Making Nitric Acid, oopsie

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GoldTJ

Active member
Joined
May 30, 2022
Messages
35
Location
Edmonton
So I was Making a batch of nitric acid ,

With Sodium Potassium , and Sulfuric Acid ,
And distilling Nitric Acid as it goes
( mostly like this video )

The oops came from my distilling apparatus,,,
The cheap one I have has a thermometer on top thru a unknown material rubberlike stopper

This stopper didn't like the nitric acid vapor and mostly all drip down in the flask

Did I accidently produce anything explosive?

I don't want to search online too much on this topic !!!
 
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It shouldn’t be explosive but I am not a chemist. Nitric acid does not like rubber and will eat it very quick. I guess you know that by now though. I have used Teflon tape to wrap rubber stoppers to protect them from nitric fumes but still wasn’t comfortable using them.
 
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Well , I did another batch ,, with a "glass" stopper , and no thermometer , I have the "sense" of it now !

But I wasent shure about this batch,, Should I had to carefully drop it in the wood and run ? (just joking)
 
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I've had that same silly rubber grommet catch fire from the hot NOx fumes!

An all-glass thermometer adapter (wraps all the way around the thermometer with glass) will hold up to those same fumes:
24/40,Glass Thermometer Adapter,100mm Stem Tube,La Chemistry Glassware | eBay

I've had several organics catch fire in hot nitric, but as long as there's water in the process I haven't had any issues with dangerous nitration. I'd be comfortable filtering out the burnt bits and re-distilling.

Please neutralize any of your waste and dispose of it responsibly.
 
Dumping acids on the ground is never a good idea. That is why there is post in dealing with waste.
 
I've had that same silly rubber grommet catch fire from the hot NOx fumes!

An all-glass thermometer adapter (wraps all the way around the thermometer with glass) will hold up to those same fumes:
24/40,Glass Thermometer Adapter,100mm Stem Tube,La Chemistry Glassware | eBay

I've had several organics catch fire in hot nitric, but as long as there's water in the process I haven't had any issues with dangerous nitration. I'd be comfortable filtering out the burnt bits and re-distilling.

Please neutralize any of your waste and dispose of it responsibly.
You beat me to it...

They do sell thermometer adapters that have the plastic screw down cap....the caps/o-ring doesn't hold up very well to the fumes. Also, If you use those plastic Keck clips, I wouldn't recommend them at the boiling flask connection, they'll probably melt.
 
Waste treatment for the small refiner.

Most of the practicing alchemists on this forum generate waste liquids which, if you have the time and desire, can be neutralized and made free of toxic metals rather simply. The required supplies are simply a pH meter, a few plastic tanks (15 gallon size is ideal), an aquarium air pump and some tubing, slab of copper, some scrap iron. The advantage you have in being a small producer is that you have the time to let the solutions sit and react before proceeding to the next step. Because of this you do not need expensive pH controllers or a filter press and the associated pumps.

The procedure that follows is for your acid waste only, it is not for cyanide or leaching type wastes, only the spent acids used to digest the metals you have refined.

Select a plastic tank to use as a holding tank for your spent acid, if it is translucent it makes it easy to see how full it is. This tank should have a lid to keep out rainwater and it should be kept where it will not freeze. What we will do in this tank is a process called cementation, whereby you hang a slab of copper metal in the waste acid to displace any precious metals which may still be in solution. When the tank is approaching full, maybe a few inches from the top, the copper is suspended in the tank and the solution is agitated to expose the copper to as much solution as possible. An easy and inexpensive trick is to buy an aquarium pump and some tubing and weigh the end of the hose down so it is close to the bottom of the tank and let it bubble away. Overnight should suffice. The copper bar will have displaced any PM’s in the solution which will settle to the bottom. Don’t expect a lot of material to settle from each load, but in time the material on the bottom is collected and refined for values. Allow the solution to settle after removing the bubbler and the copper bar, a few hours should do it. Now siphon the acid into another tank, being careful not to suck out any of the settled material. Usually a few inches of solution left on the bottom will prevent you from sucking out the solids and it is just left in the tank as you start to accumulate more waste acid.

A simple siphon device to prevent siphoning all the way to the bottom can be easily made as follows; cut a length of ½” CPVC pipe about 24” long, glue on a tee, followed by a 6” piece of pipe and a cap on the end. I prefer to use half inch “copper pipe sized” CPVC because it is nice and slim and easy to find tubing to slip over the end. Now you will need some flexible tubing to slip snugly over the end of the pipe opposite the capped end, about 4 or 5 feet will do. You will now have a hose and a short length of pipe which has an opening (because of the tee) 6” from the capped end. To start a siphon, place a finger over the hole in the tee and fill the entire hose and pipe with fresh water, then quickly submerge the capped end and place the end of the hose lower than the solution level in the tank. With this setup you don’t have to worry about sucking the solids off the bottom of the tank. One drawback is the tank you are siphoning from has to be higher than the tank you are siphoning to, so you’ll have to lift the full cementation tank on to a table to siphon it completely.

This second step can boil over if you’re not careful so I would transfer the liquid from the 15 gallon cementation tank into a 30 gallon tank if you’re going to process this all at once. Add your air bubbler to the 30 gallon tank and start bubbling. Check your pH, it should be close to zero when you start. Slowly add soda ash to the bubbling liquid, it will foam and generate CO2 so be careful not to boil it over, since an aquarium pump doesn’t move the liquid aggressively, add the soda ash slowly and stir with a pvc pipe occasionally to make sure it all is dissolving. Slowly over the course of a day or two raise the pH to 2.5.

Now you will add scrap iron to the tank, it can be done by placing the pieces of iron directly in the tank and fishing them out later, (needless to say with rubber gloves on) or you can get a plastic tank that fits into the 30 gallon tank, drill holes in it on the sides and bottom, and immerse the iron in all at once. The iron will displace copper and other metals from solution and slowly dissolve in the liquid. The iron will get coated up and a good shaking will remove the coating from the iron. After a few hours, the solution will have a green tea look to it which is ferric chloride. If you leave the iron in longer it will continue to dissolve so remove it and rinse it well. The copper and other metals will accumulate on the bottom of the 30 gallon tank where they are from time to time collected and dried.

You now use the siphon device to siphon the liquid to a final tank. Your primary contaminant now is iron. You can raise the pH with sodium hydroxide and the iron will drop out of solution which is quite easy to recognize. Unfortunately this liquid is a bit gel like and doesn’t filter well. A better way is to raise the pH with Magnesium hydroxide, the resultant sludge settles better and dries nicely. You cannot measure the pH of the reaction while adding magnesium hydroxide because it is slow to change the pH and you will over add, just go slowly and when you get the color change you’ll know the iron has dropped out. Let the iron settle and you can siphon off the now clear liquid to discard.

I really need to learn to copy links on this new phone.
 
Fuming nitric acid is NOT recommended in refining. Not only does it create a safety/fire hazard, but in most cases it slows the process down....you need the water to dissolve the metal salts.

As a side note, Nilered and Nurdrage has some good video's.
 
Since i didnt realy split the water fraction comming out, i tink I got a mix in the asiotropic range and even below. It doest react much with copper (even if i add water)

Iv tried before the bubling gaz in water method, and the steve one with ice bath without as much yeld as this this distiling method :)
 
With Sodium Potassium , and Sulfuric Acid ,
And distilling Nitric Acid as it goes

So that does not make nitric. Sodium nitrate or potassium nitrate and sulfuric acid does.

I have been playing with potassium nitrate to come up with nitric acid in the 65-70% range.

My last test batch came in at 72%

Potassium nitrate stump remover 160 g
Distilled water 40ml
Sulfuric acid drain opener. 120ml
 
I've been using the same recipe for years to make cold nitric and it seems to work fine. But, I've seem so many different recipes that it makes me wonder if mine is correct. (Actually if I remember right it's Lazersteve's recipe)

172 g of sodium nitrate (nitrate of soda from Ace hardware)
100 ml of water
56 ml sulfuric acid (drain cleaner)

or

202 g potassium nitrate (stump remover)
100 ml water
56 ml sulfuric acid (drain cleaner)

Can anyone comment on if I need to make adjustments to improve the recipe....thanks
 
Some recipes using the distiling method call for adding water , other not.
I guess it only help to disolve the potassium nitrate first, but after that it just end up with more water in the first distilation fractions.
Or is it ?

I didnt use any water,
Like nilered did here

110g potassim nitrate (kno3)
60ml conc. sulf acid

mabee the small water amount in the drain cleaner was enough, or water is useless. Or adding water help to stay in a lower concentration nitric ~67% instead of the useless for us higher 90%+ red fuming
 
No water makes 90% or higher mixing in water lowers the concentration if to much water is added you get water first then diluted then the azeotropic with the amounts in my previous post the temp went straight to 115-120C with no pause for water at
100c an excess water would have come over as diluted nitric but it was so minimal I don’t separate the fractions
 
You can use only dry ingredients, such as Sodium Bisulphate (Monohydrate) and a dry nitrate salt (most will do), heat it and condense the vapors (NOx), make sure the condenser water is no more than 5 Celsius collect the liquid in a flask with a vacuum adapter and pipe that to another flask (also with a vacuum adapter) in an ice bath and you will end up with a decent nitric yeald better than 80%. You should use the monohydrate as you do need a little water for the reaction. If you only can get the anhydrous version you should add 1M water to the Bisulphate to make the Monohydrate equivalent.
You can combine the output from the 2 flasks and then distil it if you like.

Good luck..
 
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I've been using the same recipe for years to make cold nitric and it seems to work fine. But, I've seem so many different recipes that it makes me wonder if mine is correct. (Actually if I remember right it's Lazersteve's recipe)

172 g of sodium nitrate (nitrate of soda from Ace hardware)
100 ml of water
56 ml sulfuric acid (drain cleaner)

or

202 g potassium nitrate (stump remover)
100 ml water
56 ml sulfuric acid (drain cleaner)

Can anyone comment on if I need to make adjustments to improve the recipe....thanks
There's no recipe per-se. The stoichiometry of the reaction for potassium nitrate (KNO3 + H2SO4 = K2SO4 + HNO3) can be found in this calculator
For sodium nitrate, this calculator.

This presumes dry/100% ingredients. The more water in your reaction vessel, the more dilute your acid will be. The less water in the starting reactants, the closer you'll get to fuming nitric acid. Since your sulfuric acid is not 100%, you will adjust for the percentage of water in the acid.

So, for 172 grams of potassium nitrate, you should use 99.239 grams of (100%) sulfuric acid, or (very approximately) 117 grams of 82% sulfuric acid. (I personally have a difficult time calculating molarity, and this calculation involves converting percentages using the molar mass of both H2SO and water, but a rough estimate will do here) You can estimate the concentration of your sulfuric acid by density here, and the final concentration of your nitric acid here.

My Rooto drain cleaner is about 82% sulfuric acid. I use this straight, with potassium nitrate stump remover, and it produces just barely fuming nitric acid (just enough to ignite a nitrile glove).
 
There's no recipe per-se. The stoichiometry of the reaction for potassium nitrate (KNO3 + H2SO4 = K2SO4 + HNO3) can be found in this calculator
For sodium nitrate, this calculator.

This presumes dry/100% ingredients. The more water in your reaction vessel, the more dilute your acid will be. The less water in the starting reactants, the closer you'll get to fuming nitric acid. Since your sulfuric acid is not 100%, you will adjust for the percentage of water in the acid.

So, for 172 grams of potassium nitrate, you should use 99.239 grams of (100%) sulfuric acid, or (very approximately) 117 grams of 82% sulfuric acid. (I personally have a difficult time calculating molarity, and this calculation involves converting percentages using the molar mass of both H2SO and water, but a rough estimate will do here) You can estimate the concentration of your sulfuric acid by density here, and the final concentration of your nitric acid here.

My Rooto drain cleaner is about 82% sulfuric acid. I use this straight, with potassium nitrate stump remover, and it produces just barely fuming nitric acid (just enough to ignite a nitrile glove).

Thanks for the links...I'll check it out.
 

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