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Author: Subject: Separation of a US nickel
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[*] posted on 18-10-2013 at 10:28


Well I dissolved a nickel in some vinegar/H2O2, then evaporated hoping to get pretty crystals. well I got some nice crystals but I noticed the crystals were either blue, or green. With 2 different shapes. Green were more "diamond" shaped, and the blue were ehhh "more dimensional". here are some pics.





I dont think they separated cleanly, but due to a slow evaporation they did separate to an extent.




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[*] posted on 18-10-2013 at 11:58


Try sorting them out as best you can with tweezers, then recrystallize each batch again with distilled water.



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[*] posted on 18-10-2013 at 15:22


is the ratio of blue to green crystals anywhere close to blue75% green 25%?

[Edited on 10-18-2013 by cyanureeves]
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[*] posted on 19-10-2013 at 01:39


I haven't read the whole thread but would reduction with Al of Ni and Cu chlorides work to precipitate metal powders, wash in NaOH to get rid of aluminum and then magnet to separate nickel?
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[*] posted on 19-10-2013 at 16:26


Quote: Originally posted by Random  
I haven't read the whole thread but would reduction with Al of Ni and Cu chlorides work to precipitate metal powders, wash in NaOH to get rid of aluminum and then magnet to separate nickel?


No. I personally tried this and gave up quickly. The metals are too interleaved to even mill and sort with a magnet.

I'm catching up on the latest posts since I last checked. Glad to see there still seems to be some interest on this topic.

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[*] posted on 20-10-2013 at 08:11


Add a sodium thiosulfate solution to your Cu/Ni nitrate solution and heat gently. Copper sulfide should percipitate, filter and you are left with a solution of Nickel thiosulfate and sodium nitrate. Add NaOH to the soution and filter the nickel hydroxide. Add the nickel hydroxide to the acid of you choice and percipitate the nickle with aluminum.



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[*] posted on 20-10-2013 at 12:37


Quote: Originally posted by bismuthate  
Add a sodium thiosulfate solution to your Cu/Ni nitrate solution and heat gently. Copper sulfide should percipitate, filter and you are left with a solution of Nickel thiosulfate and sodium nitrate. Add NaOH to the soution and filter the nickel hydroxide. Add the nickel hydroxide to the acid of you choice and percipitate the nickle with aluminum.

Here's a reference for you:

sodium_cuprous_thiosulfate.png - 47kB

Analytical chemistry, Volume 1
Frederick Pearson Treadwell
Wiley, 1921

In the case of silver thiosulfate, it looks unstable unless it is quickly dissolved in excess thiosulfate, forming a soluble complex. Ag2S is precipitated on boiling in this case. CuS is precipitated upon boiling the acidified copper thiosulfate complex. I don't know the relative stability of a complex with nickel thiosulfate in the same environment. If the idea works, then it might be necessary to acidify the solution first, and then heat. Doing it the other way around might cause NiS to co-precipitate.

thiosulfates.png - 122kB

[Edited on 20-10-2013 by WGTR]
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[*] posted on 3-11-2013 at 10:35


Quote: Originally posted by The_Davster  
Drive to Canada. Go to a bank. Ask for a brick of nickels (100$ worth) Those from 1955 to 1981 are pure nickel metal.

Naturally, only f you are after the metal, and not just looking for some chemistry to do...


If you are searching for pure nickle, the Canadian quarter was pure nickle from 1999-1968.




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[*] posted on 11-11-2013 at 06:24


I was actually performing this experiment over the summer, and thought I'd add a few ideas I tried:

The first was to dissolve the alloy in either nitric acid or a mixture of sulfuric or hydrochloric acid and an oxidizer. It doesn't really matter, because after this you mix the solution with sodium bicarbonate and filter it so that you can make a clean mixture of nickel and copper chloride using HCl. It is important to do this because if you just use hydrochloric acid and an oxidizer, you can't use a reduction agent reliably (oxidizer will tend to interfere).

Then after you have the clean mixture of chlorides, adding Ascorbic acid reduces the copper(II) chloride to insoluble copper(I) chloride. I didn't like this method very much though because unless you're in a vacuum or inert gas environment, it readily becomes copper(II) chloride from the atmosphere and from air entering the water you use.

Another solution I found interesting, but haven't perfected, is to use acetylsalicylic acid (Aspirin). Apparently aspirin will form copper aspirinate, but nickel will not. I discovered that adding sodium aspirinate (made by adding sodium carbonate or bicarbonate to aspirin in water) to a mixture of copper and nickel chlorides will precipitate the insoluble copper aspirinate. Adding ascorbic acid seems to precipitate any remaining aspirin from the solution, leaving you with what should be nickel chloride.

Edit: I also had the idea to try and make a saturated solution of either the chlorides or sulfates and try a recrystallization, since the copper chloride or sulfate would precipitate since it's the majority. I haven't tried it yet, but at the very least it should concentrate the nickel by removing the copper.

[Edited on 11-11-2013 by cjevancich]
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[*] posted on 12-11-2013 at 18:45


@cjevancich:

Some more details (if available) would be nice.. Something that can be tested and maybe reproduced by others.

I believe all of your points have been raised or attempted further upthread.

Quote:
Edit: I also had the idea to try and make a saturated solution of either the chlorides or sulfates and try a recrystallization, since the copper chloride or sulfate would precipitate since it's the majority. I haven't tried it yet, but at the very least it should concentrate the nickel by removing the copper.


This I know has been done, albeit unintentionally, by Sedit and yours truly. Again, check upthread because as I recall, there was a good explanation of the common ion effect by blogfast. Copper sulfate did precipitate first but according to Sedit, his solution still contained a lot of copper. I never got around to testing my solution. Crystallization can probably be sped up by gently warming then cooling the concentrated sulfate solution repeatedly (ugh..).

Quote:
Run a stream of acytelene through the solution of copper/nickel nitrate then filter the solution.
Be warned this makes copper acetylide, a sensitive explosive.


I'm still holding out hope for a simple-ish way to quantify the proportion of metals in solution (for analysis, not bulk separation). Bismuthate's acetylene idea sounds good right about now and is reported and demonstrated to work with copper chloride as well.

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[*] posted on 12-11-2013 at 20:59


I use a scanning electron microscope (SEM) to quantize things around here, but why not precipitate out the respective sulfides, and
weigh those? Nickel and copper ions can be separated quite distinctly in this way.
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[*] posted on 13-11-2013 at 01:54


Removed some crap from Ph.D.Chemist user.



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[*] posted on 17-11-2013 at 07:25


i just dissolved some nickels in both hydrochloric acid and nitric acid and ran a stream of acetylene from my bottle.the nitrated cupronickel solution has not reacted as i wanted with acetylene as nothing happened.the hydrochloric acid solution however looks promising because i ran acetylene through it and also nothing but when i added ammonium hydroxide,the magic happened.i added ammonium hydroxide from ace hardware and it just disappeared into the hydrochloric solution so i added more and just when i thought it was going to drop the hydroxides it turned blood red.i went this route after watching the youtube video how to make copper acetylene.i added acetylene to the blood red solution and it has not settled yet. the hydrochloric solution was made by dissolving nickels with 5volts in Hcl acid and removing the copper sponge so the red is what little copper is in solution.i do not know how much nickel is in solution or in the removed sponge nor do i know if nickel will also drop as a hydroxide or remain in solution.i plan to nickel plate with whatever is in solution because if it all precipitates i will be back to square one again with 0 for 0.

[Edited on 11-17-2013 by cyanureeves]

[Edited on 11-17-2013 by cyanureeves]
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[*] posted on 17-11-2013 at 07:34


Acetylene separation, very very promising, although extremely unsafe in larger quantity.

Here is a rough idea:
Electrolysing Cupronickel in ammonium chloride solution, adding ammonia and copper powder. Wait a few day and precipitate the copper I with acetylene, filter the nickel solution and destroy the copper acetylide with strong hydrochloric acid. The nickle solution could be reduced to elemental nickel probably.




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[*] posted on 17-11-2013 at 10:45


it has been a couple of hours now since the acetylene was bubbled through the Hcl acid solution and alot of red precipitate has developed and has occupied half of the reaction flask.i now have half red precipitate and half blue solution which i wishfully think is the nickel ammonia complex.the nitric solution did not work in the same manner because i added ammonium hydroxide to it and as all you here would probably guess,i got nickel and copper hydroxide.RATS! Big Effing rats says johnny!
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[*] posted on 17-11-2013 at 12:57


Interesting experiment @cyanureeves. From what you say, I deduce that the solution should be only slightly acidic (near neutral?) while bubbling acetylene. Is that correct?

The only potential drawback I can think of at the moment is the addition of NH4 ions. It may not hinder anything, just something to keep in mind if one wants a more refined product later..

I'm interested to know what you find after filtering off the copper acetylide (don't let it dry out completely). If possible, leave one part for plating, another for dropping with aluminum, and another for.... whatever. lol More acetylene --> more precipitate? This would indicate incomplete saturation/reaction on the first round.

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[*] posted on 17-11-2013 at 13:04


CR:

The nickel ammonia complex is a very specific colour, I wouldn't describe it as blue, more a kind of light purple. But Cu (I) does form a diammine complex and believe it's blue (like its Cu(II) counter part).

Careful with that copper (I) acetylide: explosive when dry! Shock sensitive too...




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[*] posted on 17-11-2013 at 14:39


correction:(DARK purple) is what the nitrated solution looks like which did actually precipitate a jet black charcoal which i now have drying. nickel does indeed make up most of both left over blue and purple solutions because i totally nickel plated a copper penny with both solutions. i added sodium carbonate to both and added a bit of Hcl acid to make the plating solutions and both are effective. when carbon steel is immersed in the plating bath it will however draw out a little pink hue at first.adding some of the ammoniated solutions give more nickel power but will add alot of soot that has to be rubbed off and then exposes the shiny nickel. i have two coffee filters full of the precipitates drying but the red stuff is way,way more.seems every darn by product is volatile,from farts to bombs.i'll be careful. @ tank, yes indeed i have some unadultered solution and it was exactly what i had in mind(mo gas) i didnt check the acidity i just went by color, you cant miss it!it turns red before your eyes in a fraction of a second.one thing to note is that both precipitates are hard to clean off and messy as hell!

[Edited on 11-17-2013 by cyanureeves]

[Edited on 11-17-2013 by cyanureeves]
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[*] posted on 18-11-2013 at 05:40


Quote: Originally posted by cyanureeves  
i have two coffee filters full of the precipitates drying but the red stuff is way,way more.


If the red stuff is copper (I) acetylide that sounds rather a lot. At the risk of sounding like a broken record, be very careful with it. I would decompose it with HCl if I were you: it has fulfilled its desired purpose but now isn't needed anymore.




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[*] posted on 18-11-2013 at 15:48


yes all i want is a nickel plating solution and have no desire for explosives but either way i did not make copper acetylide because my stuff does not deflagrate. i probably did not have strong ammonia or acetylene was not enough but anyhow the precipitates have shrunk to about 1/4 it's original mass.i have to be very careful that i do not intentionally make explosives or poisons for poison's sake.i think i owe it to all sciencemadness members that i be responsible with what i learn here and everywhere.
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[*] posted on 20-11-2013 at 16:44


update: the solution containing what i thought was mostly nickel has a crapload of copper still because reduction with aluminum proves it.i get red sponge just as if i used a battery and furthermore the untouched blue solution does not turn red with more acetylene nor with more ammonium hydroxide.at this point i am stopping until i come up with some sort of bladder to keep the copper sponge on the aluminum away from the rest of precipitates as i do the reduction.i swear explosives are the result of frustration stemming from failure and wars are all caused by copper.give nickel a chance!
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[*] posted on 20-11-2013 at 17:11


Sorry it's not working. On the bright side I just realized we could percipitate 2CuI+I2 by adding KI. This seems to good to be true!



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[*] posted on 20-11-2013 at 18:41


bismuthate when i said a crapload of copper i was exagerating a bit. the acetylene dropped more copper than i have ever before.i think i should have added more ammonia or acetylene. acetylene and a bladder to filter the remaining copper will be my next attempt.the aluminum is actually turning black rather than produce more sponge. thanx for your u2u. nickel or bust!or bust,or bust,or bust!
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[*] posted on 21-11-2013 at 04:04


Ok. Also after further research I found that my KI idea would not work...:(
but AlI3 should work to percipitate CuI.




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[*] posted on 21-11-2013 at 17:41


Quote: Originally posted by cyanureeves  
update: the solution containing what i thought was mostly nickel has a crapload of copper still because reduction with aluminum proves it.


Not so fast cyanureeves.... What was your Al source? Check about half way down page 6 of this thread..

http://www.sciencemadness.org/talk/viewthread.php?tid=16811&...

I proved that Al foil (alloy) will give deceiving results. If you have access to a more pure Al source, you could rule out the above. If you don't, then let us know how it behaves around a strong magnet, por favor.

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