# Nitric acid production questions



## fivel_976 (May 8, 2019)

I have a few questions I'd like to get answers to before I start. First of all my set up will be simple distillation 1000ml boiling flask 500ml catch flask the setup came with a 200mm condenser I felt like I'd get more if I bought a 400mm so I did. I'll be heating this with a propane berner I use to use for lead smelting since it's an open flame I decided to go with a sand bath. My chemicals consist of spectracide and hi-yeald stump remover that I heated in distilled water and crystallized to purify it and rooto sulfuric acid drain cleaner my plain is to mix 400 grams of each and distill. My question is in a few you tube videos people heat this to different temps one guy says at 250 you distill 68% nitric and at 315 you get 95% nitric but others say heating this high runes it. I want to get the most that I can outa each batch and I also beleave the higher % the better as I won't need to stock pile mass amouts of acid just more water so I'm confused at what temp is gonna be the best yield. Also I. Wondering if I piggyback my liebig 200mm and 400mm condensers together will I net more acid as the fumes pass through. Thanks in advance for any advice


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## Shark (May 8, 2019)

I have never used anything stronger than 67% although I have used some at less than that. Even at 67% I use 50/50 water to nitric most of the time. It will work fine on silver.

I don't recall off the top of my head right now what temps to distill it at (been a while since I made any) but 250 sounds way high. Like refining it needs time to come out right.


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## niks neims (May 9, 2019)

fivel_976 said:


> I have a few questions I'd like to get answers to before I start. First of all my set up will be simple distillation 1000ml boiling flask 500ml catch flask the setup came with a 200mm condenser I felt like I'd get more if I bought a 400mm so I did. I'll be heating this with a propane berner I use to use for lead smelting since it's an open flame I decided to go with a sand bath. My chemicals consist of spectracide and hi-yeald stump remover that I heated in distilled water and crystallized to purify it and rooto sulfuric acid drain cleaner my plain is to mix 400 grams of each and distill. My question is in a few you tube videos people heat this to different temps one guy says at 250 you distill 68% nitric and at 315 you get 95% nitric but others say heating this high runes it. I want to get the most that I can outa each batch and I also beleave the higher % the better as I won't need to stock pile mass amouts of acid just more water so I'm confused at what temp is gonna be the best yield. Also I. Wondering if I piggyback my liebig 200mm and 400mm condensers together will I net more acid as the fumes pass through. Thanks in advance for any advice




why would you need that high nitric % ? you are not trying to make explosives are you?

for recovery/refining nitric azeotrope of 68% works fine


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## g_axelsson (May 9, 2019)

Please, don't double post. I deleted your other post.

Göran


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## fivel_976 (May 9, 2019)

Sorry I wasn't getting any answers here so I thought the need help would be better


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## fivel_976 (May 9, 2019)

I just figured at 95% I could store less volume of acid and just use more water to get to 35% needed for silver


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## anachronism (May 9, 2019)

fivel_976 said:


> I just figured at 95% I could store less volume of acid and just use more water to get to 35% needed for silver



You don't want to be making 95% Nitric. Stick to the lower concentration.


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## fivel_976 (May 9, 2019)

So to get 68% do I bring the boiling temp to 250 degrees Fahrenheit and hold the temp there until the sulfuric acid is almost gone? And will I benefit from running a longer condenser like butting my 400mm to the 200mm?


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## FrugalRefiner (May 9, 2019)

Fivel, you really need to study the process more before you jump into this. The questions you're asking show you don't understand it.

When you mix your nitrate salt with sulfuric acid, you end up with nitric acid and a sulfate salt, so you're not boiling the solution till the "sulfuric acid is almost gone".

95% nitric acid is horribly dangerous, and you can't get it by simple distillation regardless of the temperature.

When distillation is properly run, the length of the condenser is not important. You balance the temperature of the solution with the cooling capacity of the condenser. You won't "net more acid" by connecting two condensers together unless you're heating the solution too much with just one condenser.

Lazersteve and others have worked out the proper amounts of nitrate salt and sulfuric acid to use. Mixing 400 grams of each just wastes chemicals.

Don't rely on YouTube videos. Study what's been written here on the forum before you start mixing chemicals.

Dave


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## butcher (May 9, 2019)

fivel_976,
The boiling point of the solution is determined by the concentration.
While the concentration will be determined by how much water is involved in the original solution being distilled.

Take a look at one method I like to make my nitric acid while recovering gold from electronic scrap in the same process, although it is not what you're trying to do, the information there will help you gain some understanding of distilling nitric acid.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&p=54264&hilit=kill+two+birds+one+stone#p54264




Pure water has a boiling point of 100 degrees Centigrade.
20% Nitric acid boiling point of 103 degrees Centigrade and a density of 1.115 g/cm3.
30% HNO3 boiling point of 107 degrees Centigrade and a density of 1.180grams per cubic centimeter
50% nitric boiling point 116 degrees Centigrade and the density of 1.310
68% nitric is the azeotrope of nitric acid.
70% nitric boiling point 121 degrees centigrade and density of 1.482 g/cm3 
90% nitric boiling point 102 degrees centigrade density 1.482 g/cm3
98% nitric acid boiling point 86 degrees centigrade density 1.503 g/cm3


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## fivel_976 (May 9, 2019)

Reading the linked post doesn't really help me flooding my mind with different processes only further confuses me. I just want to start by making my nitric acid by simple distillation I'm trying to do this whole process 1 step at a time all I want at this moment is to make a nitric acid capable of dessolving silver I just need a simple how to guide


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## anachronism (May 9, 2019)

fivel_976 said:


> Reading the linked post doesn't really help me flooding my mind with different processes only further confuses me. I just want to start by making my nitric acid by simple distillation I'm trying to do this whole process 1 step at a time all I want at this moment is to make a nitric acid capable of dessolving silver I just need a simple how to guide



It may just be me but I'm struggling with how this post is worded. 

Jon


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## Shark (May 9, 2019)

I was just as confused when I first started. I also had no way to buy nitric acid and started by making some using the cold method as it could be done without distilling it. Knowing it would cost me a small bit of silver, I used it anyway to learn the process of cementing silver from a nitrate solution. I used the cold method several times until I had figured out some of the things I wanted to learn. Since it worked so well, I mixed up some of the chemicals for the cold method then distilled it as it was. While there are better ways, it done the job for quite some time until I became able to purchase a small amount that I am just now getting low on. Used right, 5 gallons of 67% nitric will process a good amount of silver, or in my case gold filled. 

I am happy now, (not so much so back then) that it took me a while to study it out. Along the way I learned a few things that really became useful later and had no idea at the time I would ever need them. Refining is something that takes time, each step is whole process in its self. In the five or six years I have been doing this, even the things I have learned that didn't work were worth the time to learn.


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## anachronism (May 9, 2019)

Well worded Shark.


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## fivel_976 (May 9, 2019)

Just looking for a simple guide to distilling nitric acid in a 1000ml set up . Like how much of each ingredient what temp how long to go for. If I can't find the answers I'll just put equal amounts of nitrate crystals and sulfuric acid and turn the heat up and let her buck see what comes out of the other end


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## FrugalRefiner (May 9, 2019)

OK, here's are a couple of links: Simple Answers, Tips.

Dave


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## fivel_976 (May 9, 2019)

Im well aware of the risks in the vary spot I smelted my lead will be the spot I do my distilling 18" wall fan that can move alot of air. Is you think hot acid is that dangerous try melting 3000+ lbs of lead wheel weights and poring 3000+ ingots id rather have hot acid on me then 700+ degree molten metal witch will bond to your skin not to mention the toxic fumes from melting it


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## anachronism (May 9, 2019)

fivel_976 said:


> Im well aware of the risks in the vary spot I smelted my lead will be the spot I do my distilling 18" wall fan that can move alot of air. Is you think hot acid is that dangerous try melting 3000+ lbs of lead wheel weights and poring 3000+ ingots id rather have hot acid on me then 700+ degree molten metal witch will bond to your skin not to mention the toxic fumes from melting it



I'll get pilloried for this but I think your attitude sucks. I don't expect any support for my position but I'm going to say it as I see it. 

You are here seeking knowledge. You are entitled to nothing. Knowledge is earned so go search and when you have looked at that knowledge and find a part you don't understand THEN come back and ask for clarity. 

People supply information here out of the goodness of their hearts. No financial gain, nothing. You would be well advised to take note of that.


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## FrugalRefiner (May 9, 2019)

anachronism said:


> I'll get pilloried for this but I think your attitude sucks. I don't expect any support for my position but I'm going to say it as I see it.
> 
> You are here seeking knowledge. You are entitled to nothing. Knowledge is earned so go search and when you have looked at that knowledge and find a part you don't understand THEN come back and ask for clarity.


I'll not put you in the stocks. I provided a couple of links that tried to communicate the same message.

I'd rather have the molten wheel weight metal hit me than fuming nitric acid.

Dave


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## Shark (May 9, 2019)

700*+ molten lead worries you but boiling acid doesn't? You have a window box fan to blow air with? Where would you put the fan that would aid you the best? 

Besides that you ask for a simple method to make nitric acid. I gave you a simple answer, the cold method. It worked for me and it worked very well. If I am going to research methods I most often prefer to waste my time searching for things that pertain to my needs first. I have much to learn yet and that is why I come here everyday. If I can help others in a small way, I will try repay those who taught me by trying to offer help to those with the very basic questions. 

Here, I will hold your hand just once..........

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=19806&p=201787#p201643


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## anachronism (May 9, 2019)

And so you shouldn't Dave. In this circumstance you agree with me, we just have different ways of expressing it. Just because you said it one way and I did another is no different in reality, and given that we both give our time and information freely I have as much right to say it as you do.

My/your information - your/my choice. 

We need less of the entitlement here from people demanding that we give them an A to Z guide.


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## fivel_976 (May 9, 2019)

I did my research and have read many post I asked a simple question as to what temp to distill at no answer. You can read about things all day but until you auctuley get hands on experience your not gonna learn much I came here to seek answers but I'll end up teaching myself as I always do. I seek guidance not lectures on safety but I guess YouTube is gonna be my only option


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## galenrog (May 9, 2019)

If a box fan is all you are using, you may (likely will) harm or destroy your lungs, among other things.

Time for more coffee.


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## fivel_976 (May 9, 2019)

This is not a box fan


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## fivel_976 (May 9, 2019)




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## galenrog (May 9, 2019)

Ok. Wall fan. Unless it is design and installation is for evacuation of toxic fumes, at a rate that would easily satisfy OSHA, it is inadequate, and my short analysis stands.

Still time for more coffee.


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## fivel_976 (May 9, 2019)

It moves alot of air plus I'll probably put up a hood again


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## butcher (May 9, 2019)

I am more worried about you exploding or more likely imploding your glassware apparatus with boiling hot concentrated acid mixture that's when the Stuff hits the fan what good it will do you then?

a simple step like changing temperature can be extremely dangerous.

There are dangers which reading and gaining an understanding of the basics can keep you from harming yourself, some of which you seem to refuse to spend the time on.

How many safety devices on an industrial boiler? Even an experienced boiler operator can cause an explosion or an implosion if his boiler is not operated and maintained properly, Now stand in front of that same boiler made out of glassware with boiling hot acids without the basic understanding of the principles involved and your just a train wreck of a disaster waiting to hit the fan.


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## fivel_976 (May 10, 2019)

I've read alot on safety but to safely operate the still I need details temps amounts


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## goldandsilver123 (May 10, 2019)

There isn't a fixed temperature for doing what you want.

There's several details that needs to be considered, like heat of the flask lost to air, thermal resistance between the flask and hotplate, etc etc etc

To distill a 130 °C compound, 360 °C on the hot plate wasn't enough with the air flow from my fumehood.

Heat to the boiling temp of nitric, if nothing is coming out, increase temperature a little bit, wait half an hour (the system has inertia) and repeat until you get ~1 drop per second.


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## fivel_976 (May 10, 2019)

Ok that helps. Is there something safe I could distill besides water to kinda get a feel for the whole set up is there any common substances that would simulate distilling nitric? I'd rather be safe then sorry but just reading on the topic doesn't help much I'm really a hands on kinda person but I think making a few runs of something this is nontoxic would really help and would help see it all work and to see if I'm sealing my joints properly and that all my equipment is functioning as it should


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## butcher (May 10, 2019)

Even distilling water can be dangerous if not done properly, the NOx gases and the acids are not the only dangers involved.

Without seeing the type of still you plan on using it is hard to give advice on the operation it.

Water for example, when heated to steam expands 1700 times in volume if the vessel is not vented this expansion can become an explosion in a closed vessel, if the heat source is removed from the boiler the steam will condense this fast reduction in volume creates a suction that can suck colder condensed liquid back into the hot boiler or distilling rig full of boiling hot liquid shattering the glass through thermal shock and abrupt pressure changes...

Distilling can be done as safely as making cold poor-mans nitric acid, with the understanding of the dangers and proper operation of the still.


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## g_axelsson (May 10, 2019)

Nurdrage is a good channel on youtube. He does a lot of different distillations with various substances.

Cooling of your setup will affect how the distillation progresses, concentration of the mixture too and even the air pressure. When distilling you can look for the vapor front and make a judgment call at what stage the distillation is at.

If you try to distill a solution with a lot of salts in it, it might shatter the boiling vessel when the salt crystallizes. I suggest that you start with making the acid via the cold method first, then distill the product to clean it up. That way you will have a minimum of salts that crystallizes out , keeping the process safer.

Göran


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## fivel_976 (May 10, 2019)

Here's my set up


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## butcher (May 11, 2019)

I do not like the looks of doing this indoors without a proper fume hood. 
Anything in the room is subject to corrosion.
You need to have adequate air coming into the room to supply the amount of air you are attempting to be removing from the room with the fan, the fans electrical is in the path of any fumes which can become acidic in the oxygen and moisture of the air on the room.

NO gas will not condense, but when mixed with the oxygen in the air of the room this nitric oxide gas will become NO2 gas this nitrogen dioxide gas with any moisture water from the air in the room, air and moisture in your lungs will convert to nitric acid.

I do not like the look of the propane burner and the vessel, a sand bath would help.

Catch basins for spills or worse,
Fire extinguisher. 
GFCI outlets (out of the fumes of the acids).
work outside or get a fume hood.


2NaNO3 + H2SO4 --> 2 HNO3 + Na2SO4 
170 grams NaNO3 dissolved in 100ml H2O and 56ml 98% H2SO4
or 
202 grams KNO3 dissolved in 100ml H2O and 56ml 98% H2SO4

Most important is to study. From the setup and your questions you clearly have not studied the safety aspects, and clearly, have very little understanding of the acids your planning on distilling.


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## fivel_976 (May 11, 2019)

is adding the water important all the videos on you-tube use = amounts of of nitrate and sulfuric acid no water. i could not help myself once i had it all set up i decided to make a run anyway i ended up with some yellow acid blowing into it make white fumes i weighed 50 ml and came out at 72.88 grams im unsure how to calculate the percent tho.


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## anachronism (May 11, 2019)

fivel_976 said:


> is adding the water important all the videos on you-tube use = amounts of of nitrate and sulfuric acid no water. i could not help myself once i had it all set up i decided to make a run anyway i ended up with some yellow acid blowing into it make white fumes i weighed 50 ml and came out at 72.88 grams im unsure how to calculate the percent tho.



By not responding to anyones' safety concerns you're making it pretty clear that you're just ignoring them and carrying on with technical questions. You've made it clear that you're either not listening or think we are being stupid so under those circumstances why should people help you kill yourself and others?


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## butcher (May 11, 2019)

Water added will be helpful in converting the decomposition gases like Nitrogen dioxide back into nitric acid. it will produce less of the nitric oxide gases that would normally just escape the system to make nitric acid in the air around you.

Adding enough water to produce azeotropic 68% nitric would be an ideal mixture, for recovery and refining.
The formula provided above will give a pure nitric acid solution although will make a solution of slightly less than azeotropic nitric acid, when used with but heating the slight excess of water in the solution will easily evaporate to provide you with azeotropic to 68% nitric acid.

Yes, I am concerned with your attitude towards safety and educating yourself so I am also reluctant to provide answers in this thread, as are many others, which would gladly help you if you were less inclined to jump into a dangerous situation, and more inclined to gaining an education and working safely...


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## Lelander (Jan 30, 2020)

I've just recently joined this group, and have kept my mouth shut while trying to learn from all that's offered here, so this is my first post. It's inevitably difficult for a newbie to find his or her way around an unfamiliar forum, but I've been getting a little frustrated by comments like the following one. I'm not asking to be spoon fed, but I think it would help me and others a lot if comments like this were accompanied by a specific reference. In this case, exactly where can I find the proper amounts of nitrate salt and sulfuric acid to use that Lazersteve and others have worked out? I'm all for studying what's been written here on the forum--but first I have to be able to find it.

Lazersteve and others have worked out the proper amounts of nitrate salt and sulfuric acid to use. Mixing 400 grams of each just wastes chemicals.

Don't rely on YouTube videos. Study what's been written here on the forum before you start mixing chemicals.

Dave
[/quote]


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## jarlowski1 (Jan 30, 2020)

Anyone in the Chicagoland area that needs nitric acid I can make it for you just message me


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## Shark (Feb 1, 2020)

Lelander said:


> I've just recently joined this group, and have kept my mouth shut while trying to learn from all that's offered here, so this is my first post. It's inevitably difficult for a newbie to find his or her way around an unfamiliar forum, but I've been getting a little frustrated by comments like the following one. I'm not asking to be spoon fed, but I think it would help me and others a lot if comments like this were accompanied by a specific reference. In this case, exactly where can I find the proper amounts of nitrate salt and sulfuric acid to use that Lazersteve and others have worked out? I'm all for studying what's been written here on the forum--but first I have to be able to find it.
> 
> Lazersteve and others have worked out the proper amounts of nitrate salt and sulfuric acid to use. Mixing 400 grams of each just wastes chemicals.
> 
> ...



https://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=27949&start=30#p294894

Please read the above post. The numbers you seek are there, they just need to be better understood before proceeding.


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