Sciencemadness Discussion Board - Nickel salts and compounds

Nickel salts and compounds

NEMO-Chemistry - 1-1-2018 at 09:08

I have always wanted to do some Nickel chemistry. Getting hold of Nickel isnt always easy though, i know some older coins were made from it, but i dont know which!!

in the end I paid £20 for 280g Nickel shavings, these are 94% pure, most the impurities are Iron (3.4%) and Copper (1.4%), which makes me think these came from coins originally?

Anyway, anyone got some suggestions on what salts,complexes or compounds i could make that are interesting?

I guess the first one should be dissolve some in HCl and make the chloride?

PirateDocBrown - 1-1-2018 at 09:59

Your pre-2011 5- and 10- pence coins are 25% Ni, 75% Cu. You should be able to separate those to get all the Ni you need, and at a good price.

Radium212 - 1-1-2018 at 10:04

I think sulphuric acid also works.

The Austrian Scientist - 1-1-2018 at 10:14

Ni does not disolve in HCl. You could use dilute HNO3 or ad a bit of H2O2 to the HCl to disolve it.

Here are some Ideas for compounds:

[Ni(NH3)6]Cl2 or (NO3)2
[Ni(N2H4)3](NO3)2
Ni(OAc)2

woelen - 1-1-2018 at 10:26

It's a pity you paid that amount of money for such impure nickel. The impurities stronly interfere in complex formation complexes. Both iron and copper form strongly colored complexes with many coordinating agents.

Much better to buy pure nickel metal (e.g. element samples, or powdered nickel) at better than 99.5% purity. You also can buy nickel oxide. You can easily dissolve that in hydrochloric acid to get nickel chloride solutions.

--------------------------------

Interesting nickel complexes to make are the ammonia complex (hexammine nickel(II)), periodato complexes, ethylene diamine complexes. All of these complexes can be crystallized easily and they have vibrant colors.

FlaskBreaker - 1-1-2018 at 10:41

Nickel Oxalate is a neat compound. You need basic nickel carbonate and oxalic acid. If you heat it up enough, It will create very fine nickel powder, which is pyrophoric in air. (If finely dispersed enough.)

I can also confirm that HCl will not dissolve nickel. You need a strongly oxidizing acid or a solution of an oxidizer and acid. For example, a solution of H₂O₂ and acetic acid will make nickel acetate, while acetic acid alone will not do this.

NEMO-Chemistry - 1-1-2018 at 10:53

Thank you for the suggestions!!

I will look out for the coins

. At the time i ordered the Nickel i couldnt find pure stuff at a reasonable price.

I have Nitric acid, so maybe I will start there and try and purify the Nickel I have. I am still waiting for my Oxalic acid!! Above 10% its extremely hard to get now in the UK (legally).

Some interesting ideas for salts though. I will do some research and see if I can get this to a better purity. Or I will melt it for Anodes or some other electro chem experiments.

NEMO-Chemistry - 1-1-2018 at 11:07

Well that was quick!!

http://pubs.acs.org/doi/abs/10.1021/i560113a012?journalCode=...

from that paper it looks like, oxalic Acid then Ammonium Hydroxide should separate out the Iron, I have a fairly good list of the impurities and % of each (this is what made me think the original source was coins). It might be interesting to experiment with purifying the Nickel after all!

Sometimes buying is better than making, i dont need the Nickel for anything specific. So this is one of those times where the learning out weighs the cost. It seems alot can be learnt from purifying this, if i cant get it pure then i will buy some for the complexes etc.

I admit we went on a spending frenzy with equipment and chemicals, having waited nearly 6 months to spend our savings, when the time came we got carried away

.

The Vanadium Pentoxide was a huge mistake! I wanted a powerful desiccant and mixed the names up!! So i ended up spending over £120 on 1KG of Vanadium Pentoxide!! Then discovered it wasnt actually what I wanted lol.

Dont be surprised to see it pop up on ebay soon

. I will keep some back for experiments, but probably only around 50g, so just 950g to get rid of

The other mistake was not having my glasses on, i use alot of Magnesium carbonate, so i ordered 2KG of it, only when it turned up, it turns out I ordered Magnesium SORBATE!

Absolutely no idea what I am going to use that for! Lesson for the day..... Stop buying as soon as you feel the spending frenzy taking hold lol.

[Edited on 1-1-2018 by NEMO-Chemistry]

[Edited on 1-1-2018 by NEMO-Chemistry]

NEMO-Chemistry - 1-1-2018 at 11:25

I also notice Ferric Chloride dissolves Nickel really fast, i have some for etching pcb boards (40 Baume i think), then the Nickel and Iron can be separated by use of a soluble ammine complex with the nickel.

http://lanthanumkchemistry.over-blog.com/article-the-dissolv...

Anyone got any ideas for a suitable and reach ammine to use?

Forget it! I was in stupid mode! Obviously adding Ammonia would give...... DOH

[Edited on 1-1-2018 by NEMO-Chemistry]

NEMO-Chemistry - 1-1-2018 at 14:02

agas lucky day! I have some pics, but first two confessions...
Last night a couple of friends of my mum came around for new year. Being 17 1/2 i have NEVER tasted Alcohol!! Apart from pain killers etc, i havnt touched it before because I hate even the smell of it.

My mums friends decided last night would be the perfect time to give me my first drink!! So i had Champagne for the first time! A glass of 2008 vintage Moet (YUCK!), and a forgotten number of glasses, of Vintage Bollinger Champagne (MMmmmm man that stuff is so buttery and delicious!!).

So today I am a bit messed up!

Confession 2

Because of confession 1, i stuffed up the first experiment from above lol. I thought I would try dissolving the Nickel in Ferric Chloride, i totally forgot the acidified part though! I also added Ammonium Chloride!

I am sure the ammonium chloride I used has had it though, no ammonia smell and it seems damp. Its kept in the correct containers but alot of my chems seem to get damp. I am thinking of keeping them in a large food type plastic container (each in the proper container, but inside the larger food one), I will put the desiccator packets in there as well and tape the lids shut!).

Anyway I added some (1.2ml) of 32% ammonia to it. its sitting stiring away now, but obviously all i got is brown mud and Nickel flakes!

Just for accuracy
~0.50g Nickel chips (found another container, these are 99.09% pure) impurities are Ni 99.09% Fe 0.28%,Mn 0.24%,C 0.10%

20ml water with 0.77g Ammonium Chloride (this could be no good as above)

~1.2ml 32% Ammonia

~ 3ml 39B Ferric Chloride

Pics below, I will obviously do this again properly tomorrow, once the headache has gone

.

Edit
Actually i am wrong about the ferric chloride! its 40-42% with 0.1% HCl in it, so I guess it was slightly acidified

S.C. Wack - 1-1-2018 at 15:03

There should be affordable bags of 55-81 CAN nickels for sale still; it's only .999. H with Ni and B or Al is useful in certain reductions. Precipitated nickel is also interesting.

[Edited on 1-1-2018 by S.C. Wack]

NEMO-Chemistry - 1-1-2018 at 15:13

Quote: Originally posted by S.C. Wack

There should be affordable bags of 55-81 CAN nickels for sale still; it's only .999. H with Ni and B or Al is useful in certain reductions.

Thx for that, are they still legal tender? I wonder what rules (technically) you would be breaking by importing currency into the uk?? There is bound to be some bloody rule

.

Seriously though thanks, I will keep an eye out for some, i did find a container of 200g 99.01% Nickel flakes at the back of a cupboard, i completely forgot i had it!! Its been there a while now.

S.C. Wack - 1-1-2018 at 16:02

Of course they're legal. But wait, there's more. NL and FR also made .999 Ni coinage.
10 Cent (1948-2001)
25 Cent (1948-2001)
1 Guilder (1967-2001)
2.5 Guilder (1969-2001)
5 Guilder (1987-2001)
1/2 Franc (1966 - 2000)
1 Franc (1960 - 2000)
2 Franc (1979 - 2000)

NEMO-Chemistry - 1-1-2018 at 17:02

Quote: Originally posted by S.C. Wack

Of course they're legal. But wait, there's more. NL and FR also made .999 Ni coinage.
10 Cent (1948-2001)
25 Cent (1948-2001)
1 Guilder (1967-2001)
2.5 Guilder (1969-2001)
5 Guilder (1987-2001)
1/2 Franc (1966 - 2000)
1 Franc (1960 - 2000)
2 Franc (1979 - 2000)

I couldnt find quantities on UK ebay, also the dates for Canadian coins with Nickel were slightly different in wikipedia (not that wiki is the be all and end all lol).

Do you have a link from where you saw the bags for sale? I can follow links to ebay in the states etc, but I dont seem to be able to bring a page up on its own, i click ebay and get uk ebay each time.

Thanks alot for the list! thats really helpful.

EDIT
its ok i found a way

cant find the Canadian bags though. might have lost my ebay FOO today lol

[Edited on 2-1-2018 by NEMO-Chemistry]

aga - 1-1-2018 at 23:39

Woohoo ! Photos ! Yay !

Keep them coming NEMO.

Ebay has some stuff that *might* be as described :-
https://www.ebay.co.uk/itm/7M-8mmx-0-1mm-Pure-Ni-Plate-Nicke...

Other similar items say 'Plated' so it would be best to contact the seller to confirm if those are solid Ni.

NEMO-Chemistry - 2-1-2018 at 05:17

Quote: Originally posted by aga

Woohoo ! Photos ! Yay !

Keep them coming NEMO.

Ebay has some stuff that *might* be as described :-
https://www.ebay.co.uk/itm/7M-8mmx-0-1mm-Pure-Ni-Plate-Nicke...

Other similar items say 'Plated' so it would be best to contact the seller to confirm if those are solid Ni.

Hi praise indeed! this post has been framed!
Thx aga, but i have Nickel now, actually i had some good stuff all along! I had totally forgotten about it!

My defense was my first ever hangover! never again for sure!! Seems like people are collecting Nickel as an alternative to silver hoarding??? Seems odd to me!

I got some stuff coming tomorrow, so got to make room today. I hope to do some chemistry later though. I dont have any yet but, I got to thinking about the fish and chip process. Wonder if it dissolves Nickel? Turns out very little actually dissolves it easily.

Apparently Nicker (maybe just the salts??) is carcinogenic! Bit odd seeing as so many coins contained it. Obviously i am looking for war time Nickels! It seems they cut the Nickel in them and replaced with silver, mainly because they needed the Nickel at the time!

Right back to the lab

....
Its great being able to take pics! No expensive camera to fret over lol

NEMO-Chemistry - 3-1-2018 at 02:55

This stuff refuses point blank to dissolve!! I have thrown everything at it. Time to get serious and unleash the heat and heavy duty chems!! I dont have Peroxide at the moment, but i still want to give Vit C a go first.

woelen - 3-1-2018 at 04:01

@NEMO: I can donate some dutch coins. They are appr. 99.5% nickel, the balance being mostly tin. I made solutions of nickel nitrate from these. I can send guldens, kwartjes, dubbeltjes. I keep some of these coins around, just as collector's items, but I have quite a few bad looking, mechanically damaged coins. These of course still are perfectly fine for their nickel contents. Just polish them with coarse sand or put them in acid for a few minutes to get rid of the outer damaged layer and then transfer them to a clean mix of conc. HNO3 and conc. HCl to get them dissolved for making a nearly pure solution of nickel(II).

From experiments with dutch coins I know that nickel metal indeed does not dissolve easily in acids. You really need an oxidizing solution to dissolve them. Once you do that, you get a nice bright green solution of nickel(II).

[Edited on 3-1-18 by woelen]

woelen - 3-1-2018 at 04:13

Quote: Originally posted by NEMO-Chemistry

The Vanadium Pentoxide was a huge mistake! I wanted a powerful desiccant and mixed the names up!! So i ended up spending over £120 on 1KG of Vanadium Pentoxide!! Then discovered it wasnt actually what I wanted lol.

Dont be surprised to see it pop up on ebay soon

. I will keep some back for experiments, but probably only around 50g, so just 950g to get rid of

Keep a little more of it. You can make quite a few very interesting salts of it.
One interesting compound is sodium orthovanadate, Na3VO4. You can make this by dissolving it in as little as possible of a solution of NaOH and allowing this to evaporate to dryness.
Another interesting one is making ammonium metavanadate. You can dissolve V2O5 in moderately concentrated ammonia to make this. Use excess ammonia and allow to evaporate to dryness.

Most interesting is making of deep blue vanadyl compounds. The vanadyl ion, VO(2+), is a beautiful blue (like copper(II) ions, but somewhat brighter and more strongly colored). You can make vanadyl compounds by dissolving sodium orthovanadate in water, and then acidifying this compound until an acidic yellow solution of pervanadyl ion is obtained, VO2(+) and then add sodium metabisulfitein order to convert the pervanadyl to vanadyl. If you want to synthesize vanadyl sulfate, then you can best add V2O5 to dilute sulphuric acid and bubble sulphur dioxide through this and have it reduced in that way. This reaction is slow though. Maybe you can use formic acid or oxalic acid as reductor, but I have no personal experience with that.

Rhodanide - 3-1-2018 at 08:22

Quote: Originally posted by NEMO-Chemistry

I have always wanted to do some Nickel chemistry. Getting hold of Nickel isnt always easy though, i know some older coins were made from it, but i dont know which!!

in the end I paid £20 for 280g Nickel shavings, these are 94% pure, most the impurities are Iron (3.4%) and Copper (1.4%), which makes me think these came from coins originally?

Anyway, anyone got some suggestions on what salts,complexes or compounds i could make that are interesting?

I guess the first one should be dissolve some in HCl and make the chloride?

Hexaammine Nickel (II) Chloride is also a cool reaction. Where I live, it tends to get cold during the night (usually in the negatives) which lends itself to easier precipitation of the Ammine. All you need to do is dissolve NiCl2 in aqueous Ammonia, which will form a very deep purple-blue solution. If your solution is cooled sufficiently after this, you should start to see the purple Ammine complex precipitate out as tiny, needle-like crystals. If you filter, dry, then store it, it can be isolated as the pure powder. Don't leave it in warm air for a long while, though. It can decompose that way.

MrHomeScientist - 3-1-2018 at 08:35

I did that reaction in one of my videos - you can also crash the solid out by adding (lots of) acetone! Not pretty crystals like the slow method, but beautiful purple nonetheless.

NEMO-Chemistry - 3-1-2018 at 08:39

Thx guys, those are really good ideas!!

I will break out the Nitric acid and HCl later and get some the nickel in solution

. The Vanadium Chemistry sounds interesting, i got a large amount of sodium Hydroxide prills.

Plenty to think about now!

Rhodanide - 3-1-2018 at 11:36

Quote: Originally posted by MrHomeScientist

I did that reaction in one of my videos - you can also crash the solid out by adding (lots of) acetone! Not pretty crystals like the slow method, but beautiful purple nonetheless.

Yeah, but I like the nice crystals as opposed to a powder. Also, wouldn't the reaction make Ammonium Chloride as well? (and wouldn't it co-precipitate?)

[Edited on 3-1-2018 by Tetra]

[Edited on 3-1-2018 by Tetra]

MrHomeScientist - 3-1-2018 at 11:50

Hm good question. Wiki states NH<sub>4</sub>Cl is "slightly soluble" in acetone, so you might get away with washing the product several times with the solvent. But it will decompose over time in air as the ammonia escapes and revert back to green nickel(II) chloride, so it might not last long enough to wash!
I never noticed extra crystals; the whole thing is a nice uniform purple (NH<sub>4</sub>Cl could be embedded in it though, I guess).

NEMO-Chemistry - 3-1-2018 at 19:32

What about Iodine and Nickel with a drop of water? I am thinking heat nickel in a tube and them pass iodine vapor over it

NEMO-Chemistry - 4-1-2018 at 10:02

Well the answer is....Nothing! I got a cracked tube but thats about it, i honestly thought hot Nickel and iodine would react. Hmmm

I cant make any Iodine monochloride at the moment, i bet it would react with that

woelen - 4-1-2018 at 23:41

Maybe if you use powdered metal, the reaction works better.
Nickel has a tendency to form a thin protective layer which prevents further reaction. For this reason it is even possible to store fluorine in a nickel container. The formed layer of NiF2 protects the underlying metal. This almost certainly also is true for NiCl2 and NiBr2. Maybe it also is the case for NiI2, but I can imagine that this halide is not sufficiently stable and simply decomposes on heating. I have no personal experience with that though.

NEMO-Chemistry - 5-1-2018 at 02:52

Quote: Originally posted by woelen

Maybe if you use powdered metal, the reaction works better.
Nickel has a tendency to form a thin protective layer which prevents further reaction. For this reason it is even possible to store fluorine in a nickel container. The formed layer of NiF2 protects the underlying metal. This almost certainly also is true for NiCl2 and NiBr2. Maybe it also is the case for NiI2, but I can imagine that this halide is not sufficiently stable and simply decomposes on heating. I have no personal experience with that though.

I closed the tube with a heavy glass thimble on top, i had a tiny amount of water in the tube. Looking at it afterwards something did react a little and I also saw a few red drips.

Some of the powder is alot finer than the rest, i will separate this out. I could do with a decent ball mill! That way I can keep the bulk in larger flakes and the mill it as I need it,

I am also storing it in a pretty airtight container. I will try again later

DraconicAcid - 5-1-2018 at 11:25

You might also find that it works better in a solvent that will dissolve iodine (I've reacted zinc with iodine using methanol as the solvent, and have vague memories of trying it with iron and possibly nickel).

NEMO-Chemistry - 5-1-2018 at 14:14

Quote: Originally posted by DraconicAcid

You might also find that it works better in a solvent that will dissolve iodine (I've reacted zinc with iodine using methanol as the solvent, and have vague memories of trying it with iron and possibly nickel).

That I can go do now! I have Methanol handy. A couple of coffee things i want to do as well. Then i got to clear the lab up!

Really i should get it sorted first, i got the inspection coming up. This is where a dishwasher for the lab would be cool.

Not good! Maybe its way too cold in the lab, going to have a clean and tidy and reflux this.

[Edited on 5-1-2018 by NEMO-Chemistry]