Sciencemadness Discussion Board - Weird reaction, that produces spiky crystals.

Weird reaction, that produces spiky crystals.

MeshPL - 10-6-2016 at 10:42

Hello,
First of all, sorry for not putting any photos here. I did that at school, and I won't be able to photograf anything until monday due to the weekend.

I'll try describing what happend the best way I can.

I dissolved cupronickel coins in a mixture of H2O2 and acetic acid and later I added hydrochloric and nitric acids, just because the reaction was so slow.

The resulting solution was put in a test tube and diluted a bit. It was acidic. I added potassium sodium tartrate, just to see whether anything would percipitate. Nothing did, but mixture turned more blue.

Than I added a bunch of reducing agents, sodium thiosulphate and I think sodium sulphite and oxalic acid, just for giggles (and to see if any thing would percipitate). But noyhing happened.

A few days later, that is today, I found out that the mixture got lighter in colour and there were 3 gray, metallic-like "spiky balls" floating in a solution, nearly the diameter of the test tube.. There was also a piece of polycrystal resting on top of them, simmilar in colour, but rather irregular in shape.

What I think happened is:
The thiosulphate started hydrolysing, producing some sulphide ions.
Tartrate was complexing most of the Cu and Ni, making them soluble despite some sulfides hanging around.
A little of the free Cu an Ni and sulfides were percipitating slowly resulting in a formation of well formed, bizarre structures.

Again sorry for the lack of photos, but I had no time to do them today.

I will try replicating results in near future.

[Edited on 10-6-2016 by MeshPL]

Cryolite - 10-6-2016 at 11:46

Did you characterize the crystals? Did they conduct electricity? Did they release a sulfurous smell when dilute HCl was dripped on them? What happens when the crystals are heated strongly in a test tube? Did you take a flame color?

MeshPL - 10-6-2016 at 12:00

I had no time to do so. But thanks for the suggestions, on what to check.

As I said, I had no time even to do photos today (yay, school where you do a bunch of useless stuff instead of science).

aga - 10-6-2016 at 12:15

The photos sound like they will be awesome !

Fortunately we're patient here, and a few days wait won't spoil the 'mazement.

Edit:

Here's some spiky crystals to be going along with

Sodium sulphate by-product from making some glacial acetic acid via the 'normal' route with sodium acetate and conc H₂SO₄.

The Green colour is due to idiocy and trying to reduce the water content of a strong sulphuric acid-containing solution in a stainless steel pot.

Fizzy Fizzy fizz and the pot is now stained.

[Edited on 10-6-2016 by aga]

MeshPL - 13-6-2016 at 07:03

So here they are. They don't look exactly as I remembered them, but they look quite cool anyway. This only stresses the need to document what we do.

Sorry for the photos being rotated the weird way.

I will try to analyse the crystals soon.

[Edited on 13-6-2016 by MeshPL]

phlogiston - 13-6-2016 at 07:36

If you are really interested in finding out more about these crystals, including what they might be, you should probably start with finding and documenting a reliable protocol for producing them. You added unknown amounts of many different compounds, some of which you may or may not have added.

aga - 13-6-2016 at 08:01

They look really quite cool !

phlogiston is right though - without measuring stuff, nobody (not even you) can easily re-create those crystals.

Try it again and weigh everything before you start.

Add random amounts of whatever, then weigh it all afterwards to see exactly how much you used of each reagent.

NEMO-Chemistry - 13-6-2016 at 08:47

They do look really cool! I am looking for unusual crystals so i hope you follow it up, if you do can you post what you try please? I would like to have a go at reproducing them.

I know your not meant to bung things into a tube, but sometimes you you do get lucky

, would look cool in a collection but even better if you work out what they are.

Forgive the edits!

I wanted to do some digging about to see if i could find anything that matched your crystals, keep in mind i am a noob please.

You mentioned copper nickle coins so i assume these are American coins? My thinking goes something like this.

You know you have nickel and copper for sure, you also used acetic acid first, then added hydrogen peroxide. So i started looking for acetate pictures of nickle and copper, i think i have found the shape that matches but not the colour.

The picture came from a google search, but the page it links too i could find the crystal. This is a screen shot of the search page and a link to the page the pic relates too.

If you click on the pic you can read it mentions dropping a sodium acetate crystal into something. I tried to find the pic and information on the linked page but failed. here is the page it linked too
http://www.fphoto.com/

I will edit again if i find anything else, the colour might be a mix of nickle copper acetate? all speculation but might be useful to you

[Edited on 13-6-2016 by NEMO-Chemistry]

Edit 2

Maybe copper frost crystals?? I found this from this page, take a look at the video.

http://www.waynesthisandthat.com/crystals.htm#exotic

[Edited on 13-6-2016 by NEMO-Chemistry]

NEMO-Chemistry - 13-6-2016 at 09:34

Copper chloride looks like another possible??

I dont have any nickle or American coins, but i can try some copper ones out. The chloride I mentioned because of the Hcl you added.

MeshPL - 13-6-2016 at 10:34

For coins, I used silver PLN coins, which are 25% Ni and 75% Cu.

The "coin solution" is highly acidic and contains acetates, nitrates and chlorides as well as Cu and Ni, that's all that matters. I think I'll need to get a bunch of test tubes and add controlled amounts of reagents to each tube, along with Cu/Ni solution. And take notes.

morsagh - 13-6-2016 at 11:27

I agree with that sulphide, but that thing with tartarate... you should filtrate off and add to crystal Ca2+ to be sure it isn´t oxalate coordination (spiky crystals with copper, don´t know about nickel but their coordination chemistry is quite similiar).

DraconicAcid - 13-6-2016 at 11:53

Copper and nickel chloride, acetates and nitrates are going to be very soluble, and unlikely to crystallize. Tartrates may be a possibility.

NEMO-Chemistry - 13-6-2016 at 12:33

Quote: Originally posted by DraconicAcid

Copper and nickel chloride, acetates and nitrates are going to be very soluble, and unlikely to crystallize. Tartrates may be a possibility.

I have some tartaric acid some will do some test tubes with that.
Thanks for the input,personally i would really like some of the crystals.

myristicinaldehyde - 13-6-2016 at 13:36

If it helps, I made a similar Cu-Ni solution (but more Ni), neutralized it with sodium carbonate, and left the leftover solution to dry. Needles were seen in the residue- so I guess sodium acetate crystals, with the reduced Ni/Cu trapped in it?

aga - 13-6-2016 at 14:21

OK. I'm getting pissed off by the utter crap now, much more so than the small quantity of entertaining Politics we had here until a few months ago.

This forum is generally assumed to be for Chemistry.

Can you all quit the "i added some kryptonite then zapped that with some star dust and made a bag of bosons" garbage.

Post at least a procedure that a fellow amateur scientist can follow, or get another hobby.

Preferrably not the "let's irritate amateur Chemists to the point that they Combust" hobby, which seems quite popular, here.

Just say HOW F**KING MUCH kryptonite you used, and how much gold dust, and what the yeild of bosons was.

It is not difficult to go from (useless, unscientific):-

'wow that was amazing'

to (repeatable, scientific)

'wow ! try this: add 14.6g of kryptonite to 12.2 g fairy dust in 12.6 ml of cat piss to get a mol of bozos'.

Just measure things and tell how/when you did it.

It's not Rocket Science (yet) just basic communication.

[Edited on 13-6-2016 by aga]

MeshPL - 18-6-2016 at 10:44

Ok, here are some facts I know about the liquid, which remained above crystals:
-it is slightly basic. In fact it contains ammonia. Yay! Another reagent I may/must have put in there.
-as you might guess, it contains very little copper, since copper amine complex is brightly coloured.
-adding some CuSO4 produces a greenish (!) blue solution, indicating the presence of ion which produces a grren colour with copper. Probably chloride.
I tried replicating results, yet I'm not very succesful. I'll post more when I know more.

NEMO-Chemistry - 18-6-2016 at 11:36

Quote: Originally posted by aga

OK. I'm getting pissed off by the utter crap now, much more so than the small quantity of entertaining Politics we had here until a few months ago.

This forum is generally assumed to be for Chemistry.

Can you all quit the "i added some kryptonite then zapped that with some star dust and made a bag of bosons" garbage.

Post at least a procedure that a fellow amateur scientist can follow, or get another hobby.

Preferrably not the "let's irritate amateur Chemists to the point that they Combust" hobby, which seems quite popular, here.

Just say HOW F**KING MUCH kryptonite you used, and how much gold dust, and what the yeild of bosons was.

It is not difficult to go from (useless, unscientific):-

'wow that was amazing'

to (repeatable, scientific)

'wow ! try this: add 14.6g of kryptonite to 12.2 g fairy dust in 12.6 ml of cat piss to get a mol of bozos'.

Just measure things and tell how/when you did it.

It's not Rocket Science (yet) just basic communication.

[Edited on 13-6-2016 by aga]

Thats a bit out of order, the guy wanted some help working out how and what he got, yes ok super humans always write it down, but sometimes others dont.

Why start getting all out of shape? It really does make people like myself uncomfortable, you dont have to read it if you dont like it.

He gave as much info as he had, the rest is kind of detective work. Some people like that, ok i am new here but surely there is room for people who make mistakes and dont write the whole thing down!

Maybe you should do a template and all posts that dont conform get destroyed?

Mesh so far i have got nothing like yours using tartrate, i only get weekends to actually do stuff so progress is slow. I will try some acetates after i finish distilling some more vinegar.

Not sure i will get time this weekend as i been making copper nitrate/sulphate/carbonate etc

.

Have the crystals changed colour at all?

No nickle but i might also try with zinc?? At the moment i am just using copper.

[Edited on 18-6-2016 by NEMO-Chemistry]

myristicinaldehyde - 18-6-2016 at 12:05

Can you filter out the crystals? I am curious to see if they are metal or not, I can't really tell from the photos. I hope it turns out to be repeatable.

Aga, if your post was directed at mine, I prepared the soultion the sma e way OP did sans HCl, then added carbonate until no bubbling was observed. A total of 10 mL of acetate solution was used.

MeshPL - 18-6-2016 at 12:22

Yes, on Monday I will do tests on crystals. I will try to do a flame test, put one in sulfuric acid, the other in nitric, maybe one in conc. NaOH? Once I get them dissolved I'll do some tests.. oh and I will check for the sulfurous smell produced.

I really think theese crystals are some kind of sulfide... but who knows? Actually, since there is very little copper in solution, enough for the intensly coloured tetraamina complex to form only a faint colour, they must contain most of the copper, which was present in solution. And therfore the substance there is probably very insoluble.

[Edited on 18-6-2016 by MeshPL]

PHILOU Zrealone - 19-6-2016 at 08:39

Quote: Originally posted by MeshPL

Ok, here are some facts I know about the liquid, which remained above crystals:
-it is slightly basic. In fact it contains ammonia. Yay! Another reagent I may/must have put in there.
-as you might guess, it contains very little copper, since copper amine complex is brightly coloured.
-adding some CuSO4 produces a greenish (!) blue solution, indicating the presence of ion which produces a grren colour with copper. Probably chloride.
I tried replicating results, yet I'm not very succesful. I'll post more when I know more.

Nope!
No NH3 inthere!
NH3 (NH4OH) + Ni(2+) also makes a deep blue complex, just like copper does!

MeshPL - 20-6-2016 at 00:43

More tests were done. What I determined is:
-crystals react with acids to produce insoluble, orange percipitate.
-crystals react simmilarily with bases, but to a lesser extent
-crystals dissolve in ammonia to form blue solution
-crystals contain copper-determined with a flame test