Concentrate Nitric Acid ?

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About the cooling process with the nitric when it needs -5 C, is there any difference if i keep the vessel sealed or opened?
Will toxic fumes or anything else dangerous be created?

And as i have understood it, is the sodium bisulphate which is the "sludge" useless for any other use?
 
Zorba,


Sometime back I posted a process for recycling the bisulphate and/or sulphate produced. It's titled something like 'Nitric Acid Everything but the Squeal'.

I've also since penciled a few other ways to recycle the sulfate by-product.

Steve
 
lazersteve said:
Zorba,


Sometime back I posted a process for recycling the bisulphate and/or sulphate produced. It's titled something like 'Nitric Acid Everything but the Squeal'.

I've also since penciled a few other ways to recycle the sulfate by-product.

Steve

Alright, i will check that out.
Still, will it be any difference if i seal my vessel with the nitric when storing it in -5 C ?
 
I do not seal any vessels that go into freezer, or for that matter if they are heated, I keep them open to atmosphere as a heated or cooled liquid needs room to expand or contract with temperature change, I may put a lid on loose.

sealing may not be a problem here but I will not take that risk of a broken vessel with nitric acid.
 
Maybe an awkward question, but when i have boiled off all the H2O from the battery acid, will it differ if
the coulour of the approximately 98 % H2SO4 is amber or just "ordinary" white ?
At one stage i got the amber colour and at another white, like water.
 
Here is a transcription of the Prof. Osborn prospector´s book from 1910, and I think today the problem no have great changes.
I hope you find it useful.
Regards.
 

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Dr. Cooper,

That's the standard method of distilling nitric acid. Unfortunately, most people here don't have access to the required glassware, that's why the cold methods are usually preferred.

I just bought a copy of the same book last week and page 142 in my version does not have the recipe!?! I guess Uncle Sam decided it needed to be removed. Page 144 in my version picks up where the author discusses using potash for sulfide ores, your page 143.

Steve
 
Tried this twice now.

Ist try I used battery acid where the H2O was boiled off - resulting reaction was weak because of a mistake between C and F.

2nd try I used Easyflow for H2SO4 everything went like it was supposed to except that when I poured off what looked like a colorless and oily liquid into another container it immediately turned into a yellow - bubbly - semi-soild. Cilled further after letting get to room temp - have a solid mass.

Any ideas?


lazersteve said:
Chris,

Nothing appears wrong with yours a first glance, except in mine I'm not leaving any Hydrogen behind as follows:

H2SO4 + 2 NaNO3 --> Na2SO4 + 2HNO3

The big difference in my recipe is the solubility of the sodium sulfate salt (as opposed to sodium hydrogen sulfate you produce) and the fact that my equation yields twice the nitric acid at a higher temperature ( no dry ice, just salted ice ). :wink:

I've run the numbers like you did and ended up with about 160 mL of 50% nitric (give or take a few percent) for a single mole of 96% sulfuric and using 100mL H2O to dissolve the nitre.

I won't bore everyone with the math, but here's my summary (PM me to see all the factors I used to derive this reaction):

skullnbones_smallrev.jpg


Reaction:

-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm K / 170 gm Na)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil!
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)
-When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3

skullnbones_smallrev.jpg


Steve
 
Noxx said:
Hello,
Is there a way to concentrate my nitric acid without distillation ?
I made it with with Sulfuric acid and Potassium Nitrate. Final product is about 30% Nitric.
Thanks

Why do you want to increase it's concentration? It's very difficult to store concentrated nitric acid because it's very sensitive to light and temperature.
 
Do not boil, evaporate to concentrate nitric acid, you can get it too hot and loose acid, depending on the concentration the boiling point changes, and the highest you can concentrate nitric (evaporate off water) is to about 68%, this is the Azeotrope of nitric acid and water.
 
If this helps anyone.I make my red fuming Nitric with Soodium Nitrate and store bought Sulfuric for drain cleaning.I never used any water in the setup.Just use enough acid to make the Nitrate very moist and start distilling.The nitric starts at about 85c and finishes at about 110c.I have done this numerous times with perfect results everytime.Some say to use ice water to cool your condenser but i found tap water worked great for me .Now this is to make high concentration acid which woul dhave to be dilluted for the purpose of refineing,but concentrated takes up less room and dillute as needed.
 
brjook, there is no reason on this forum for fuming HNO3, many here may know how to make it but we may not share that here on the forum, I personally do not think the forum needs that attention from authorities, or the people that may want a recipe for purposes illegal or that could harm others, information regarding fuming nitric is not needed here on the forum or for refining metals.
 
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