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Author: Subject: Weird things during nitric acid synthesis
Sir_Gawain
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[*] posted on 2-11-2023 at 17:02


You could just add an excess of sulfuric acid to convert it all into bisulfate.



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[*] posted on 3-11-2023 at 01:12


Because there are not enough K+ Ions, so only one per sulfuric acid molecule(=potassium bisulfate), instead of two (potassium sulfate), right?
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[*] posted on 3-11-2023 at 03:39


Quote: Originally posted by Nikotin  
Because there are not enough K+ Ions, so only one per sulfuric acid molecule(=potassium bisulfate), instead of two (potassium sulfate), right?


That'a way to see things. The (mostly accepted) view is one of pH equilibrium. KHSO₄ is a weak acid, therefore the proportion of KHSO₄ vs K₂SO₄ is pH dependent. But both are equivalent. That is, if you start from one mole of H₂SO₄ and add one mole of KOH, considering that the former is a strong acid and the latter a strong base, you should end up with one mole of KHSO₄. But since that KHSO₄ is in solution in water, there will be a non-zero number of HSO₄⁻ anions that will give away a proton to a water molecule and transform into SO₄²⁻, which you can consider as diluted potassium sulphate.

Beside, if you heat it over 600 °C, potassium bisulphate will lose SO₃ (that you can make sulphuric acid back with) and transform into potassium sulphate:

2 KHSO₄ → K₂SO₄ + SO₃ + H₂O
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[*] posted on 3-11-2023 at 23:53


Quote:
Beside, if you heat it over 600 °C, potassium bisulphate will lose SO₃ (that you can make sulphuric acid back with)

I tried that once, not willing to do it again.
That stuff is nasty. Like really nasty, total containment is a must.
It eats gloves, mask, wood. Watch my new tongs rust before my eyes.
Leave that reaction to the professionals please.




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[*] posted on 4-11-2023 at 02:23


Quote: Originally posted by Rainwater  
Quote:
Beside, if you heat it over 600 °C, potassium bisulphate will lose SO₃ (that you can make sulphuric acid back with)

Leave that reaction to the professionals please.


I’m not sure why you say that. The setup is very simple and there is really little danger if you do things correctly. I use a quartz tube, a borosilicate bent tube and a condenser. Of course, do that outside. My starting point is sodium bisulphate, that you can buy cheaply as pH minus for swimming pool. I got 5 kg for 2 € at the local LIDL.

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[*] posted on 21-11-2023 at 16:31


I am happy I found this site. I have built a lab to make 99.X% nitric and going through the struggles

Stopping NO2 leaks and corrosion is the first thing - I found these along with the PTFE coated metal clips (https://www.labunlimited.com/cms.jsp?menu_id=29544&descr...)

I installed a separate birkeland eyde reactor that will have a cooled liquid jacket and stiring and I am going to heat the NO2 post arc reactor.

The first stage distillation to 68% nitric seems to be straight forward with a glass rashing ring distillation stage I just need to seal it up, got up to about 110 F in the bulb then just started running out of liquid which suggests poor yield in the creation of dilute nitric.

I have a separate still for distilling sulpheric and still need to break up a bunch of tiny glass for that still.

It sounds like from above the best mixture for the final distillation is 50% 90%+ sulpheric and 50% 68% nitric

I hope these little seals work because the thin teflon sleves didnt and its safety first, I will abandon this entire buisness venture if I cant do it safe.
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[*] posted on 21-11-2023 at 18:28


I use a water asporator to place the appratus under reduced pressure.
Any leaks, leak in, keeping total containment.
The asporator with a baking soda solution, is an almost perfect gas scrubber
You get less decomposition of your product.
And of your slick, you can include a bubble capillary to prevent bumping.




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[*] posted on 22-11-2023 at 22:49


Quote: Originally posted by Rainwater  
I use a water asporator to place the appratus under reduced pressure.
Any leaks, leak in, keeping total containment.
The asporator with a baking soda solution, is an almost perfect gas scrubber
You get less decomposition of your product.
And of your slick, you can include a bubble capillary to prevent bumping.


Thats a great idea, I just ordered this - https://www.amazon.com/dp/B071X63B2R?psc=1&ref=ppx_yo2ov...

With 24/40 connections - one connection will be the bubbling frit introducing the NO2 another will be a suction tube (I have a 500 micro vacuum pump connected to the still to create enough vacuum to force the liquid over to the boiler.

The 3rd is the vent that I could put the aspirator on (or eductor maybe?) - can you recommend one that I could use like a fish tank bubbler instead of water. I dont have water running to this building but i have a large water tank I could circulate with a pump but using air as the motive fluid would be easier.

Could the still be operated in a similar manner with an asperator on the outlet of the top side condenser it would be mixed phase flow (liquid water and water vapor mixed with nitric carry over)
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