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Author: Subject: Dissolving Calcium ammonium nitrate in Ethanol
Kobold vor NH4
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[*] posted on 27-8-2019 at 19:20
Dissolving Calcium ammonium nitrate in Ethanol


Hello everyone!
After I saw the solubility of Ca(NO3)2 and Nh4NO3 in EtOH, I thought I would try it as a method of separation, however when I put the CAN in the ethanol, it started giving off gas of some kind, and when I stoppered the tube, the bubbles stopped and when I released it, it started bubbling again. Anyone know what's going on? Or is this something that happens with some compounds?
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Ubya
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[*] posted on 28-8-2019 at 07:03


big bubbles or small bubbles? it could just be air trapped in the prills, by dissolving them air is escaping as bubbles




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Kobold vor NH4
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[*] posted on 28-8-2019 at 18:25


Hello Ubya!
They were small bubbles, I'll try powdering it and see if there is any difference.
Would you want to see any pictures?

EDIT: the bubbling was the same with the powder, it took about 10 ~ 15 minutes to stop, and for a second heaver later to appear, which, when removed and replaced with more ethanol, continued to bubble.
The second layer also appeared in the first test.
Also the ethanol I used was diggers methylated spirits UN 1170 (so it isn't pure, but according a post on here, it was something like denatonium benzoate).


[Edited on 29-8-2019 by Kobold vor NH4]




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Corrosive Joeseph
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[*] posted on 28-8-2019 at 22:24


Quote: Originally posted by Kobold vor NH4  

After I saw the solubility of Ca(NO3)2 and Nh4NO3 in EtOH


Any chance you could post these numbers..........?


/CJ




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Kobold vor NH4
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[*] posted on 28-8-2019 at 22:50


Sure!

Calcium nitrate: 51.4 g/100g
( https://en.wikipedia.org/wiki/Calcium_nitrate )

Ammonium nitrate 3.8 g/78g
( https://pubchem.ncbi.nlm.nih.gov/compound/Ammonium-nitrate#s... )




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[*] posted on 29-8-2019 at 12:50


Do you have the NPK number for your nitrate? And what does it look like? I've seen this name coming by before but still don't understand what the stuff is really, although I have an idea.
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[*] posted on 29-8-2019 at 13:57


In my experience CAN is more like a mixture of calcium carbonate mixed with ammonium nitrate. Dissolved in water the fines (mainly CaCO3) are allowed to settle then the supernatant is filtered (recycling the initial turbid filtrate). At this point there is little calcium, but still some left in the solution. I believe this because when you treat that solution with potassium carbonate only a small amount of insolubles (CaCO3) are formed. And after hot filtration one can obtain pure KNO3 by crystallization.

So perhaps those bubbles are CO2. Apparently ethanol dissolves calcium nitrate but not ammonium. If so that would push reaction between calcium carbonate and ammonium nitrate to the calcium nitrate + ammonia + CO2 side.

Would be a neat trick if that also works for the heavier earth alkali metals, say strontium and barium. Kohbold, do you have solubility data for strontium or barium nitrate in ethanol?
Edit:
Cursory search show they are alot less soluble than ammonium nitrate. :(

[Edited on 29-8-2019 by Sigmatropic]
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Kobold vor NH4
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[*] posted on 29-8-2019 at 16:15


@Tsjerk
No, the only things written on bag is "calcium nitrate, 1KG", they are prilled and off~white in color.
Tests that I have done on it show it is a mixture of calcium nitrate and ammonium nitrate.

@Sigmatropic
When I first got the stuff, I made KNO3 with it, using KOH because I had a kilo or two of it.
two things happened: 1 a white precipitate appeared, and it got quite thick. 2 the smell of ammonia appeared instantly and strongly. But your hypothesis sounds quite plausible, I plan on bubbling ammonia through the CAN to get AN, I'll mix some solid AN with some CA(CO3)2 and see If it bubbles, I'll also try it with just CN.
About the Heavier alkali metals, those are the sort of ideas that fill my mind when i find info like this,
but apparently barium metal is soluble in ethanol.
https://www.nap.edu/read/11778/chapter/5

EDIT: Adding conc. Alkali hydroxides to solid CAN looks like a good way to get both ammonia gas and alkali nitrates, if CAN is the only nitrate you can get (like me), that is.

[Edited on 30-8-2019 by Kobold vor NH4]




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[*] posted on 29-8-2019 at 21:02


You might want to try using methanol. I've done many purifications of Ca(NO3)2 using methanol (I found it at race tracks/drag strips - they often sell it at ~$4/gal and it's pure - make sure to get the stuff w/o engine lube added). I think the solubility was close to about 180g/100ml of methanol.

I'd suggest dehydrating the nitrate first as it is usually the tetrahydrate. You won't get as much dissolved but it gives a better product in the end.

I've also tried methanol and ethanol to clean up what was supposed to be ammonia nitrate (cold packs) but it turned out to be CAN. Both did a very poor job of dissolving the CAN, though it did do a better job when heat was applied.

There seems to be a problem in many places that sell generic Ca(NO3)2 as I've found it to be CAN almost all the time. The only brand I found to be real Ca(NO3)2 is the Norweigan and Israeli fertilizer manufacturers (I forget the company names).

I've never had any of these release bubbles upon dissolving unless maybe when adding something like a base (KOH, NaOH, Na2CO3) where ammonia is released but that is very apparent by the smell. Maybe your alcohol has some acid in it and is reacting with the CaCO3 that is in the nitrate?

[Edited on 8-30-2019 by RogueRose]
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[*] posted on 30-8-2019 at 00:53


@RougeRose
There is a racetrack in the town near me, but a look at the website doesn't say anything about products for sale, so I guess I'll need to go in person to see if they sell Methanol. Might do that sometime in the future (not too keen on methanol and is toxicity).

Here's a picture.
This was taken a few minutes after addition of EtOH.
All of those white specks were moving up.

T.jpg - 454kB

[Edited on 30-8-2019 by Kobold vor NH4]

[Edited on 30-8-2019 by Kobold vor NH4]




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[*] posted on 30-8-2019 at 04:11


Quote: Originally posted by Kobold vor NH4  
@Tsjerk
No, the only things written on bag is "calcium nitrate, 1KG", they are prilled and off~white in color.
Tests that I have done on it show it is a mixture of calcium nitrate and ammonium nitrate.
[Edited on 30-8-2019 by Kobold vor NH4]


I used to find something called "calc ammon nitrate" in stores sold as fertilizer. It was 85% ammonium nitrate and 15% brown calcium carbonate. It was perfect to get ammonium nitrate from by dissolving and decanting.

Your stuff doesn't sound similar and indeed to be a mix of calcium nitrate and ammonium nitrate. Sounds fine as a nitrate source though!

You can get ammonium nitrate by adding ammonium sulfate by precipitation of the calcium sulfate.

Ammonium nitrate is a nice starting point for other nitrates by reacting it with metal hydroxides, yielding ammonia gas in the process.

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[*] posted on 30-8-2019 at 10:14


The fertilizer grade of calcium nitrate has an approximate composition 5Ca(NO3)2.NH4NO3·10H2O. I could not figure out how to separate a pure calcium nitrate. The concentrated solutions of this fertilizer turn to syrupy liquid instead of crystalize.
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[*] posted on 30-8-2019 at 10:24


Quote: Originally posted by egret  
The fertilizer grade of calcium nitrate has an approximate composition 5Ca(NO3)2.NH4NO3·10H2O. I could not figure out how to separate a pure calcium nitrate. The concentrated solutions of this fertilizer turn to syrupy liquid instead of crystalize.


Calcium nitrate is extremely soluble in water (the tetrahydrate is actually used as a low-temperature ionic liquid). You could get rid of the ammonium nitrate by adding calcium hydroxide, but you'll want to figure out what solvent to crystallize the calcium nitrate from first.




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[*] posted on 30-8-2019 at 17:42


@egret
Something like an hour ago, I tried evaporating down a conc. solution of CAN in my makeshift watch glass (a glass lens) on maybe 50C_70C, and I came back half an hour later, only to find chunks glass laid out in a circular pattern around the hotplate with dried up solids in the middle of the hotplate.

Maybe dissolving the CAN in ethanol, then add a conc. ethanol solution of calcium chloride which should precipitate ammonium chloride, filter then evaporate, that's probably what I going to do once I get some CaCl2. Anyone know of any OTC sources in Queensland? It doesn't snow here, so I don't think De-icer is an option for me.

By the way is that post up there from matbrown spam?

[Edited on 31-8-2019 by Kobold vor NH4]




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[*] posted on 31-8-2019 at 07:49


I would leave the CaCl2 out of the solution and use it as dessicator. You will get the hydrated salt of calcium which is fine, I think adding calcium chloride will give a mess of mixed salts.
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[*] posted on 2-9-2019 at 02:02


Alright, I finished titrating the the Calcium Ammonium Nitrate.
Unfortunately, I lost the titrant info (forgot to write it down, whoops),
but I got 3g of Ca(OH)2 from 10g of CAN, so ... 7CA(NO3)2 · 3 NH4NO3 ... right?

Please correct me if any of this is incorrect.

Here's my math : ([Ca(OH)2]=74g/mol) (74 divided by 23=3.2)
([Ca(NO3)2]=164g/mol) (164 divided by 23=7.1)
So that leaves the leftover 3g to be NH4NO3... Is this correct?




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