Sciencemadness Discussion Board

Nickel Nitrate fail

fx-991ex - 11-6-2023 at 11:02

I put some pre 2000 canadian nickel quarter into H2SO4, added some 20% H2O2 because it was too slow.
2 piece of 5g Ni + 5ml H2SO4 and about 10-15 drop of 20% H2O2

It was still very slow so i added some 2.5g KNO3. It really did help dissolve more of it and made a green sln.
1.267g of Ni dissolved into the acid.

I went ahead and added some KOH to remove the excess H2SO4 with hope to crystallize out K2SO4 leaving behind a green solution of Ni(NO3)2.
All i got is a blue salt which i though was NiSO4 from the lack of NO3 ion.

I still went ahead and added stoichiometric amount 1.267g of KNO3 + an excess of 10% to make sure all of the NiSO4 convert to Ni(NO3)2 and for the slight loss to NO2 gas.

But it did nothing, am still left with a blue salt and a clear solution(so that blue salt is very insoluble).

Dont know if i made some complex like K2Ni2(SO4)3 or something else but well, i think i failed. I kept the blue salt underwater for now but ill probably dispose of it and distill some HNO3 to make the Ni(NO3)2.

Any idea what it could be and what can i do to turn it into Nitrate for NHN or to sulfate for electroplating? I didnt dry it in case its accidently energetic from the Nitrate but i doubt so.

ManyInterests - 11-6-2023 at 12:26

I can't help with sulfates, but there is someone else who made a thread on nickel sulfate. As for me, I can help you with nickel nitrate. I've made it multiple times. Albeit I use this forum as an open lab notes which means I often need to hunt for them! I will make another copy-paste here:

https://www.sciencemadness.org/whisper/viewthread.php?tid=15...
Quote:
I just want to report what happened in my first attempt at making Nickel Nitrate... it was very much a cartoon event! Thankfully I escaped unharmed and none of the equipment was harmed and I cleaned the spill.

I added 20 grams of nickel metal (cut into chips) and added around 6 ml of 35% hydrogen peroxide... but I didn't realize just what an effect adding the nitric acid to it would have (I used 30ml of 70%)... I had a small fountain of nitric acid fumes and liquid. I quickly put the thing down in my balcony and immediately poured large amounts of bicarbonate water. I had to wipe a lot of the spill by hand after and tried to collect as much of the nickel metal chips as I could. This was quite an event, but my only real loss is that I didn't have much nitric acid left. I had enough for one more synthesis of this kind. I had some more nickel metal chopped up and ready, so I used them. I added the nitric acid first, and I carefully put it below my reflux column first BEFORE (drop wise) adding around 2 or 3 ml of hydrogen peroxide. I nearly had another fountain event, but I quickly put it in the column and no spill occured.

Damn that was something! I put the small (100ml) boiling flask that I am using for this and putting that in a 1000ml beaker full of boiling water at 100C. It's not refluxing yet, but I hope it will. making nickel nitrate is an adventure!

I don't know how long it needs to be doing that in the hot water, but I hope I will be good in four hours or so.


Quote:
I didn't write it down, but I believe around 8 grams or so were fully reacted. The other bits have some tarnish on them, so I assume they were partially reacted, but not fully.

I am running another synthesis. I added 8 grams of the previously used nickel metal to 14 ml of nitric acid. I also added around 4ml of slighly diluted hydrogen peroxide (I put in 2.5ml of my 35% and added another 1.5 ml of water. It still reacted quite violently, but I was expecting it and well prepared for it).

I'm glad that at least the pH is good. You did tell me that the pH is important when it comes to NHN synthesis...

All I need now is to make some good hydrazine sulfate. I hope my next batch will be the last I will need to make.


Edit: Hydrazine question: I realize the answer might probably be no but... I am guessing that after making the hydrazine after adding the hydroxide, bleach, and urea/gelatin and heating for 5 minutes at 85C is not good enough, but can it be used immediately after the addition of hydrochloric acid and sulfuric acid?



Basically what you need is no sulfuric acid, that'll make nickel sulfate as far as I know. to make nickel nitrate, get some COLD azeotropic nitric acid (65-75% is fine) only a few drops of H2O2. The hydrogen peroxide is a catalyst and just helps to move things along.

I used a lot of nickel metal (I used nickel strips that I bought off amazon, and I cut them into little pieces before adding) and added the nitric acid to it. It will start to react immedaitely so be sure to be able to snap it on your reflux condenser immediately, you can drip the H2O2 from a pipette slowly and a bit later. Once you have all the reagents added, I used a beaker water bath to heat it to 100C and let it reflux for a few hours. After that I let it cool. you'll see some nice nickel crystals forming in the flask. I get them out of there by dissolving in them in minimal boiling water. I never tried to boil off the water, but it shouldn't be difficult to gently evaporate the water in a glass baking pan.

The reason why I use an excess of nickel is that it insures that all the nitric acid is used up, and therefore you don't need need to worry about cleaning the nickel nitrate of any nitric acid. The nickel metal pieces can be more easily removed.

B(a)P - 11-6-2023 at 15:24

What you have is a solution containing nickel, potassium, sulfate and nitrate ions.
The method that you have posted will not get you to nickel nitrate.
To isolate the nitrate from what you have you could try adding some barium nitrate to remove the sulfate, but you will still have potassium ions to contend with. Your best bet is to start from nickel metal and nitric acid as you propose.
With regard to plating I do not know what impact the potassium ions will have on the process, why not try on a piece of scrap and see what happens?
You could also add some potassium hydroxide or carbonate to isolate your nickel ions, then add nitric acid to your nickel carbonate/hydroxide precipitate once you have distilled your acid.

DraconicAcid - 11-6-2023 at 15:41

Quote: Originally posted by B(a)P  

You could also add some potassium hydroxide or carbonate to isolate your nickel ions, then add nitric acid to your nickel carbonate/hydroxide precipitate once you have distilled your acid.


That's the best way to get nickel nitrate out of what you've made.

fx-991ex - 13-6-2023 at 12:46

Thanks for the reply's.
Ill convert it to the hydroxide and react with acid once ill make it.
I used NaOH instead of KOH, is there a reason to use KOH?. i dont have alot of KOH and ido have alot of NaOH.

About HNO3 distillation(ive done it before, but i got myself a fabric mantle). Should i use stir bar/stirring or not? all the video on youtube dont use any stirring.
Last time i did it on an oil bath without stirring.
Just wondering for the foaming if it will help or make it worst, i think it will speed the distillation too right?

[Edited on 13-6-2023 by fx-991ex]

DraconicAcid - 13-6-2023 at 13:35

Quote: Originally posted by fx-991ex  
Thanks for the reply's.
Ill convert it to the hydroxide and react with acid once ill make it.
I used NaOH instead of KOH, is there a reason to use KOH?.


Either hydroxide should work equally well.

With nickel, I have found that the precipitate is often fine and unfilterable, and centrifuging works much better. YMMV.