# Making Nitric Acid, oopsie



## GoldTJ (Jun 22, 2022)

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 !!!


----------



## Shark (Jun 22, 2022)

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.


----------



## GoldTJ (Jun 22, 2022)

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)


----------



## olawlor (Jun 22, 2022)

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.


----------



## Shark (Jun 22, 2022)

Dumping acids on the ground is never a good idea. That is why there is post in dealing with waste.


----------



## eaglekeeper (Jun 23, 2022)

olawlor said:


> 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
> ...


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.


----------



## GoldTJ (Jun 23, 2022)

Shark said:


> Dumping acids on the ground is never a good idea. That is why there is post in dealing with waste.


I did not write it correctly ,, I was joking


----------



## GoldTJ (Jun 23, 2022)

nothing


----------



## Yggdrasil (Jun 23, 2022)

It is all in here.
Search and you shall find


----------



## Shark (Jun 23, 2022)

4metals said:


> 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.
> 
> ...



I really need to learn to copy links on this new phone.


----------



## eaglekeeper (Jun 24, 2022)

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.


----------



## GoldTJ (Jun 24, 2022)

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


----------



## Jimbriese (Jun 24, 2022)

GoldTJ said:


> 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


----------



## eaglekeeper (Jun 24, 2022)

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


----------



## GoldTJ (Jun 25, 2022)

Jimbriese said:


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


other oops

i meant (Potassium nitrate (KNO₃))


----------



## GoldTJ (Jun 25, 2022)

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


----------



## Jimbriese (Jun 25, 2022)

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


----------



## Punterr (Jun 26, 2022)

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..


----------



## Dorcas Nimrod (Jun 27, 2022)

eaglekeeper said:


> 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
> ...


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).


----------



## eaglekeeper (Jun 27, 2022)

Dorcas Nimrod said:


> 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.
> ...



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


----------



## Daniel0007a (Sep 17, 2022)

Has anyone used Nitric acid with Spark gaps and an Air pump? You could if you do a distillation a large amount of fuming Nitric acid. It is very complex I know but the advantage is that the procedure does not need Sulfuric acid or Potassium Nitrate which may be restricted.


----------



## Daniel0007a (Sep 17, 2022)

I mean Made Nitric acid by High voltage? I may if I had a good transformer.


----------



## olawlor (Sep 17, 2022)

Daniel0007a said:


> I mean Made Nitric acid by High voltage? I may if I had a good transformer.


I've made a few grams of arc nitric with a neon sign transformer, but Quic's setup here is a lot nicer:
The Birkland Eyde process/reactot

An un-tuned arc mostly produces ozone, which makes it both inefficient at making acid and very hard on nearby elastomers. Both the NOx and ozone produced by the arc are insidiously deadly to human lungs, and need a careful ventilation strategy. Overall, if you need liters of nitric and have access to a nitrate salt, I'd recommend distillation.

The maker of the above video needs to wear gloves when handling both the acids (the metal salts are surprisingly toxic) and high voltage, and pay more respect to things that can kill him.


----------



## Daniel0007a (Sep 17, 2022)

Yes I made a TEA Nitrogen laser in College and build a UV spectrometer. The transformer was 9000 volts 60 ma quite nasty if you mess up you could die. I tried building a flat Nitrogen laser but the power circuit was too high 15 ma DC required 5 ma DC, 8000 volts. I will stick to extracting gold from bars and cpus maybe with hot HCl 31 percent, 3 percent H202 or cold 31 percent HCl and 25% H202.


----------



## Yggdrasil (Sep 17, 2022)

If you are going to dissolve any quantity of Gold, it need to have a large surface area.
But why do you want to dissolve bars?
It can be done with just nitrate salt and HCl too, so called poor mans AR.


----------



## Daniel0007a (Sep 17, 2022)

Because it is better quality and it less money than buying a huge amount of CPUs or ICs. It 99.99 percent gold. A lot of stuff that gold is fake and too cheap to be used in any plating techniques.


----------



## Daniel0007a (Sep 17, 2022)

Also, I need just small amounts of gold. Would something like Magnesium nitrate and HCl also convert tin and other salts into sludge that is not something I want I will just dissolve the bar in hot HCl 31 percent with 3 percent H202.


----------



## Yggdrasil (Sep 17, 2022)

Daniel0007a said:


> Also, I need just small amounts of gold. Would something like Magnesium nitrate and HCl also convert tin and other salts into sludge that is not something I want I will just dissolve the bar in hot HCl 31 percent with 3 percent H202.


So you are going to use it for plating?
How about buying plating solution?

The HCl H2O2 route especially with 3% will be very slow. 
Even 30% is slow. 
Might be better with pool tablets and HCl.
Bleach will neutralise the solution too fast to be if much use for solid Gold.

Anyway if you use a bar as feed stock you should either roll it thin and snip it up or melt it and pour shots that are then pounded or rolled thin.
You have to maximise surface area.


----------



## Daniel0007a (Sep 17, 2022)

Yes I may buy 30 percent H202 to increase the process. I will need a lot of H202 for that and slowly add it to the HCl cold.


----------



## Daniel0007a (Sep 17, 2022)

I have a question would 35% H202 (160 ml) in 500 ml of conc HCl 35% be powerful enough to dissolve tin and lead into a colliod like sludge?


----------



## Daniel0007a (Sep 18, 2022)

Compared to Nitric acid in HCl that is the H202 question.


----------



## Yggdrasil (Sep 18, 2022)

Daniel0007a said:


> I have a question would 35% H202 (160 ml) in 500 ml of conc HCl 35% be powerful enough to dissolve tin and lead into a colliod like sludge?


HCl don't need help to dissolve Tin and Lead


----------



## orvi (Sep 18, 2022)

Yggdrasil said:


> HCl don't need help to dissolve Tin and Lead


If time isn´t a concern for you, then you will better left it alone only with hot HCL. True.


----------



## nitrous (Sep 18, 2022)

Daniel0007a said:


> Yes I made a TEA Nitrogen laser in College and build a UV spectrometer. The transformer was 9000 volts 60 ma quite nasty if you mess up you could die. I tried building a flat Nitrogen laser but the power circuit was too high 15 ma DC required 5 ma DC, 8000 volts. I will stick to extracting gold from bars and cpus maybe with hot HCl 31 percent, 3 percent H202 or cold 31 percent HCl and 25% H202.


gee, I made a TEM in highschool.... oh... I forgot, the question was about making nitric acid using the birkland Eyde method..... what has a TEA N2 laser got to do with your original question?? 
Ammonium Nitrate is pretty easy (and cheap) to get from cold packs here in Ontario. And it will be much more easily concentrated then from BE process.


----------



## yellowfoil (Sep 19, 2022)

Could anybody make a proper list of all the glassware needed to make HNO3? Including all the adapters, connectors, thermometers and connecting clips which will survive this process. I would like to reclame HNO3 from copper nitrate as well. Thanks.


----------



## yellowfoil (Sep 19, 2022)

nitrous said:


> gee, I made a TEM in highschool.... oh... I forgot, the question was about making nitric acid using the birkland Eyde method..... what has a TEA N2 laser got to do with your original question??
> Ammonium Nitrate is pretty easy (and cheap) to get from cold packs here in Ontario. And it will be much more easily concentrated then from BE process.


Where do you buy cold packs with ammonium nitrate in Ontario. I tried everywhere and there is no ammonium nitrate any more. There is some kind of mixture, which looks like a mud. Home Hardware sells some kind of stump remover under the brand name "Fallen Leaf" which contains potassium nitrate and you have to produce ID for a pound of nitrate. And it is not cheep, like $17 + 12% tax. Times are changing.


----------



## Daniel0007a (Sep 19, 2022)

Making Nitric acid by heating copper Nitrate only. Someone asked this on a blog here so I am answering here it would be useful if you had a lot of copper nitrate but it is very expensive.


----------



## olawlor (Sep 20, 2022)

yellowfoil said:


> Could anybody make a proper list of all the glassware needed to make HNO3? Including all the adapters, connectors, thermometers and connecting clips which will survive this process. I would like to reclame HNO3 from copper nitrate as well. Thanks.



For distilling dilute nitric, I basically started with a 24/40 glass distillation apparatus:








500ml,24/40,Glass Distillation Apparatus,Laboratory Vacuum Distill Device | eBay


Find many great new & used options and get the best deals for 500ml,24/40,Glass Distillation Apparatus,Laboratory Vacuum Distill Device at the best online prices at eBay! Free shipping for many products!



www.ebay.com




(This was years ago, so I can't find exactly the same set now, but it came with 1000mL round bottom flasks. Make sure the first T has three ground glass joints, not two and an O-ring for a thermometer.)

You need to use a glass thermometer adapter for nitric, because the default rubber O-ring thermometer adapter above will catch fire with hot NOx fumes.








24/40,Glass Thermometer Adapter,100mm Stem Tube,La Chemistry Glassware | eBay


100mm Stem(Below The Ground Joint). 24/40 Glass Ground Joint. We will be very glad to help you. All pictures are of real products.



www.ebay.com





The first few Keck clips should be stainless so they hold up to the heat without deforming:








24#,Metal Steel Clip,Keck Clamp,For 24/29,24/40 Glass Ground Joint,2Pcs/Lot | eBay


Find many great new & used options and get the best deals for 24#,Metal Steel Clip,Keck Clamp,For 24/29,24/40 Glass Ground Joint,2Pcs/Lot at the best online prices at eBay! Free shipping for many products!



www.ebay.com





A "powder funnel" makes it easier to pour materials in and out of beakers without smearing them all over the ground glass joint:








90mm,24/40,Glass Powder Funnel,100ml,Brand New Chemistry Laboratory Glassware | eBay


Find many great new & used options and get the best deals for 90mm,24/40,Glass Powder Funnel,100ml,Brand New Chemistry Laboratory Glassware at the best online prices at eBay! Free shipping for many products!



www.ebay.com





You'll need to hold all the glassware securely. These two seemed to work nicely together:








Flask Clamp,Condenser Lab Iron Holder,Total Length 250mm | eBay


Find many great new & used options and get the best deals for Flask Clamp,Condenser Lab Iron Holder,Total Length 250mm at the best online prices at eBay! Free shipping for many products!



www.ebay.com












Lab Stands BOSS HEAD Clamps Holder,Laboratory Metal Grip Supports | eBay


Find many great new & used options and get the best deals for Lab Stands BOSS HEAD Clamps Holder,Laboratory Metal Grip Supports at the best online prices at eBay! Free shipping for many products!



www.ebay.com





All above links are the same store, deschem. I have no connection with them except buying glassware a few times several years ago--they packed the glass quite well in a foam box and each piece encased in bubble wrap.

I circulate the cooling water with a little fountain pump, and scrub the uncondensed NOx with an alkaline gas scrubber. You'll need something that won't oxidize to seal the glass joints: concentrated sulfuric acid is traditional, which should clue you in as to the level of hazard here! I tried a silicone & castor oil based vacuum grease the first time, which nitrated itself a vivid red. This should all be sitting inside a fume hood. Use ceramic secondary containment vessels for when the glassware breaks while full of hot acid.

For what it's worth, my standard operating procedure for distilling nitric is here: Nitric acid not condensing.


----------



## Daniel0007a (Sep 20, 2022)

Yep, everything must be glass if you're going to make concentrated Nitric acid. Ideal for AR.


----------



## Daniel0007a (Sep 20, 2022)

You may want to invest in an IR digital thermometer too.


----------



## yellowfoil (Sep 25, 2022)

Thanks a lot for all your tips. I have no idea what all those numbers mean, but as long as I know what to buy, its Ok.


----------



## Daniel0007a (Sep 25, 2022)

Well, I had trouble finding a good video on making tin(II) chloride without tin. 15 g of tin (II) chloride in 100 ml of 31% HCl, add 50 ml of distilled water and you may want to add tin metal. Why? Slowly with Air tin(II) Chloride converts into tin(IV) chloride and tin metal reduce the reaction. Since Hydrogen gas is given off you need to vent the gas regularly or it could spray corrosive tin (II) chloride and HCl all around you. I use amber bottles 220 ml with caps for many storing of chemicals. The shelf life of tin (II) chloride salt is normally 12 months and solutions only last 1-2 weeks.


----------



## Daniel0007a (Sep 25, 2022)

This is vital if you want to qualitative measure gold in solution. Tin. I think that is what you mean correct?


----------



## Yggdrasil (Sep 25, 2022)

Daniel0007a said:


> Well, I had trouble finding a good video on making tin(II) chloride without tin. 15 g of tin (II) chloride in 100 ml of 31% HCl, add 50 ml of distilled water and you may want to add tin metal. Why? Slowly with Air tin(II) Chloride converts into tin(IV) chloride and tin metal reduce the reaction. Since Hydrogen gas is given off you need to vent the gas regularly or it could spray corrosive tin (II) chloride and HCl all around you. I use amber bottles 220 ml with caps for many storing of chemicals. The shelf life of tin (II) chloride salt is normally 12 months and solutions only last 1-2 weeks.


You can not make Stannous without Tin.
One can of course buy it in salt form, but it cost more of course.

You seem to very dependent of videos and detailed lists of what to do?
Better study so you understand why we do the different things we do.
There recipe you listed up here is way to much for any one in here apart from the professionals maybe.

There is no need to view videos for making Stannous.
That is over complicating things.
And you should not make more than 50ish ml at a time.
That will go bad long before most of us managed to use it up.
Take any HCl you have 29-38% add some 20+ ml to a bottle put in a few grams of Tin metal, preferably not a single button.
Add a bit of water and let it dissolve with open cap.
If you have HCl with less than azeotropic strength just use as is, no water needed.
When the bubbling has stopped, if there are still Tin metal it is ready.
If all is dissolved add a bit extra metal and it is ready.


----------



## Daniel0007a (Sep 25, 2022)

Yes I do over complex things but however, this is a method of making it but you need to heat up tin (II) chloride carefully in HCl with good stirrering and heating.


----------



## Daniel0007a (Sep 25, 2022)

My background is in BioPhotonics, Electronics, and Biotech but I studied 10 years (Photonics, Biotech, Water and waste management) and work too. I do have a lab with hot plates, chemicals, Digital scale, etc. Not a cheap hobby but I branched out a lot.


----------



## yellowfoil (Oct 7, 2022)

olawlor said:


> For distilling dilute nitric, I basically started with a 24/40 glass distillation apparatus:
> 
> 
> 
> ...


Thanks for your tips Olawlor, will look into this as soon as possible.


----------



## Sancho_n_Pedro (Oct 8, 2022)

Yggdrasil said:


> You can not make Stannous without Tin.
> One can of course buy it in salt form, but it cost more of course.
> 
> You seem to very dependent of videos and detailed lists of what to do?
> ...


Trying to make a small sample of Stannous Chloride, but the HCL I have is only Patio cleaner with a % of between 10 - 20. Will this still be suitable, just don't add extra water?


----------



## Yggdrasil (Oct 8, 2022)

Sancho_n_Pedro said:


> Trying to make a small sample of Stannous Chloride, but the HCL I have is only Patio cleaner with a % of between 10 - 20. Will this still be suitable, just don't add extra water?


Should be ok. Only a little more time needed.


----------



## FrugalRefiner (Oct 8, 2022)

Yep.

Dave


----------

