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ronstark
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[*] posted on 2-2-2017 at 23:12
Nickel Chloride


Can Nickel Chloride be made from Nickel Acetate? Thanks!

[Edited on 3-2-2017 by ronstark]
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JJay
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[*] posted on 2-2-2017 at 23:37


I'm sure it's possible. It would be trivial to make nickel chloride from nickel sulfate.



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j_sum1
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[*] posted on 3-2-2017 at 01:36


Nickel acetate (like most (all?) acetates) decomposes on heating. That would leave you with an oxide presumably. You could then react with HCl and you would have your chloride.

There are probably easier ways but that is what came to mind.
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[*] posted on 3-2-2017 at 01:40


Nickel chloride is needed and you have nickel acetate and an insouble acetate salt where there is some insouble chloride also exists example silver ions
calcium chloride with nickel acetate would work
But must be percipitated with an alcohol insouble
calcium acetate
insoluble in acetone and ethanol
Slowly adding the solution to absolute ethanol
This Method avoids using HCl acid
But absolute ethanol or acetone is needed

[Edited on 3-2-2017 by symboom]
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Praxichys
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[*] posted on 3-2-2017 at 05:21


You could add sodium bicarbonate or sodium carbonate to a solution of the nickel acetate. This will precipitate insoluble basic nickel carbonate, leaving sodium acetate and excess sodium carbonate in solution.

Filter and wash the nickel carbonate and react it with HCl, which will release CO2 and form a clean solution of the chloride.




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Melgar
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[*] posted on 3-2-2017 at 05:58


The trouble with heating nickel acetate to decomposition is that some carbon and carbon monoxide is produced, which can reduce nickel back to the metal form:

http://link.springer.com/article/10.1007%2FBF02546925

Apparently though, heating to 350˚C will decompose the acetate to the carbonate and the oxide. Adding HCl to either will form the chloride salt, and either water or CO2, which will evaporate when you dry the salt out.
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[*] posted on 3-2-2017 at 06:21


Melgar, that reminds me: Nickel tetracarbonyl can be prepared with nickel powder and carbon monoxide at about 130˚C. I'm not sure if a significant amount of it would form during the decomposition of nickel acetate but I would worry about breathing the effluent gas from such a reaction. Nickel tetracarbonyl is extremely poisonous, about 6 times more than hydrogen cyanide.

From wiki:

Its LD50 for a 30-minute exposure has been estimated at 3 ppm, and the concentration that is immediately fatal to humans would be 30 ppm.

The vapor decomposes quickly in air, with a half-life of about 40 seconds.




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Melgar
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[*] posted on 3-2-2017 at 07:00


I believe that the temperatures at which CO is evolved are too high to form the tetracarbonyl. Of course, if you have a lot of the acetate salt and you're applying heat unevenly, there's always a chance of making some, but I don't think it's very thermodynamically favorable.
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JJay
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[*] posted on 3-2-2017 at 16:40


Quote: Originally posted by Praxichys  
You could add sodium bicarbonate or sodium carbonate to a solution of the nickel acetate. This will precipitate insoluble basic nickel carbonate, leaving sodium acetate and excess sodium carbonate in solution.

Filter and wash the nickel carbonate and react it with HCl, which will release CO2 and form a clean solution of the chloride.


Precipitating the nickel as a carbonate and then reacting it with HCl is an excellent idea.




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CharlieA
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[*] posted on 3-2-2017 at 17:46


Quote: Originally posted by Praxichys  
You could add sodium bicarbonate or sodium carbonate to a solution of the nickel acetate. This will precipitate insoluble basic nickel carbonate, leaving sodium acetate and excess sodium carbonate in solution.

Filter and wash the nickel carbonate and react it with HCl, which will release CO2 and form a clean solution of the chloride.


I second the motion! After reaction with the stoichiometric amount of HCl, filtration to remove insolubles (if any), then simple evaporation will yield the Ni(II)Cl.
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[*] posted on 4-2-2017 at 01:54


Is the carbonate a lot easier to deal with than the hydroxide? Because that was a pain to filter by gravity. Washing, settle, decant, wash, settle, decant, SLOW filtering to a gelatinous mess, slowly shrank down to a paste then a putty as I wanted the hydroxide.

If its similar and you don't have a vac filter, it will be a while. It was just so gel like I didn't trust it would wash out easy. Nor did it settle quickly. Added a fair amount of liquid to my waste bucket too.




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[*] posted on 4-2-2017 at 11:23


Pretty much all the metal carbonates and hydroxides are difficult to filter by gravity. Before I used vacuum, I used to pour basic copper carbonate through an old T-shirt stretched over a bucket. It doesn't catch everything but it does catch something like 95% of it. Once most of the water is gone, you can put on some gloves and twist it up to squeeze the rest of the water out, then scrape the paste off the shirt to dry on a plate. It's messy and lossy but it works.



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[*] posted on 4-2-2017 at 11:40


Some metal hydroxides form oxide upon heating, which filter out much more easily (copper, for example). Nickel isn't one of them.

If you have really concentrated ammonia, you can dissolve the nickel acetate in that and then add ammonium chloride. Ni(NH3)6Cl2 has a low solubility, and then can be heated gently to give NiCl2 (easily recrystallized to give the hexahydrate).




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[*] posted on 4-2-2017 at 14:22


The t-shirt/bucket technique is extremely flexible and works well for a variety of hard-to-filter calcium salts, hydroxides, carbonates, etc. I wouldn't do this with a t-shirt that I ever planned on wearing again.



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[*] posted on 4-2-2017 at 17:45


A word of care: when dissolving Ni-carbonate, make sure not to breathe the aerosole formed. Nickel salts are carcinogens.

Nickel hydroxide can be voluminous, but does not need to be. It dissolves to some extent in ammonia solution, check atomistry. The solubility of Ni(OH)2 decreases with temperature, which allows for a way to purify the crude Ni(OH)2. This takes a huge amount of ammonia, though, but you could take a household ammonia solution, which is cheap. The hydroxide separating from heated ammonia solutions is crystalline and therefore compact, contrary to the Ni(OH)2 obtained from adding a hydroxide (NaOH, ammonia, etc.) to a solution of a Ni(II) salt. This type of hydroxide is also far less reactive than the voluminous amorphous Ni(OH)2.
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[*] posted on 4-2-2017 at 19:11


Quote: Originally posted by j_sum1  
Nickel acetate (like most (all?) acetates) decomposes on heating. That would leave you with an oxide presumably. You could then react with HCl and you would have your chloride.

There are probably easier ways but that is what came to mind.


This would be the simplest way, make sure to use an excess occupied HCL though.
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[*] posted on 4-2-2017 at 22:18


The carbonate method is by far the simplest and easiest. If you don't have access to vacuum filtration, you don't necessarily need to filter the precipitate at all. Decant as much of the supernatant solution as you can, then add more water, swirl the beaker, and let it settle out again. Repeat that a few times and you'll have <1% soluble impurities in there (you know, like homeopathy ;) ). Then decant one more time and simply add HCl. Boil down or evaporate the solution.

Vacuum filtering it would of course be preferred, but if it's not available and you don't require ultra high purity, the decanting method should be very effective.

I wouldn't recommend decomposition of the acetate because you'll have to heat it very strongly to ensure that you won't be left with any organic tar, and if you do that, you're likely to render the resulting oxide less reactive than is desirable. It's just an unnecessarily messy route to take.

[Edited on 2-5-2017 by zts16]




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[*] posted on 4-2-2017 at 23:43


How many times do I forget carbonates? The fact that they are nearly all insoluble (except K and Na which is so useful) and the fact that they react with nearly every normal acid to produce a desired salt -- it is such a sensible and reliable pathway.
Decomposing the acetate might work but going via carbonate is a far superior idea.
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[*] posted on 9-2-2017 at 00:48


Nickel Acetate (aq.) was mixed with Sodium Bicarbonate (aq.). The precipitate was filtered. The colour looks the same as Nickel Carbonate. After drying in the open on a dish, HCl was added until no more fizzing. The colour changed again from a light green to a deep green. It was left to evaporate in the open without heating.

[Edited on 9-2-2017 by ronstark]
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Godrick VanHess
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[*] posted on 6-10-2017 at 18:41


Someone correct me if I'm wrong, but could you not just add HCl to form acetic acid and NiCl2 since HCl is a much stronger acid than acetic acid? If this indeed works you could distill off the acetic acid or even evaporate it off.

[Edited on 7-10-2017 by Godrick VanHess]
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