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Author: Subject: Nitric acid from calcium nitrate
Chemgineer
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[*] posted on 8-6-2024 at 15:55
Nitric acid from calcium nitrate


I normally produce nitric acid from magnesium nitrate and sodium bisulfate dry distillation and it works great.

I have however allot of calcium nitrate I want to use but the Nurdrage procedure for the distillation of this with sodium bisulfate works great but erodes chunks of glass from my flasks and breaks them!

Do you think I should be converting the calcium nitrate to another nitrate salt to avoid this or would a wet distillation of calcium nitrate and sodium bisulfate be better.... with a fractional distillation of the nitric acid later?
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Rainwater
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[*] posted on 8-6-2024 at 18:32


CaSO4 is a real pain in the !@@ to clean. I experienced glass etching with sodium metabisulfate and CaNO3
It was only noticeable after 3~4 runs
And again with potassium bisulfate(leftovers from making HNO3 via sulfuric acid & potassium nitrate)

I think its the little bit of water trapped in the salt that lets it eat glass if at any point a hydroxide forms.




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Chemgineer
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[*] posted on 9-6-2024 at 05:01


Quote: Originally posted by Rainwater  
CaSO4 is a real pain in the !@@ to clean. I experienced glass etching with sodium metabisulfate and CaNO3
It was only noticeable after 3~4 runs
And again with potassium bisulfate(leftovers from making HNO3 via sulfuric acid & potassium nitrate)

I think its the little bit of water trapped in the salt that lets it eat glass if at any point a hydroxide forms.


Yes always 3-4 runs before it starts, making you think everything will be fine! Perhaps the first few runs allow some calcium sulfate to stick to the glass and get a better adhesion on the later runs.

Hmm I wonder if it would help to alternate between magnesium nitrate anc calcium nitrate runs, would this help to clean the flasks?
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Rainwater
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[*] posted on 9-6-2024 at 07:42


Quote: Originally posted by Chemgineer  
would this help to clean the flasks?

Not sure, a 20 minute boil in hot water usually breaks up and softens the larger chunks of plaster. My problem is getting the rbf absolutely clean. No matter how many times i wash it, there is always a little caso4 still left in there. Washing with hot diluted H2SO4(~5%) does the trick.




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fx-991ex
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[*] posted on 9-6-2024 at 08:00


I may be wrong but i think calcium ion are known to attack glass.
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Sir_Gawain
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[*] posted on 9-6-2024 at 09:28


Do a double displacement with sodium carbonate.



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charley1957
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[*] posted on 9-6-2024 at 09:29


I have a container of steel BBs at the sink where i wash my glassware. Swirling/shaking them around in the flask works wonders to help break up stuck-on stuff. Saves acid too.



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Rainwater
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[*] posted on 9-6-2024 at 18:12


Charley, you are a genuine genius. And its simple, love it



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[*] posted on 10-6-2024 at 07:04


Quote: Originally posted by Sir_Gawain  
Do a double displacement with sodium carbonate.


Thanks, that is probably the best idea as long as calcium carbonate settles out of the solution nicely.
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[*] posted on 10-6-2024 at 07:59


Quote: Originally posted by Chemgineer  
Quote: Originally posted by Sir_Gawain  
Do a double displacement with sodium carbonate.


Thanks, that is probably the best idea as long as calcium carbonate settles out of the solution nicely.

Yes it do and its very easy to filter too.
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[*] posted on 10-6-2024 at 08:00


Quote: Originally posted by charley1957  
I have a container of steel BBs at the sink where i wash my glassware. Swirling/shaking them around in the flask works wonders to help break up stuck-on stuff. Saves acid too.

I do the same thing but i use coarse salt instead loll, i guess sand could work well too.
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[*] posted on 14-6-2024 at 13:09


Does this sound reasonable volumes for double displacement of sodium nitrate from calcium nitrate using sodium carbonate?

120g Na2CO3 in 300ml water
185g Ca(NO3)2 (not anhydrous) in 100ml water

Should produce 190g of NaNO3 in 400ml of water once the calcium carbonate is filtered off.

Or should I add my 300ml solution of sodium carbonate directly to my calcium nitrate prills and heat and mix ending up with only 300ml volume with less boiling down needed?
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[*] posted on 14-6-2024 at 13:45


Make sure your Ca(NO3)2 are in fact Ca(NO3)2 and not CAN calcium amonium nitrate.
If its CAN then:
For 120g of Na2CO3 you should use 222g of CAN to get 192g of NaNO3, 103g CaCO3, 37g H2O, 10g (NH4)2CO3(will decompose upon heating to recrystallize).

If your Ca(NO3)2 is indeed pure then the ratio/weight are correct.
Just use as little water as possible.

Id avoid pouring the Na2CO3 sln into the Ca(NO3)2 prill, you may want to filter the Ca(NO3)2 sln before rxn.
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[*] posted on 14-6-2024 at 22:30


The test for CAN should be easy. In Aceton 1l disolve 330g Calciumnitrate and only 1g ammoniumnitrate. Would be a seperation methode too.

[Edited on 15-6-2024 by Alkoholvergiftung]
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[*] posted on 15-6-2024 at 01:35


The simplest test for CAN is to mix it with sodium hydroxide in solution. CAN will give off ammonia.



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[*] posted on 15-6-2024 at 09:33


You could also convert the calcium nitrate to potassium nitrate with potassium chloride if that's easy to find in your country. Potassium chloride can be brought in large quantities in some places as water softener.
Then you have nitrate salt thats easier to dry and keep dry as it is not hygroscopic like sodium nitrate.

Distillation with concentrated sulfuric acid and done:)




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[*] posted on 15-6-2024 at 11:57


Quote: Originally posted by greenlight  
You could also convert the calcium nitrate to potassium nitrate with potassium chloride if that's easy to find in your country. Potassium chloride can be brought in large quantities in some places as water softener.
Then you have nitrate salt thats easier to dry and keep dry as it is not hygroscopic like sodium nitrate.

Distillation with concentrated sulfuric acid and done:)


It work but purity will be better with KOH, or he could just re-crystallize twice of course.
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[*] posted on 21-6-2024 at 06:33


Yeh I produced some sodium nitrate as above but it's not convenient to use since it is so hygroscopic.
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