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Author: Subject: Separation of a US nickel
Melgar
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[*] posted on 21-7-2011 at 13:54


If pre-1981 canadian nickels are too hard to find, pre-1999 canadian quarters and dimes are also pure nickel. If you've got a few bucks handy, go onto ebay and you'll find people selling loads of pre-1981 canadian nickels for the nickel content. I bought around 30 nickels for $10 once. Sure, it'd be cheaper to find them myself, but that's still a great price for pure nickel metal.
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cyanureeves
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[*] posted on 21-7-2011 at 16:07


tank that is the idea. nickel can be gotten as coins or salt but if i could avoid buying it would be great because if you look around there is stainless and cupronickel everywhere.to me nickel in any form is good because even if you could afford to buy nickel salts or metal for plating it will require alot to plate something bigger than a rim or even a hubcap.i would fill a trash can full of nickel plating solution if i could grab it from pesos or nickels.copper is beautiful but in this case i wish it were'nt ever discovered. patience and determination to you.
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[*] posted on 22-7-2011 at 12:29


Reeves, you'd have one hell of a task disposing of a trash can full of spent or contaminated nickel solution. Either way, dissolving nickels by electrolysis coupled with Sedit's ammonia separation method makes small scale nickel salt procurement very feasible, I'd say. It's unlawful to use currency for this purpose (as we all probably know). Poor Thomas Jefferson!... :D

Having said that, I have a ton of Mexican pesos put away somewhere that I never got around to exchanging back to dollars. Care to enlighten me some? ;)

Tank
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cyanureeves
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[*] posted on 22-7-2011 at 15:30


no tank it was not conclusive yet. sedit separated nickel and copper in their hydroxides by adding ammonium hydroxide as the copper hydroxide is supposed to be insoluble and nickel complexes going into solution with ammonium hydroxide and then precipitating. i was to able to nickel plate a pair of pliers with the solution. i turned it back to the carbonate then eventually to the acetate with vinegar but even then copper plated out as well .sedit went on further to say his blue nickel precipitate did not produce a blue solution any further upon adding ammonium hydroxide again. mine did! although it was much lighter, others said it was not possible as a nickel ion is a nickel ion is a nickel ion and the complex will always turn blue with ammonia. geesh i got to get a life! pesos have very little nickel but they are plentiful and when you dissolve them using current they turn bright red then alternating to fluorescent yellow- green. who needs stinkin nickel when you have pretty colors amigo?
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m1tanker78
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[*] posted on 23-7-2011 at 07:59


Speaking of colors: Some of my samples have produced colorful layer effects. A good portion of the copper was reduced out so the liquor was nickel-heavy to begin with. It took A LOT of household ammonia to treat a small volume of liquor so I opted for concentrated ammonia.

I momentarily bumped the voltage up twice toward the end of the run and a nice nickel foil plated out amid the copper sludge (at the cathode). Most of the copper that I periodically removed from the cathode was in the form of Cu2O, Copper(I) Oxide. Because this form of copper is spongy, I'll have to wring it out in a water wash in order to remove much of the nickel solution trapped within it. This conforms to my other goal here which is to collect the copper in a usable form.

I hope to have some time to do a few more experiments when I'm back home later today.

Tank
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[*] posted on 23-7-2011 at 08:44


oh man only once have i produced a nickel foil with the guts of a nickel cadium batttery but i didnt record what all i did so i couldnt reproduced it again. what are you using as solution? hcl acid or sulfuric? and at what voltage do you recall you were using when you got the foil? pesos ( Contenido: 65% de cobre, 10% de níquel y 25% de zinc) 65% copper,10% nickel 25%zinc. but looks as if they add paprika, lemon and cilantro with all the great colors they produce.
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[*] posted on 23-7-2011 at 08:45


Quote: Originally posted by cyanureeves  
no tank it was not conclusive yet. sedit separated nickel and copper in their hydroxides by adding ammonium hydroxide as the copper hydroxide is supposed to be insoluble and nickel complexes going into solution with ammonium hydroxide and then precipitating.


This is not how it works. Honestly I'm not sure what exactly is taking place. When I started it seemed straight forward and proceeded as planned yet when I brought the experiment to the attention of people here they stated that it wouldn't work;). This is one case where theory does not exactly match experiment.

The idea came from a patent that I posted in another thread that spoke about precipitating Ni oxide/hydroxides onto activated carbon to make a highly active Nickle reducing agent. They used Ammonium hydroxide to precipitate the nickle and that's when I decided that it should work well for separating Cu and Ni since Copper complexes with NH3 and I was unaware that Ni also did.

Experiments showed that Nickle can in no way complex half as much as Copper does and I believe this is why the nickle precipitates out instead of complexing with the Ammonium ion.

The only thing that did not make sense was the fact that after washing the precipitate repeatedly and adding more ammonia there was no sign of any complex yet the precipitate tested positive for Ni. I added HCl to it and it crystallized into the distinct green Nickle chloride hydrate.

The process is in no way stream lined however the principle of it does work. I wish I was 100% sure how it worked but it does indeed precipitate the Nickle while holding the Copper in as its soluble amine complex. I have never obtained yeilds or much other data I wished to have so if someone wishes to further the experiment please be a doll and see what you can gather. Its a huge pain in the ass, the main issue is the fineness of the precipitate. Its next to impossible to filter out.

I also one time much later then those experiments managed to dissolve all of the precipitated into excess NH3. I left this solution sit out for god knows how long and in the bottom large green crystals precipitated out. I still have them crystals but I don't know what they are. I would post a picture but it will be very large and I don't know to re-size it to fit into the window here.





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[*] posted on 23-7-2011 at 10:45


i have it all wrong and i'm sorry for that.
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[*] posted on 23-7-2011 at 13:43


Quote: Originally posted by cyanureeves  
[...] but looks as if they add paprika, lemon and cilantro with all the great colors they produce.

LMAO! Yeah, I think I'll leave the pesos alone. IIRC, I bumped up to 1.7V (drawing ~ 3A). I used a relatively low concentration of HCl.

Sedit, oddly enough, it appears that the blue liquid layer contains a much higher proportion of nickel than the precipitate. I can't confirm that just yet, though. I took a small sample of both and subjected to heat. Both release a fine white smoke when dry. My first thought was ammonium chloride. I 'condensed' some of the smoke on a cool surface. This left a fine bright yellow powder when heating the blue complex. I neglected to collect the white smoke from the other stuff that precipitates. I performed these experiments outside. I'm not comfortable taking chances with heating unknown nickel salts.

Next up, I would like to reacidify a sample of both and try converting them to carbonate. The color of the precipitate might yield some clues about the content of each. Ammonium chloride should easily remain dissolved and not interfere with the experiment in any way.

Tank

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[*] posted on 23-7-2011 at 15:12
Sorry for double posting...


I went ahead with the carbonate prep I described above. I used HCl and a strong sodium carbonate solution. The fluff didn't fully redissolve when acidified. It left a murky solution (but no longer brown). I think it was slightly OD green. When the solution returned to basic, the brown fluff reappeared. No sign of copper or nickel but it was hard to tell. BTW, this precipitate was washed meticulously prior...

On the other hand, the blue complex turned a nice green when acidified. I didn't observe any insoluble crap at this point. When basified, the solution turned sky blue and a white precipitate began to fall out. As the precipitate layer grew in thickness, the light lime-green color became more and more obvious. What bothers me is why the solution remains colored baby blue.

[EDIT]: The blue is probably dissolved Ni2+?

Regardless, here's a pic I snapped. I didn't realize it turned out blurry until after I uploaded it...



Tank

[Edited on 7-23-2011 by m1tanker78]

[Edited on 7-23-2011 by m1tanker78]
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[*] posted on 23-7-2011 at 17:40


is the green copper? the green looks like nickel in the carbonate and in the chloride and in the sulfate but copper in the chloride is green also. isnt copper known to look green or black in concentration then turn blue as it gets more diluted?hey maybe copper and nickel swapped around and the more you dilute it the more copper disperses and nickel sinks. i know i'm dreaming but nickel does get pulled down to the bottom in darker concentration in some solutions.
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[*] posted on 24-7-2011 at 06:07


I prepared some nickel chloride a while ago by dissolving 6 1970's canadian nickels in HCl. The resulting solution was a very deep emerald green, and I stored the concentrated solution in small 125 ml pyrex bottle. I never attempted to reduce the solution by evaporation or boiling off to make crystals because frankly, nickel salts and their vapors scare me!

Is my little bottle of NiCl2 okay for storage in my lab or should i seal it ever further? It's just about 75ml but I treat it as if it were metallic mercury... very carefully!

But definitely, trying to separate nickel from other metals might be an interesting acadmic endeavor, but I'd rather start with pure nickel to start with if I wanted to prepare a nickel salt... you're sure of the end result then. Perhaps we could try to find potential sources for pure nickel... as mentioned above, a lot of canadian coinage was made out of pure nickel, the coating of many rare earth magnets too...

Robert





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[*] posted on 24-7-2011 at 12:00


I'm open to suggestions for a more conclusive test. Until I can perform such test(s), here's the way I see it. The precipitate is Nickel(II) Carbonate. The solution contains a small amount of Nickel(II) ions aside from Na, NH4, etc. A recap of how I got to this point:

Dissolved some US nickels (cupronickel) and simultaneously dummy plated out some of the copper.

Treated sample of dark emerald green liquor with concentrated ammonia.

Separated blue complex from brown/green precipitate.

Added concentrated HCl to blue stuff (turned emerald green).

Added saturated solution of sodium carbonate until basic. Solution turned sky blue color and white precipitate formed. Precipitate appears light green (accentuated in above pic). Solution remains smurf blue.

++++++++++++++++++

On the other hand, the precipitate from the ammonia treatment appears to be a mixture of copper and iron or some other component. I used distilled water at every stage (as needed) but my HCl is tech grade. :(

I suppose I'll wash the greenish ppt a few times and go from there?...

Tank
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[*] posted on 24-7-2011 at 12:20


tank on the second part of your answer are you saying that the brown/green precipitated from ammonia was iron and copper? then the blue liquid had all your nickel which turned green when hcl acid was added and precipitated with sodium carbonate as nickel carbonate? why the sad face icon? who gives a rat blankety about iron and copper?boy i hope you got nickel carbonate. if it is then drying it and adding a bit of vinegar and warming the solution will make nickel acetate and should be enough to nickel plate a penny with about 4 or 5 volts. if it plates pink then you know you have copper in your precipitate.
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[*] posted on 24-7-2011 at 14:17


Well, It's hard to tell what's in the precipitated crap from the ammonia treatment. After several washes, the ppt remains brown. It settles rather neatly and leaves perfectly clear water at the top of the 'test tube'. I was hoping to be able to isolate or at least see some conclusive indications of copper in this stuff.

On the plus side, I'm almost certain that nickel is absent from the ppt (after a couple of washes, anyway).

Now, washing the precipitated carbonate still yields a green-tinted white ppt and a light baby blue supernatant. :cool: The reason I'm banking on fairly pure nickel(II) carbonate is...

*Apparently, nickel is absent in the ammonia-precipitated crud. By this, I mean after a couple of washes. The as-precipitated crap is too murky to draw any conclusions (but gives an indication of copper).

*Nickel(II) carbonate is verrrry slightly soluble in water so in theory, I'll never have a perfectly colorless solution no matter how many times I wash the carbonate.

*The pure carbonates of nickel and copper can be distinguished somewhat by color. I prepared a small batch of copper carbonate so that I could compare side-by-side.

*Pure copper carbonate will leave a perfectly colorless supernatant, unlike nickel carbonate.

I don't want to jump to conclusions so I'll take this a step or two further. I might even try plating a small part like cyanureeves suggested. I'd be inclined to plate from a sulfate solution, though. Why acetate (for nickel)?? :o

Tank



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[*] posted on 24-7-2011 at 16:59


geesh man i just got too excited, there is no better reason for the acetate over the sulfate as a test. just that i have pure nickel sulfate and as a matter of fact its even easier to plate with nickel sulfate but nickel acetate can readily plate in the cold. you dont even have to warm nickel acetate like i said before but you do nickel sulfate to adhere better. i saw a guy on you tube plate out of a cold acetate solution and i also plated a pair of kleins like that. carry on, carry on youre doing great. i didnt know about copper carbonate leaving a clear solution i thought only the hydroxides were hard to dilute.
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[*] posted on 25-7-2011 at 07:27


Im a bit confused as to whats going on here mainly due to the talk of the carbonate,

Do I understand correctly that your saying the green precipitate formed from treating the dissolved coin salts in (aq)NH<sub>3</sub> tested negative for Nickle?





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[*] posted on 25-7-2011 at 08:22


Quote: Originally posted by Sedit  
Do I understand correctly that your saying the green precipitate formed from treating the dissolved coin salts in (aq)NH<sub>3</sub> tested negative for Nickle?

I haven't conducted any conclusive tests yet. The brown/green precipitate from ammonia treatment gives a very strong indication of iron(II). The only possible sources of iron contamination were my tech grade HCl and/or iron leaching from the SS cathode. I took care to remove and replace the cathode live to prevent corrosion but the potential was so low that a little undoubtedly leached and dissolved.

Although I plated out a lot of the copper, there MUST be a measurable amount left in the liquor. The cell liquor started out emerald blue and slowly transformed to emerald green as the nickel concentration rose and copper concentration fell.

The most troublesome part of my series of experiments on this is not being able to find the copper! It may well be hidden among the precipitated nickel carbonate. The iron contamination is also a PITA because it screws the simple tests I've run so far with the ammonia-precipitated stuff.

I may need to repeat this experiment from the very beginning using an insoluble (filter-able) cathode due to the low cell voltage and hence, lack of cathodic protection. Graphite should work just fine for this, I think.

Tank
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[*] posted on 25-7-2011 at 15:28


Convert it to there respective sulfates and precipitate the Iron by bubbling air in, use Pb next time. Filter this and it should remove most of the Fe contamination.

The precipitate in my test from the Ammonium hydroxide treatment is what was washed repeatedly with water then converted to the chloride yielding green needle crystals presumed to be pretty pure Nickle chloride. HCl and aluminum foil precipitated a black substance that was strongly attracted to a magnet.





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cyanureeves
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[*] posted on 25-7-2011 at 16:40


both of you gentlemen are at exactly opposite poles of each other unless tank isolated the nickel from the very start with ammonium hydroxide.
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[*] posted on 26-7-2011 at 07:09


Sedit, the magnet test (which I forgot about) will be useful once I remove iron from the mix. Thanks for the suggestions. Just to clarify, you precipitated nickel powder from an acidic solution of nickel chloride with aluminum, right? Seems easy enough for a qualitative test for nickel...

+++++++++++++++++++++++

I dried a sample of the freshly prepared carbonate (same as the pic I posted before). For clarity, this carbonate is prepared from the ammonia complex, not from the original precipitate.


Although the image is crap, the powder bears a striking resemblance to 'the real deal', nickel(II) carbonate. Then, I'm reminded, "Don't judge a chemical by its color."

So what's better here, acetate for a plating test or chloride then reduce with Al for a magnet test? It's probably too little to practically plate anything except maybe the tip of a copper wire or similar. I have ~ 500mL of cell liquor left from this batch.

Tank
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[*] posted on 26-7-2011 at 15:02


drop the metal with aluminum because whatever it is you can always redissolve it. go for the magnet because really my main interest is all about plating,besides you still have the brown precipitate. is that a bottle cap? its an awful tiny bit but another reason not to plate is because if it is copper then you will introduce nickel into your test and contaminate it with the anode. good work either way. you said you used household ammonia didnt you?was that the regular clear stuff? i am out of ammonium hydroxide and dont know if it is safe to use an aluminum jogger's water bottle to heat ammonium nitrate and sodium bicarbonate to generate ammonia.

[Edited on 26-7-2011 by cyanureeves]

[Edited on 26-7-2011 by cyanureeves]
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[*] posted on 27-7-2011 at 07:27


Reeves, it's a large pill bottle cap. I poured a little out to show the color. The yield was just over a gram from the sample I took from the cell; I hesitated to do the entire batch since I'm still not sure what's what. If this stuff is relatively pure nickel carbonate then I'll drop the rest of the nickel out of the remaining liquor.

I used concentrated ammonia. 'Clear' ammonia seems to work but you'll need a s*it load of it. The extra water isn't a problem if you're collecting the precipitate. If you're going for the ammonia complex, you'll probably lose some nickel to the extra water. That's if my assessments so far are correct.

If you have or can get ahold of some ammonium sulfate and calcium hydroxide (hydrated lime), that's another convenient route to ammonia. Even a crude distillation setup will yield concentrated ammonia of high purity from that mix. The byproduct is calcium sulfate (plaster).

Quote:
i am out of ammonium hydroxide and dont know if it is safe to use an aluminum jogger's water bottle to heat ammonium nitrate and sodium bicarbonate to generate ammonia.

Aqueous ammonia will corrode aluminum so, no.
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[*] posted on 28-7-2011 at 17:01


I plated a piece of copper pipe today. The idea was to determine whether nickel ions are present in the ammonia complex that forms when a mixture of copper(II) chloride and nickel(II) chloride is treated with aqueous ammonia. For this, I had to prepare a new batch since I plated out much of the copper from my previous batch in an attempt to pre-refine the liquor. The problem with iron contamination was eliminated in this new batch. This experiment can't quantify nor rule out the presence of copper ions in the complex.

Contrary to what has been proposed and reported before, the experiment clearly demonstrates that nickel ions are present, possibly in abundance, in the ammonia complex. The proportion of copper ions (if any) of the same is unclear as of yet.

Again, forgive the poor quality photo. It's the cell camera, not me (I swear). :D


The overall nickel concentration per volume of electrolyte is very low so it's difficult to produce an even deposit, let alone a lustrous one.

I'm still open to suggestions for a relatively garage-friendly way to quantify the copper proportion in the complex.

Tank
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[*] posted on 28-7-2011 at 18:41


wonderful. nickel plating is not like silver plating in which silver is atractted to the cathode at all areas. nickel is not as simple and an even deposition on a round object is harder than laying it on a flat surface. even if you plate a flat surface it will depend on which side is facing the anode thats why multiple anodes are used. dont worry about the brightness because usually it takes a bit of nickel chloride,nickel sulfate and even epsom salt and boric acid to make the famous watts solution.that is just great.
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