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Sedit
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Quote: Originally posted by blogfast25  | Stainless steel flatware”? What do you mean?
Strange indeed that no Ni(NH3)6 (2+) formed… You sure about this?
Freshly precipitated hydroxides can often be compacted by means of gentle simmering because they lose water: M(OH)m.n H2O (s) === > M(OH)m.n-x H2O
(s) + x H2O (l)
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Wikis stainless steel artical shows flatware, as in forks and spoons ect.., as "typical composition of 18% chromium and 10% nickel, commonly known as
18/10 stainless".
Im not sure about it blogfast but what I am sure about is that there was absolutely no color to the solution at all other then a grimmy oxidation
product of the Fe dropping out of solution making it a dull orange until it settled. Nickle complexes like copper was described in the other thread on
the topic to turn a blue color just like copper. There was no blue color when excluding the copper from the equation. This time it was just green
precipitate and clear supernatant fluid.
This is inline with other experiments I performed when seperating the Copper before. After a complete washing of the formed precipitate I proceeded to
add HCl and formed what by all means looked like Nickle chloride crystals. I put them back in ammonia solution expecting to see some kind of a blue
color yet I saw nothing that backed up the old text describing the complex.
The only explinations I can think of, and bear with me because im just musing here, is that the ammonia salt does not allow the complexes formation
somehow... The precipitated hydroxide does form a complex but its not soluble so its of little concern, or... It just does not exist at all.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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woelen
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[Ni(NH3)6](2+) is a well-known complex of nickel. It is formed when ammonia is added in large excess amount to a solution of a nickel salt. It has a
nice blue/purple color, somewhat like the [Cu(NH3)4](2+) complex, but the color is less intense and it is a little bit more purplish.
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Sedit
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I have seen that slimy green a number of times, thats the precipitate I always see yet never caught the complex at all. Its interesting to say the
lest. I see you have mentioned a large exess is needed to form the complex and the fact im using a dilute solution may have alot to do with it.
All in all however that would mean that since copper forms quickly and easily with NH3 and Nickle needs excess it should be no problem to extract the
nickle from the copper using ammonia hydroxide because the Cu will want the amine much more then the nickle and when using the dilute solution the
precipitate should stay in solution where as the nickle will precipitate.
This is inline with what I have been seeing and when I isolated the nickle and converted it to its chloride I got deep green needles formed from it on
drying. It looked almost exactly like this web image I managed to pull up
[edit...NM I can not get the photo to link for some reason....]
The only issue now is getting the precipitate to clump to the point where it can be seperated because it is very fine and generally hard to filter
without serious looses. Im going to try placing it on a warm plate later and see if the convection will clump it up for me.
[Edited on 14-2-2011 by Sedit]
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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smuv
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Much flatware today is made with nickel free alloys. In order to determine if it is 18/8 (304) you should test to see if it is magnetic. 304
stainless is generally non-magnetic but can be faintly magnetic in areas where it has been worked (read: sharp bends). On the other hand 4xx series
stainless have no nickel and are by far more popular for cheep flatware.
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Sedit
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In that case I have what Im pretty sure is some scrap Nichrome wire that I can always run a test with that but I don't feel the results are going to
be much different. Ill see if they have the piece labled for simplicity.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Sedit
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Sorry to double post but I thought I would bump this real quick since I figured out the last piece of the extraction puzzle.
The basic process for say US Nickle coins would be to dissolve them in a suitable acid Nitric being the fasted but I have found H2O2+HCl to work
albeit in a day or so.
Next you would dry your resulting solution to get crystals or just reduce your solution enough to carry on to the next step which would be
basification with ammonia hydroxide to precipitate the Nickle hydroxides and trapping the Cu ions in solution as an amine complex. Once precipitation
stops on the addition of more Ammonia then one should stop.
Allow the precipitate to settle and wash it a couple times with distilled H2O. Each time allowing it to settle a bit to make working with it a bit
simple.
The final piece of the puzzle is something I have used before but it just never struck me to use it here and that is to just pour the sample into an
unglazed ceramic dish. Terracotta pots would work here assuming the bottoms have been sealed. This will dry your preciptate in relatively short order
compaired to filtering.
Mix your precipitate with HCl or H2SO4 and dry to aquire the desired Nickle salt.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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not_important
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You do know that nickle also forms ammonia complexes similar to those of copper, don't you? With just enough ammonia a deep blue complex is formed,
a large excess of NH3 shifts this to a lavender hued complex.
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Sedit
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Yup, thats what we have been discussing yet it takes an excess of NH3 to form the complex and from experiments its showing that the Copper is much
more hungery for that ammonia then the nickle is. I recall that in the other thread you are the one that brought this complex to my attention some
time back and after some experimenting with it I can honestly say that as long as the NH3 is not over done one can simply extract Nickle from a
mixture of Copper and Nickle using Ammonia hydroxide.
Its a simple enough experiment to try out and I would suggest to anyone to give it a shot. If nothing else to prove me wrong or point out something im
missing. One thing that still has thrown me off however is that after getting the precipitate and cleaning it addition of alot of Ammonia hydroxide
does not produce the blue color and I don't understand that one bit.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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plante1999
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wath pourcentage of H2O2 chould i use for 30%HCl?
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Sedit
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I use 35% H2O2 for Muratic acid. Performing an electrolysis with the Nickle bearing material as the electrode in HCl would also more then likely speed
up the process a bit without having to use H2O2 to oxidise the HCl.
I also want to add that I tested my flatware to see if there is Nickle present by taking the solution and reducing it with Aluminum foil. It was very
slow at first to displace anything only producing a small amount of silvery metal on the surface of the Aluminum so I added a bit of HCl to speed
things along which worked well. A magnet showed indeed that there is Nickle present yet with Ammonia hydroxide there was absolutely NO blue color or
any color for that matter. This shows that the complex does not form without some effort in a dilute solution.
The only other metals present in this test are Iron and Chromium is Wiki is to be trusted. I realize I will have to do a photo assay of the process to
show everyone and I will indeed do that soon enough in the Cu++/Ni++ seperation thread.
I have to ask Plante, are you non american or lazy? Could you please try to spell a little better or atlest show some effort.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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plante1999
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| Quote: Originally posted by Sedit | . I realize I will have to do a photo assay of the process to show everyone and I will indeed do that soon enough in the Cu++/Ni++ seperation thread.
I have to ask Plante, are you non american or lazy? Could you please try to spell a little better or atlest show some effort. |
1-if you do thant it will help me alot
2-sorry for my not very well spelled english but i make very high effort to writh wath i think in english,im a French Canadian and my commune language
is french, because i think french forum is done wrong and are not familiar with chemistry (sorry for those like French forum) i prefer to go to much
more specialised english forum like sciencemadness , i will try to make less mistake.
thanks!
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cyanureeves
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sedit. i dried my nickel carbonate i made from the sulfate and some copper was in the drying slurry because i could see bright blue swirls on the
surface of the light green mass although not much.i added ammonia hydroxide to some of the dried carbonate and sure enough i got a blue that rivals
prussian blue in color.i now have a precipitate of a light green color on the bottom of the blue liquid and no matter how much water i keep adding it
still precipitates as a light green carbonate color.would this be my nickel hydroxide or just cleaner nickel carbonate?i dont plan on going any
further with this nickel other than into a pot for an attempt to acquire an oxide to convert to acetate,and onto my home made lab stand as plating.all
this time i thought only silver electrolyzed in ammonia and absent of oxygen would make the bright blue color.
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Sedit
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I think thats your hydroxides or oxides I can't remember which and the blue was your Copper complexing into solution. Test for yourself by drying the
precipitate and washing it. After that try to add it to Ammonia solution and see if you can still get that blue color. I personally have not obtained
it yet although i'm going to keep trying to get Nickle blue just to understand a bit better but I have on a few occasions added HCl to the precipitate
and dryed it to yeild what is with out a doubt fairly pure NiCl<sub>2</sub>
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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cyanureeves
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sedit. thanks.it would be cool if indeed it was pure nickel on the bottom because i didnt even use much ammonium hydroxide or maybe i just made a hell
of a strong hydroxide with my ammonium nitrate/sodium hydroxide.i dont understand much about your complex and i'm eager to just bake any nickel salt
in search of the oxide because it can plate out of a cold solution.sorry for seeming selfish but perhaps i'll only set you back in your search if i do
this test, only to find that i still have some impurity with an affinity for ammonia and turns blue.
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Random
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I think I posted one thread earlier and I remember that one metal of these two can be precipitated with salicylic acid.
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kmno4
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Separation Cu/Ni from mixure of their sulfates is extremely easy.
Simple electrolysis with C anode will remove practically all Cu.
Fe contamination is easy to remove as "Fe(OH)3".
Precipitating of Ni carbonate (to convert it to another salt) should be done after Cu-Fe remove. Conversion of contaminated Ni sulfate to contaminated
Ni carbonate is rather losing time...
BTW: ammonia-nickel complexes are blue.
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Sedit
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I think better then US currency in order to get Nickle the flatware or Nichrome wire would be a much better solution.
I decided to take my entire dark green "Flatware solution" and toss in Aluminum and after a hell storm of bubbles because of the excess acid, I was
greeted with a seemingly large amount of grey/black magnetic powder precipitate which im, assuming to be elemental Nickle, and a bluish solution. Sure
there is alot of contamination in it since I never precipitated the Fe as the hydroxide but this could work as a means of Ni for the determined. Due
to the fact that the solution is still blue I believe that the Chrome did not precipitate out like the Nickle did.
Knowledge is useless to useless people...
"I see a lot of patterns in our behavior as a nation that parallel a lot of other historical processes. The fall of Rome, the fall of Germany — the
fall of the ruling country, the people who think they can do whatever they want without anybody else's consent. I've seen this story
before."~Maynard James Keenan
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Random
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| Quote: Originally posted by kmno4 | Separation Cu/Ni from mixure of their sulfates is extremely easy.
Simple electrolysis with C anode will remove practically all Cu.
Fe contamination is easy to remove as "Fe(OH)3".
Precipitating of Ni carbonate (to convert it to another salt) should be done after Cu-Fe remove. Conversion of contaminated Ni sulfate to contaminated
Ni carbonate is rather losing time...
BTW: ammonia-nickel complexes are blue. |
Can this maybe be done with electrolysis of copper/nickel acetate mixture? I should try this. What will happen with nickel though?
Do you mean copper cathode on which will copper be deposited and C anode?
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cyanureeves
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sedit i decided to go ahead with the ammonia thing and i got the royal blue color solution on adding ammonium hydroxide to the nickel carbonate.if i
use just enough to get the blue solution and stop there will be nice green crystals on the bottom.when added more ammonium hydroxide to the remaining
dried green crystals i got a carribean blue.a chart i read stated that royal blue is the nickel complex and the sky blue was copper.i dont know why
nickel would beat out copper first if this is my case,but remember i used a high copper content coin.im sure i will get the lilac color if i add more
ammonia to the royal blue solution.anyway i made nickel carbonate from nickel sulfate and roasted it on a s.steal pot and i finally got what looks
like the oxide(yellow-lime green) this time i used a propane burner instead of oxy-acetylene.i was going beyond melting and wiki said the salt
decomposes before melting.i'm pure nickel rich right now but one day i'll come back to this thread to dig for nickel metal i'm sure.
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Random
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I think I figured out the best way to do it. Cuprous chloride is insoluble in water, we must then reduce copper (ii) chloride. But HCl with air
oxidizes it again into copper (ii) chloride. That means we need to have solution that won't contain any more HCl or very little and then filter
cuprous chloride fast!
1. Dissolve cupronickel coins in HCl (maybe add very little of some nitrate solution to speed the reaction a little bit).
2. Add baking soda to destroy excess HCl until the carbonates will start precipitating.
3. Add just enough HCl to dissolve the resulting carbonates.
4. Make a solution of potassium metabisulfite and mix it with cupronickel chlorides.
5. Resulting SO2 and metabisulfites reduce copper (II) ions to copper(I) ions. Cuprous chloride precipitates.
6. Filter that very fast and you have solution of nickel, sodium, so4, so3 and chloride ions.
7. Precipitate nickel carbonate using baking soda .
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bbartlog
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One flaw in your proposed method is that sodium chloride solubilizes cuprous chloride. So while only 1.5g of CuCl will dissolve in 100ml of water
(which may be an acceptable level of impurity, I don't know; but it's still not a very clean separation), a solution with 20g of NaCl dissolved per
100ml of water will dissolve a little over 7g of CuCl.
Some other chlorides also increase the solubility of CuCl (KCl and HCl among them).
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Random
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| Quote: Originally posted by bbartlog | One flaw in your proposed method is that sodium chloride solubilizes cuprous chloride. So while only 1.5g of CuCl will dissolve in 100ml of water
(which may be an acceptable level of impurity, I don't know; but it's still not a very clean separation), a solution with 20g of NaCl dissolved per
100ml of water will dissolve a little over 7g of CuCl.
Some other chlorides also increase the solubility of CuCl (KCl and HCl among them). |
Actually, solubility of CuCl is 0.0062 g/100 mL (20 °C). It is almost completely insoluble. Well then, the method can be adjusted to avoid NaCl.
1. When you have cupronickel chlorides solution, add baking soda and precipitate copper and nickel carbonates.
2. Filter and dry them.
3. Add HCl drop by drop to dissolve the carbonates, be careful not to use excess HCl.
Now, add metabisulfite solution and proceed as above, nickel carbonate should really be enough pure now.
I think this is perfected, only maybe nickel carbonyl method can produce it more pure.
I also read that nickel sulphide is soluble, while copper sulphide isn't so you can separate these two with sodium sulphide or H2S. But metabisulfite
way seems way easier and a lot less toxic.
[Edited on 18-2-2011 by Random]
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cyanureeves
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well random you should be able to plate out the copper because my carbonate now aceatae is contaminated with copper and i now have a pink pair of vice
grips and dikes.i used a nickel anode and hopefully i will plate out all the copper because it bubbles great without even hooking up the juice. but i
cheated on the vinegar by adding a bit of kodak bath stop acetic aacid.maybe if you use a s.steal anode or welding rod but no more copper for anode.i
never could plate copper on carbon steal.darn copper! nickel plating is so begginer friendly too.
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Random
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Though, it's a lot easier if you separate them chemically, though ss anode should get oxidized too.
I actually again made mistake, maybe dissolving cupronickel carbonates in vinegar and then treating them with metabisulfite would work better.
Just, does someone know solubiility data for copper (I) acetate and can nickel (II) acetate be reduced too with SO2 to form insoluble compound? What
is also the solubility data for copper (II) and copper (I) sulfites and nickel sulfites?
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