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Author: Subject: Semi metals or metalloids as anions: a preparation thread.
bismuthate
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[*] posted on 20-10-2013 at 06:10
Semi metals or metalloids as anions: a preparation thread.


I have been interested in metals as anions for quite a while and I thought that we should have a thread that describes how to synthesise compounds with poor metals as anions. If anyone here has prepared one please describe the procedure.

I have changed the title to reflect what I think is a better expression of the original poster's intention in English.

Science Squirrel

[Edited on 24-10-2013 by ScienceSquirrel]




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[*] posted on 20-10-2013 at 06:40


Do you mean things like nickel antimonide?



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[*] posted on 20-10-2013 at 06:42


Yes. Also things like aluminides, bismuthides, stannides, and more.



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[*] posted on 20-10-2013 at 07:27


By chance, I was looking at this wiki photo of nickel antimonide the other day... it's really stunning stuff, reminds me of red/pink gold.


Photo by Heinrich Pniok a.k.a Alchemist-hp from Wikimedia commons under these licensing conditions.





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[*] posted on 22-10-2013 at 05:15


Ammonium hexachlorostannate:

http://www.sciencemadness.org/talk/viewthread.php?tid=14593#...

Potassium hexachlorostannate, from pewter:

http://www.sciencemadness.org/talk/viewthread.php?tid=14668&...

[Edited on 22-10-2013 by blogfast25]




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[*] posted on 22-10-2013 at 08:18


If anybody is interested, the gentleman who made that photo of NiSb I posted in the beginning has just mailed me that he has a few grams left and is selling for $25/g, excl. postage... just thought I would pass that along. PM me for his contact details if interested. He says it's 'very nice and pure' :)



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[*] posted on 4-11-2013 at 04:06


Hi. I just recived 20g of gallium:D and I've decided to mak sodium thiogallate. Wiki (on it's page about gallium) says that it is synthesised by mixing sodium carbonate, gallium oxide and hydrogen sulfide. I couldn't find the syn thesis of sodium thiogallate elswhere, so I'd like to know if this route has been done by anyone. (I can find the synthesis for other thiogallates).

[Edited on 4-11-2013 by bismuthate]




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[*] posted on 4-11-2013 at 04:11


Quote: Originally posted by bismuthate  
Hi. I just recived 20g of gallium:D and I've decided to mak sodium thiogallate. Wiki (on it's page about gallium) says that it is synthesised by mixing sodium carbonate, gallium oxide and hydrogen sulfide. I couldn't find the syn thesis of sodium thiogallate elswhere, so I'd like to know if this route has been done by anyone. (I can find the synthesis for other thiogallates).

[Edited on 4-11-2013 by bismuthate]
Wow... ambitious, best of luck, should prove to be really fun! Incidentally, was your gallium very costly?



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[*] posted on 4-11-2013 at 04:24


It was $25.11 with shipping so it was pretty well priced. Oddly enough I had a gift card worth $25.11....:).
Maybe I shoul start out with calcium thiogallate... or barium I've found patents on those.




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[*] posted on 6-11-2013 at 07:35


Bismuthate, please tell me how your thiogallate syntheses turn out. I'd be very interested to see samples and attempt them myself.



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[*] posted on 6-11-2013 at 14:18


It is possible to make salts containing the Na<sup>-</sup> anion. They are called sodides or natrides. Some of these salts are stable at room temperature. The other alkali metals can similarly form alkides.

http://en.wikipedia.org/wiki/Alkalide




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[*] posted on 6-11-2013 at 16:44


That's absolutely amazing, although I can't imagine what it would take to synthsise and store them. I am also unsure if NaK is a compound or merely an alloy.

I now have a crude set up for what I plan to do. It is a H2S generator that leads to a test tube with a stoichiemetric mix of BaCO3 and Ga2O3. After the gas is channeled through the test tube it will be lead through multiple copper sulfate solutions to absorbe the excess gas. Any flaws or improvements to be made?

Also I'd like to take a field trip to the land of magnificent tohubohu and madscience of the most theoretical and impractical type.:) I was wondering if it would be possible to synthesise barium thiogallate from an excessive amount of H2S and anhydrous barium gallate at elevated temperatures.




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[*] posted on 6-11-2013 at 16:47


Quote: Originally posted by bismuthate  
That's absolutely amazing, although I can't imagine what it would take to synthsise and store them. I am also unsure if NaK is a compound or merely an alloy.


NaK is an alloy. To keep an alkanide stable, the cation has to be very stable towards reduction- ordinary alkali metal cations won't do (because Na+ + Na- -> 2 Na is very favourable). You have to encase the sodium cation in a cryptand-type ligand to make sure it doesn't react with the sodide/natride anion.




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[*] posted on 6-11-2013 at 17:28


Thanks for the quick response. On this subject I was reading about dilithium (an interesting Li-Li covalent bond containing compound) on wiki. I've got the dilithium prepare for warp speed.:D

[Edited on 7-11-2013 by bismuthate]




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[*] posted on 7-11-2013 at 15:43


Quote: Originally posted by phlogiston  
It is possible to make salts containing the Na<sup>-</sup> anion. They are called sodides or natrides. Some of these salts are stable at room temperature. The other alkali metals can similarly form alkides.

They are great!!!!!

I made K+K-. It had a beautiful blue color and reacted readily with a lot things. I made an indole synthesis with this nice little thing(:




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[*] posted on 7-11-2013 at 16:23


Quote: Originally posted by kristofvagyok  
Quote: Originally posted by phlogiston  
It is possible to make salts containing the Na<sup>-</sup> anion. They are called sodides or natrides. Some of these salts are stable at room temperature. The other alkali metals can similarly form alkides.

They are great!!!!!

I made K+K-. It had a beautiful blue color and reacted readily with a lot things. I made an indole synthesis with this nice little thing(:


Out of curiosity, which cryptand did you use (your formula doesn't suggest it)?

[Edited on 8-11-2013 by deltaH]




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[*] posted on 7-11-2013 at 16:34


I used 18-crown-6 and a few other custom made crown ethers.

There is a few article where they describe blue coloration of solutions while boiling polyethers like diglyme with sodium-potassium alloy. It could be an inetesting experiment for anyone. I was totally amazed by the blue color what appeared on the surface of the metal.

The K+K- is pretty reactive, if not freshly absolutized ether is used as a solvent the blue color will never really develop. Another good to know is, that it breaks up THF forming KOCH2CH2CH2CH2K if the solution is stored for a while or it heats up. This base is also a really strong base, sadly it is not so well soluble.

Also important to note that it will eat up the teflon coating of the stir bars in a few day :D




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[*] posted on 7-11-2013 at 16:36


Quote:
Also important to note that it will eat up the teflon coating of the stir bars in a few day :D
Good to know!



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[*] posted on 8-11-2013 at 05:10


I've made some germanium sulfate solution by displacing copper ions with solid germanium (in powder form). It is yellowish and highly acidic, probably due to an equilibrium with sulfuric acid and germanium dioxide (or may-be some intermediate between sulfate and oxide).
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[*] posted on 8-11-2013 at 05:55


Mixell:

Did you obtain this as a solid? Salts of highly charged, small cations (like Al<sup>3+</sup>;) tend to be acidic:

[Al(H<sub>2</sub>O)<sub>n</sub>]<sup>3+</sup>(aq) + H<sub>2</sub>O(l) < === > [Al(H<sub>2</sub>O)<sub>(n-1)</sub>(OH)]<sup>2+</sup>(aq) + H<sub>3</sub>O<sup>+</sup>(aq)

And do you know the oxidation state of the Ge? II or IV?

[Edited on 8-11-2013 by blogfast25]




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[*] posted on 8-11-2013 at 07:16


Quote: Originally posted by bismuthate  

I now have a crude set up for what I plan to do. It is a H2S generator that leads to a test tube with a stoichiemetric mix of BaCO3 and Ga2O3. After the gas is channeled through the test tube it will be lead through multiple copper sulfate solutions to absorbe the excess gas. Any flaws or improvements to be made?



Out of curiosity, how are you planning on making the Ga2O3 from the gallium?

[Edited on 8-11-2013 by sbbspartan]




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[*] posted on 8-11-2013 at 14:28


No, I've tried to desiccate it, but with no success.
The amount of copper I got points out to Ge4+.

The solution is very acidic (pH <1), probably due to the germanium cations scavenging O-/OH- from the water, leaving relatively free protons behind.
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[*] posted on 8-11-2013 at 18:44


sbbspartan, I plan to heat the nitrate until decomposition. I will make the nitrate with gallium and nitric acid. However I think that I will postpone this and look further into the possibility of synthesising thiogallates from metal gallates.



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[*] posted on 9-11-2013 at 14:32


Bismuth:

Why not simply precipitate the Ga as Ga(OH)3? Assuming Ga metal is all you have right now, dissolve in dilute HCl (and make some video/photos! You don't see that everyday) and neutralise with ammonia to precipitate the hydroxide.

I'm not sure what route to thiogallate you're looking at but freshly precipitated and washed Ga(OH)3 is likely to be far more reactive than calcined Ga2O3.




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[*] posted on 9-11-2013 at 16:15


Well blogfast, all of the procedures say that you should use gallium oxide and a metal carbonate. However as I said before I plan to make it from a gallate to increase purity. Hopefully it will work as I have not found this described anywhere. About the videos: I'm not sure I'll be able to make a video, although I'll try.
The basic idea of my newly devised (still not sure if it works) synthesis is to pass H2S over metal gallates.

[Edited on 10-11-2013 by bismuthate]




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