Chemgineer
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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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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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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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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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I may be wrong but i think calcium ion are known to attack glass.
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Sir_Gawain
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Do a double displacement with sodium carbonate.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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charley1957
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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.
You can’t claim you drank all day if you didn’t start early in the morning.
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Rainwater
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Charley, you are a genuine genius. And its simple, love it
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Chemgineer
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Thanks, that is probably the best idea as long as calcium carbonate settles out of the solution nicely.
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fx-991ex
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Yes it do and its very easy to filter too.
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fx-991ex
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| 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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Chemgineer
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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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fx-991ex
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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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Alkoholvergiftung
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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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Fulmen
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The simplest test for CAN is to mix it with sodium hydroxide in solution. CAN will give off ammonia.
We're not banging rocks together here. We know how to put a man back together.
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greenlight
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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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fx-991ex
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| 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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Chemgineer
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Yeh I produced some sodium nitrate as above but it's not convenient to use since it is so hygroscopic.
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