes
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[*] posted on 9-3-2011 at 12:44


Quote: Originally posted by Elawr  
What otc sources exist for titanium metal?
My motto: always check to see if McMaster-Carr carries it.
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UnintentionalChaos
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[*] posted on 9-3-2011 at 12:52


Quote: Originally posted by Elawr  
What otc sources exist for titanium metal?


Well, aside from buying turnings for pyro from pyro suppliers or ebay, go here: http://theringlord.com

Left bar, click specials. Then click "strip and disc specials" scroll down and find titanium discs or titanium scrap strip. It's CP grade 1. The discs are $25/lb, the strip is $16/lb and would probably make a good, cheap support for chlorate electrodes




Department of Redundancy Department - Now with paperwork!

'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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[*] posted on 10-3-2011 at 06:55


dang it all plante1999 is your life all about titanium? just joking! i thought i had titanium because i have a titanium camping pot and it turns out that it is probably just coated with titanium.its light as a feather so the base metal is also light, whatever it is.im gonna dissolve it in hcl acid and try to get a hydroxide.what do you get if you use titanium as an anode in a hydrochloric acid solution or sulfiric? i would of thought chlorotitanic acid and ticl3 to be the same thing.you got a bunch of cool colors.the eck-cuashun of titanic love!cool accent.:D
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[*] posted on 10-3-2011 at 08:26


Quote: Originally posted by cyanureeves  
i thought i had titanium because i have a titanium camping pot and it turns out that it is probably just coated with titanium.its light as a feather so the base metal is also light, whatever it is.im gonna dissolve it in hcl acid and try to get a hydroxide.what do you get if you use titanium as an anode in a hydrochloric acid solution or sulfiric? i would of thought chlorotitanic acid and ticl3 to be the same thing.you got a bunch of cool colors.the eck-cuashun of titanic love!cool accent.:D


Remember that titanium isn’t particularly light: its density is in fact about the same as that of steel (roughly speaking). But for ductile Ti the ratio of elastic modulus to density is much higher than for steel, better even than Al (off the top of my head). Unless your camping pot is particularly light because it’s particularly thin walled it’s likely to be plain ole’ aluminium…

Again off the top off my head, if is Ti, you’ll probably get plain old TiO2 with your proposed dissolution but don't quote me on that. Dissolving Ti in boiling conc. HCl works (and gives TiCl3) but is a work of patience!

'Titanium' is now also a misleading term that has entered the lexicon of greedy ad men...



[Edited on 10-3-2011 by blogfast25]
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[*] posted on 10-3-2011 at 10:12


ah, i see! titanium is lighter because less can be used to match the strength of steel, like a bantam weight packing as big a punch as a heavy weight.i filed the titanium to get to the base metal quicker by electrolyzing and it still bubbles for just a bit in sulfuric acid/water solution and then stops. the anode looks like brass when i take it out.the titanium in hcl acid is now grey and the acid is purple. i guess the color will stay purple even if the base is dissolved and i wont know how much titanium i got until i drop the hydroxide.the metal still looks intact and is turning out to be the metal from hell that would'nt dissolve.good thing i only took off one handle and it's ear.
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[*] posted on 10-3-2011 at 10:15


Quote: Originally posted by cyanureeves  
dang it all plante1999 is your life all about titanium?

cool accent.:D


1: almost,(including zirconium) is my life but i need 5% of my head for my vital function.I already try to get at 2% but I forget to breathe.

2-thanks!


and for your camping pot , the multinational like said: it is made in titanium because people thing: wow it must be really rare and good. (but in reality often only a layer of titanium is present), how many times I have understand titanium drill .. I think .. ........(someone thing he ave a titanium drill but he have a micro layer of titanium nitride).


[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]




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[*] posted on 10-3-2011 at 12:42


Quote: Originally posted by cyanureeves  
ah, i see! titanium is lighter because less can be used to match the strength of steel, like a bantam weight packing as big a punch as a heavy weight.i filed the titanium to get to the base metal quicker by electrolyzing and it still bubbles for just a bit in sulfuric acid/water solution and then stops. the anode looks like brass when i take it out.the titanium in hcl acid is now grey and the acid is purple. i guess the color will stay purple even if the base is dissolved and i wont know how much titanium i got until i drop the hydroxide.the metal still looks intact and is turning out to be the metal from hell that would'nt dissolve.good thing i only took off one handle and it's ear.


The purple sure as hell points to Ti3+. For a conclusive test, take a sample and add some peroxide to it. A red peroxo Ti [+IV] complex is formed when Ti3+ is pesent. This is considered a positive and conclusive test for Ti.
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[*] posted on 10-3-2011 at 12:45


Quote: Originally posted by plante1999  
someone thing he ave a titanium drill but he have a macro layer of titanium nitride).


[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]


He means MICRO, not macro. A layer a few molecules thick only... The thinness of the layer causes the 'rainbow efect' through thin layes diffraction...


[Edited on 10-3-2011 by blogfast25]
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[*] posted on 10-3-2011 at 15:02


red?cool! the people at snow peak camping gear e-mailed and assured me that the trek 900 cookset is made of pure titanium. the can is about 5 by 5 inches and weighs under 4 oz. it turns the anode blue in sulfuric acid solution ending in all the rainbow colors as it nears the connection,but i do see a rainbow color where i burned the pot.titanium seems to want to go on and on just making bubbles with s.steel.goodness that piece of metal is still going in boiling hydrochloric acid and even a drop produced a bit precipitate with ammonia.
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[*] posted on 10-3-2011 at 15:48


nice to understand, in a futur video i will show how to make pur sulution of H2TiCl6,or H2TiF6 a way you could use :

first get titanium piece.
than disolve man exxess of titanium in 9% hydrochloric acid with refux ((very long) or in 9% hydrofluoric acid:very dangerous:If you arent a experienced chemist dont do that)


you could make it safely from this way(take all safety gear): take a 100ml steel paint can with a steel or copper tube as condencer witch will go in a 120 ml hdpe bottle. take 21g of NaF with 60g of NaHSO4(an exess is better) and disolve it in 60ml of water outside in the steel can, pour 40ml of water in the hdpe bottle (make sur that the condenser go in the water) and make and snow/HCl bath for the bottle.Than distill the solution of NaF in the steel retort(like if you distil HCl ). go away from the set up . after that take the hdpe bottle and you have arround 8-10%HF solution.


when you ave your TiCl3 or fluoro complex you can fallow this guide from:
1=TiCl3
2=fluoro complex



1-1 take the TiCl3 and ad very large ammount of ammonia , filter the hydroxide it dont affect the finnal product if it disproportionate to hydrous titanium dioxide , it will just be more long to react.

1-2take the fluoro complex and ad very large ammount of ammonia , filter the hydroxide it dont affect the finnal product if it disproportionate to hydrous titanium dioxide , it will just be more long to react.



2-1ad the minimum amount you can of 9% HCl to the hydroxide a pale clear yelow solution will form.

2-2ad the minimum amount you can of 9% HF to the hydroxide a clear solution will form.



why all the time i sayd to use 9% is because i find it react more readily than other conssentration. for your camping pot you will probably need to cut it in piece (very difficult). also you can make very conssentred solution by boiling it to 1/4 of is volume.

with this 2 solution you can make almost all compound of titanium.

[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]




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[*] posted on 10-3-2011 at 17:17


Geesh i hope you did'nt think i got that Ti3+ with electrodes because i didn't try the hcl acid/titanium by electrolyzing i just boiled the titanium in hcl acid.now the purpleish bits that precipitate with ammonia is the hydroxide and turns to the white stuff(o2).what is Ti(OH)2 ? the hydroxide does'nt last very long does it? i found that plating titanium cannot be done but a lost russian book claims it can with Ti(OH)2.who knows? there might be a secret.
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[*] posted on 10-3-2011 at 18:16


Quote: Originally posted by plante1999  
i already do a video on this here (titanium hydroxide witch will disproportionate to hydrous tio2).

here with ticl3 and instruction.

<iframe sandbox title="YouTube video player" width="480" height="390" src="http://www.youtube.com/embed/tzD0_J03KpM" frameborder="0" allowfullscreen></iframe>





you sould read this , and understand the video. the formula is Ti(OH)2O.it will disproportionate to TiO2 nH2O witch is white.

and nice for your 100th post

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]




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[*] posted on 11-3-2011 at 07:49


Quote: Originally posted by cyanureeves  
Geesh i hope you did'nt think i got that Ti3+ with electrodes because i didn't try the hcl acid/titanium by electrolyzing i just boiled the titanium in hcl acid.now the purpleish bits that precipitate with ammonia is the hydroxide and turns to the white stuff(o2).what is Ti(OH)2 ? the hydroxide does'nt last very long does it? i found that plating titanium cannot be done but a lost russian book claims it can with Ti(OH)2.who knows? there might be a secret.


Ammonia precipitates Ti2O3.nH2O (black, basically) from a TiCl3 solution. But that hydroxide is oxidised to TiO2 even with water (it reduces water - LOL). It cannot be isolated as Ti2O3.
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[*] posted on 11-3-2011 at 07:54


Quote: Originally posted by plante1999  
nice to understand, in a futur video i will show how to make pur sulution of H2TiCl6,or H2TiF6 a way you could use :

first get titanium piece.
than disolve man exxess of titanium in 9% hydrochloric acid with refux ((very long) or in 9% hydrofluoric acid:very dangerous:If you arent a experienced chemist dont do that)


you could make it safely from this way(take all safety gear): take a 100ml steel paint can with a steel or copper tube as condencer witch will go in a 120 ml hdpe bottle. take 21g of NaF with 60g of NaHSO4(an exess is better) and disolve it in 60ml of water outside in the steel can, pour 40ml of water in the hdpe bottle (make sur that the condenser go in the water) and make and snow/HCl bath for the bottle.Than distill the solution of NaF in the steel retort(like if you distil HCl ). go away from the set up . after that take the hdpe bottle and you have arround 8-10%HF solution.


when you ave your TiCl3 or fluoro complex you can fallow this guide from:
1=TiCl3
2=fluoro complex



1-1 take the TiCl3 and ad very large ammount of ammonia , filter the hydroxide it dont affect the finnal product if it disproportionate to hydrous titanium dioxide , it will just be more long to react.

1-2take the fluoro complex and ad very large ammount of ammonia , filter the hydroxide it dont affect the finnal product if it disproportionate to hydrous titanium dioxide , it will just be more long to react.



2-1ad the minimum amount you can of 9% HCl to the hydroxide a pale clear yelow solution will form.

2-2ad the minimum amount you can of 9% HF to the hydroxide a clear solution will form.



why all the time i sayd to use 9% is because i find it react more readily than other conssentration. for your camping pot you will probably need to cut it in piece (very difficult). also you can make very conssentred solution by boiling it to 1/4 of is volume.

with this 2 solution you can make almost all compound of titanium.

[Edited on 10-3-2011 by plante1999]

[Edited on 10-3-2011 by plante1999]


That's theory, Plante. My experience with TiO2 is that no matter how 'fresh' it is, it WILL NOT redisolve in HCl, it is very much like SiO2 in that respect... But it will easily dissolve in HF... "H2TiCl6" doesn't really exist.
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plante1999
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[*] posted on 11-3-2011 at 10:37


in one of my reference about titanium it said that H2TiCl6 existe , it said that it is the acid of (NH4)2TiCl6 and it can be synthesis with titanium hydroxide or hydrous TiO2 witch have the formula : TiO2 nH2O , and with my experiment (see my video how to make chlorotitanic acid) it work(the hydroxide and the hydrous titanium dioxide disolve readily in HCl , and fallowing wath i read the formula of the hydroxide is Ti(OH)2O. and blogfast i alway experiment wath i said ( or read it) befor posting , or i will say : I think
....

@do you have pdf document about titanium chemistery , if yes can you please send it to my , i am alvay in search about titanium chemistery document , i have arround 1300 pages about titanium and zirconium chemistery. Thanks!

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]




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[*] posted on 11-3-2011 at 14:22


Plante:

The video above doesn't show the oxidation of Ti(OH)3 (or whatever way you want to formulated hydrated Ti [III] oxide) and doesn't show the dissolution of the formed TiO(OH)2 in HCl either... Are you talking about another video? If so, which one?

And if you’re into titanium you might like this article of mine. Follow the links for the serious stuff…
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[*] posted on 11-3-2011 at 14:29


yes im talking about another video sorry for the inconveniance, here the video. here in the video you can see precipitate of fresh ti hydroxide witch i react with hydrochloric acid ,it disolving it very fast.

<iframe sandbox title="YouTube video player" width="640" height="390" src="http://www.youtube.com/embed/eKfwMx824wc" frameborder="0" allowfullscreen></iframe>




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[*] posted on 11-3-2011 at 14:44


Plante… hmmm… it’s rather difficult to see any TiO(OH)2 AT ALL in the first part of this video as everything is obscured by the label (tape)!

I will be trying this maybe even tomorrow. If it really does work, why not try and isolate solid (NH4)TiCl6?
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plante1999
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[*] posted on 11-3-2011 at 15:09


i will probably made another video about it (with more small tape)also ammonium chloride and hydrochloric acide dont make an infusible white precipitate with sodium hydrogen carbonate(also i read that ti hydroxide + binary acid = alway H2TiX6 , X=halogen,in this book chlorotitanic acid solution is described like a pale clear yellow solution(witch correspond to the resuld i have obtained)) i precipitate it from fluoro complex , i dont know if you ave accex to HF or an substitute but it is very easily made, also the formula is (NH4)2TiCl6 probably i will make a reaction that i think will work (i will check in my bookshelf about titanium, if is it the best way) make this reaction:

2NH4OH + H2TiCl6 -> 2H2O + (NH4)2TiCl6

from wath i read (NH4)2TiCl6 is moderatly solube in water. and it is yellow.


[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]

[Edited on 11-3-2011 by plante1999]




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[*] posted on 12-3-2011 at 06:40


To make (NH4)2TiCl6, assuming it CAN be isolated, start from a roughly known quantity of TiCl3 or TiOSO4 in solution. Precipitate with alkali as TiO2 and filter and wash carefully with plenty water. Redissolve in excess HCl (assuming that works like you claim) and add required amount of NH4Cl (TiCl4 + 2 NH4Cl --- > (NH4)2TiCl6). Then evaporate by simmering until solution starts sputtering and/or solid matter starts to appear. Ice the solution: most of the (NH4)2TiCl6 should drop out. Gather on a plastic tea strainer and wash carefully with iced water.

The K salt may be easier (lower cold solubility, generally speaking) to obtain.

Dissolving significant quantities of Ti metal using weak HCl or (even weaker) HF, like you’ve been doing, is a very slow process though. You should really try fusing commercial TiO2 with (Na, K)HSO4 or with a mixture of conc. H2SO4 and (NH4)2SO4…


[Edited on 12-3-2011 by blogfast25]
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[*] posted on 12-3-2011 at 06:57


in fact i dont think NH4Cl will work because it is somewath acidic and H2TiCl6 is an acid , so i thinkyou need to use a base , like NH4OH.

[Edited on 12-3-2011 by plante1999]




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[*] posted on 12-3-2011 at 07:25


No, no, no, no: there’s no problem AT ALL, with NH4Cl’s weak acidity. Here’s some stuff about the preparation of a homolog of (NH4)2TiCl6, namely (NH4)2SnCl6 and K2SnCl6:

http://www.sciencemadness.org/talk/viewthread.php?tid=14911

Remember: the ‘H2TiCl6’ that you speak of is highly dissociated in water: H2TiCl6 + 2H2O < --- > 2H3O+ + TiCl6 (2-)

In fact the more acidity, the better! It prevents the TiCl6 (2-) anion from hydrolysing!


[Edited on 12-3-2011 by blogfast25]

[Edited on 12-3-2011 by blogfast25]
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[*] posted on 12-3-2011 at 07:29


o yes i have forgoted this , thank you blogfast25!


here a very long passage of brauer.


Quote:

Ammonium Hexachlorotitanate
(NH4)2[TiCl6]
This is a good, easily measured starting material for preparing hydrochloric acid solutions of titanium, since it forms concentrated, stable solutions in water or dilute hydrochloric acid.
TiCl4 + 2NH4C1 = (NH4)2[TiCl6]
189.7 107.0 29G.7
The preparation comprises precipitation of (NH4)2[TiCls] from an HCl-saturated solution, using a special apparatus which may also be employed in many other syntheses.
A 200-ml. wide-neck Erlenmeyer flask is used to hold 100 ml. of solution. The flask is closed off with a closely fitting three-hole rubber cap ("fermentation cap"). A glass stirrer, preferably of the twist drill type, is inserted in the center hole; a drop of glycerol is used for lubrication and gas seal. The use of a ground joint sealed to a mercury-seal agitator is also reccommended. Laborious centering of the stirrer is avoided and easy assembly and dismantling of the apparatus promoted by coupling the stirrer to the motor shaft (or the speed reducer shaft) by means of a piece of strong, rigid rubber vacuum hose. The direction of rotation of the stirrer is such that the center of the liquid is pushed down; higher agitation rates can be reached with this arrangement without danger of splashing, and the stirring is also more efficient.
The flask is supported at the neck by a clamp which holds it in a cooling bath at a depth so that it is covered with coolant to just below the clamp level while still leaving enough coolant underneath the flask to provide cooling of the bottom.
The gas inlet tube need not dip into the solution, since the rate of absorption of HC1 in the vigorously stirred liquid is so rapid that it is almost controlled by the input rate alone; possible plugging of the inlet tube is also avoided by not letting the tube dip into solution. The HC1 addition rate is controlled to avoid the formation of a mist above the stirred mixture, a point at which evaporation losses just begin. The greater the stirring rate, the higher the rate at which the HC1 may be introduced, and the sooner the end of the run. Complete saturation of 100 ml. of precipitation solution requires less than one hour.
The HC1 flow rate is sharply reduced toward the end of the run. The progress and termination of the HC1 absorption can be followed by means of bubble counters inserted ahead of and behind the precipitation flask.
The HC1 generator must be capable of yielding a continuous stream of gas and must also allow a wide range of adjustment in the flow rate; in addition, it should be easy to start, give an air-free gas stream as soon as possible after the start, and stop generating gas shortly after being turned turned off. The generator described on p. 280 fulfills these conditions less well than the apparatus developed by W. Seidel [Chem. Fabrik 11, 408 (1938)], in which cone, hydrochloric and cone, sulfuric acids react to give a good yield of HC1; this is accomplished by dropping the acids separately onto a packing of glass beads.
If only small quantities of HC1 are required, the most convenient generator is still the Kipp, which utilizes the reaction of cone, sulfuric acid with lumps of NH4C1, particularly since the gas does not have to be dried. However, foaming is quite pronounced at larger HC1 flows.
Returning now to the precipitation of (NH4)3[TiCl]6» gaseous HC1 is introduced at 0°C into a solution of 6 g. of TiCU in 100 ml. of aqueous (7:1) hydrochloric acid containing about 4 g. of NH4C1. The HC1 gas is added until saturation. Then the HC1 flow is stopped, but stirring is continued until complete precipitation. If the precipitation rate is low, the yellow (NH4)3[TiCl8] is obtained in the form of coarse crystals averaging 0.1 mm.
The precipitate is separated from most of the mother liquor by a short suction filtration through coarse fritted glass (without allowing air to be drawn through the compound), and the crystals are then pressed between two pieces of filter paper. If an asbestos filter is used, the compound must be repeatedly boiled with cone, hydrochloric acid and then very thoroughly washed.



PROPERTIES: Yellow octahedra, probably of the KafPtCls] structure. May be stored for an indefinite period if moistened with hydrochloric acid and kept in a closed container; on washing with anhydrous ether and drying over cone. H3SO4 in a vacuum desiccator, decomposes with pronounced evolution of HC1. In moist air, forms a white hydrolysis product, which is unusual in still being soluble in water. REFERENCES: A. Rosenheim and O. Schiitte. Z. anorg. Chem. 26, 239 (1901); W. Fischer and W. Seidel. Z. anorg. allg. Chem. 247, 333 (1941); W. Seidel and W. Fischer. Z. anorg. allg. Chem. 247, 367 (1941).


altoug it doesn use H2TiCl6 , it said the prprety.
i will try today to make a tiny amout of it.

[Edited on 12-3-2011 by plante1999]

[Edited on 12-3-2011 by plante1999]

[Edited on 12-3-2011 by plante1999]




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[*] posted on 12-3-2011 at 07:51


It would appear to prove that semi-stable chlorotitanium coordination complexes do exist. But (NH4)3TiCl8 makes no sense: that would make the oxidation state of Ti = +V, not +IV! ( + 3 - 8 + x = 0, ergo x = +5).

Check with Brauer (these texts don’t ‘export’ well…)

H2TiCl6, MAY, MAY, exist as a solid hydrate but I doubt it very much...

[Edited on 12-3-2011 by blogfast25]
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[*] posted on 12-3-2011 at 08:03


the only solution is try to precipitate it.



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