Nitric acid production questions

[anachronism]

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.

 

[fivel_976]

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

 

[galenrog]

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.

 

[fivel_976]

This is not a box fan

 

[fivel_976]

 

[galenrog]

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.

 

[fivel_976]

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

 

[butcher]

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.

 

[fivel_976]

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

 

[goldandsilver123]

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.

 

[fivel_976]

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

 

[butcher]

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.

 

[g_axelsson]

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

 

[fivel_976]

Here's my set up

 

[butcher]

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.

 

[fivel_976]

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.

 

[anachronism]

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?

 

[butcher]

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...

 

[Lelander]

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]

 

[jarlowski1]

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