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AztekShine

Well-known member
Joined
Feb 7, 2012
Messages
336
Location
Rogers,AR
I love distilling! It is a beautyful operation. My question is that if I evaporate my nitric off by useing a distillation apparatus and catch the distillate in water how high of a concentrate of nitric acid can I achieve?

I think this tecknique will be safer for everyone. The earth included!
 
if your distilling there's no need to catch the liquid in water. when you distill, the acid will come out in liquid form. catch this liquid in a beaker and transfer to your storage container or use immediately.
 
So the brown nitrogen oxide gas from desolving metal will condense back to nitric acid without the need for water?
 
no, that's not what i said. we are talking about two different processes. what you are talking about isn't distilling. its capturing NOx in liquid to make nitric acid. distilling is when you decompose a pure form of nitrate in sulfuric acid in the presence of heat, that doesn't require capturing the NOx fumes. the method you are asking about will, at best, produce a weak but workable form of nitric acid. i would substitute H2O2 for just water though and chill it in an ice bath to help capture the fumes.

although a small amount of liquid nitric acid will form the way you are talking about, it wont be much.
 
When distilling, we are heating solutions to gases, these gases need to be condensed back to liquid, some types of gases condense back to liquid and some do not convert easily back to a liquid, depending on the gas that is formed.

When dissolving metals we can form gases from the reaction of the acid on metals.

Lets look at nitric acid, as we know when we dissolve a metal with it we create a brown gas, this is not just one gas, and depending on water involved in our nitric solution can determine what form the gas takes, we can say it is ,nitrogen dioxide (NO2), nitrogen oxide (NO), nitrous oxide (laughing gas)(N20), or many of the other gases of nitrogen and oxygen, we call NOx gas to refer to the lot of them, in nitric acid the two we are mainly concerned with are NO2, and NO, the nitrogen oxide gas (NO) needs oxygen to convert to nitrous dioxide gas (NO2):

2NO + O2 --> NO2 (gas)

The oxygen is very important here, as nitrogen monoxide will not make nitric acid (when in contact with water), NO gas would just pass through the solution.

But NO2, nitrogen dioxide when in contact with water does form nitric acid, and does so better with some oxygen present:

4NO2 (g) + 2H2O (L) --> 4HNO3 (aq) .



When distilling Nitric acid (HNO3) we see we need the water.
this water can be part of our boiling solution (and condense) (cool back to liquid)in the condenser, or it can be in our receiver in which we are bubbling our NOx gases into, either way we are distilling and reacting these gases with water to form nitric acid.

So we see we can convert our NOx gas to nitric acid by bubbling them into water, some hydrogen peroxide in our receiver flask can also give the No gas some oxygen converting it to NO2 and in water forming HNO3 in solution.

The longer the gas is in contact with the water the better the conversion, the amount of water in your boiling vessel can be the major factor in determining how strong the nitric will be, if bubbling your gas into water in a receiver (condensing with water there) or (condensing in a condenser with water from reaction vessel), either is distilling nitric acid, you do not need much water if bubbling NOx gases into the receiver, as the boiling vessel is giving water from the reaction also, if you are just dissolving metals in nitric acid collecting the fumes and bubbling into water and some H2O2, you can start with minimum water in receiver, and when gas no longer converts to nitric acid (concentration of acid so high the gas does not react and passes out of solution, then just add a little more water or dilute peroxide.

NO + H2O2 --> HNO3 (plus water)
NO + H2O --> HNO3

How high of percentage of nitric acid we can make depends much on our method used to make the nitric, and since we only need azeotropic nitric for refining. (So that is the strongest I will discuss, we can make this 68% nitric from figuring the mole ratio of our chemicals we add to our boiling distillation vessel (reactor vessel), or we can actually make a weaker nitric acid (such as we need for silver), which is much easier to deal with this solution when distilling, then take this dilute nitric acid solution and then concentrate this up to 68% azeotropic nitric acid solution, as strong as we need for aqua regia.

We can also distill a 35% to 40% nitric solution for use in dissolving silver.

The more dilute solution in our boiling reactor vessel the less trouble we will have with the salts that will be left from our fertilizer and our acid sodium or potassium sulfate's left behind. And we will have less trouble with this "bumping and burning salts or hardening salts inside our reaction vessel.
 
that was kind of a two part question. I confused myself....

Really what I wanted to kno was. When nitric acid fumes is it possable to collect it in water and make nitric acid...

So are both actions Distilling or is the fume collecting just called a reaction?

I see butcher says both are distillation which is the way I understood it. But is their a separate term for "distilling" a gas?

Edit: as to not make another post....
Doubble edit: for some reason ur post didn't show up when I came back to this thread ... :facepalm:
 
To confuse you as much as I am by your question, they are both reactions, and I see little difference in either of these reactions.

The nitric acid dissolving metals and collecting the gas bubbling into water normally it would not be called distilling, unless some heat was added while you were dissolving the metals then it actually could be called distilling, (very little difference), it could also be called scrubbing fumes, or collecting fumes and bubbling into solution, and yes it would make nitric acid. the water would dilute it somewhat, less water less dilution, also when you dissolve a metal in nitric acid a good portion of the nitric acid is converted to a nitrate salt of that metal, only a portion of the nitric acid fumes off as gas, so most of the nitric is used up on the metal, and you will only get a small portion of the nitric acid back in this method, the real bonus to this is you are not wasting gases (and nitric acid polluting our air causing acid rain.

This is a hard question to answer, as I see distilling as making a gas and condensing the gas, we could do this at a low temperature in a vacuum, and here the metals are actually making the gas in a reaction.
Normally distilling is to heat a substance and collect and condense vapor to liquid (metals or chemicals in the reaction vessel can be used to assist the reaction our product formed).

If you need a more technical answer a chemist would need to give you a better answer than I could.
 
Awe he!! Butch your close enough to a chemist :p

From your info. I have an idea of a collection vessel with an inlet, outlet with return, and another outlet with return and maby another with a final outlet. Continues reintroduction of NO gas to H2O2.

The initial idea came from wanting to keep NOx out of the atmosphere.

Edit: to add an x, whoops
 
butcher said:
When distilling, we are heating solutions to gases, these gases need to be condensed back to liquid, some types of gases condense back to liquid and some do not convert easily back to a liquid, depending on the gas that is formed.

When dissolving metals we can form gases from the reaction of the acid on metals.

Lets look at nitric acid, as we know when we dissolve a metal with it we create a brown gas, this is not just one gas, and depending on water involved in our nitric solution can determine what form the gas takes, we can say it is ,nitrogen dioxide (NO2), nitrogen oxide (NO), nitrous oxide (laughing gas)(N20), or many of the other gases of nitrogen and oxygen, we call NOx gas to refer to the lot of them, in nitric acid the two we are mainly concerned with are NO2, and NO, the nitrogen oxide gas (NO) needs oxygen to convert to nitrous dioxide gas (NO2):

2NO + O2 --> NO2 (gas)

The oxygen is very important here, as nitrogen monoxide will not make nitric acid (when in contact with water), NO gas would just pass through the solution.

But NO2, nitrogen dioxide when in contact with water does form nitric acid, and does so better with some oxygen present:

4NO2 (g) + 2H2O (L) --> 4HNO3 (aq) .



When distilling Nitric acid (HNO3) we see we need the water.
this water can be part of our boiling solution (and condense) (cool back to liquid)in the condenser, or it can be in our receiver in which we are bubbling our NOx gases into, either way we are distilling and reacting these gases with water to form nitric acid.

So we see we can convert our NOx gas to nitric acid by bubbling them into water, some hydrogen peroxide in our receiver flask can also give the No gas some oxygen converting it to NO2 and in water forming HNO3 in solution.

The longer the gas is in contact with the water the better the conversion, the amount of water in your boiling vessel can be the major factor in determining how strong the nitric will be, if bubbling your gas into water in a receiver (condensing with water there) or (condensing in a condenser with water from reaction vessel), either is distilling nitric acid, you do not need much water if bubbling NOx gases into the receiver, as the boiling vessel is giving water from the reaction also, if you are just dissolving metals in nitric acid collecting the fumes and bubbling into water and some H2O2, you can start with minimum water in receiver, and when gas no longer converts to nitric acid (concentration of acid so high the gas does not react and passes out of solution, then just add a little more water or dilute peroxide.

NO + H2O2 --> HNO3 (plus water)
NO + H2O --> HNO3

How high of percentage of nitric acid we can make depends much on our method used to make the nitric, and since we only need azeotropic nitric for refining. (So that is the strongest I will discuss, we can make this 68% nitric from figuring the mole ratio of our chemicals we add to our boiling distillation vessel (reactor vessel), or we can actually make a weaker nitric acid (such as we need for silver), which is much easier to deal with this solution when distilling, then take this dilute nitric acid solution and then concentrate this up to 68% azeotropic nitric acid solution, as strong as we need for aqua regia.

We can also distill a 35% to 40% nitric solution for use in dissolving silver.

The more dilute solution in our boiling reactor vessel the less trouble we will have with the salts that will be left from our fertilizer and our acid sodium or potassium sulfate's left behind. And we will have less trouble with this "bumping and burning salts or hardening salts inside our reaction vessel.

Sorry I can't shorten the quote with my iPod ...

When you say fertilizer are you refering to useing H2SO4 and sodium/potassium nitrate?
If I am correct in that method.
 
AztekShine,

Here is how you can make Aztec nitric acid.
You will find much more about this when you study the forum, here is some basic information, but you really need to study the forum and safety and dealing with waste before messing with this acid or any chemicals.

Potassium nitrate, or sodium nitrate can be used with sulfuric acid to make nitric acid.

If making it you can use Laser Steve's recipe, make it according to his instruction
This is from memory so just use it as a guideline, research more about it before making it.
Boil 100ml H2O,
Add 170 grams sodium nitrate (NaNO3)
Or use
Add 200 grams potassium nitrate (KNO3)
Dissolve all of the salts, cool it down,
Very slowly add (as solution will heat by chemical reaction and boil over),
Add 56 ml of 98% sulfuric acid (H2SO4)
Let cool some salts will form, slower the reaction cools the better the conversion and less nitrate will be trapped in sulfate salts that form.
Chill in a freezer; decant the liquid from sulfate salts.
This is about 50% nitric acid (HNO3) approx. 160ml,
This liquid can be distilled for use on silver.
Or this can be used to make an aqua regia solution with heat as is, or it concentrated up to 68% azeotropic solution with heat of evaporation.

The above formula can be scaled up proportionally for larger volumes of nitric acid, (5 times volume of each of the ingredients, and can be done in coffee pot on electric hot plate with solid heating element, (sit pot in casserole dish, do not use a coil type burner, and 2 quart canning jars, use plastic lids, some old peanut butter jar lids will fit).


Formula for above:
Sodium nitrate plus sulfuric acid gives nitric acid and sodium sulfate (solids) salts.
2NaNO3(s) + H2SO4 (aq) --> 2HNO3 (aq) + Na2SO4 (s)
Or
Potassium nitrate plus sulfuric acid gives nitric acid and potassium sulfate salts.
2KNO3(s) + H2SO4 (aq) --> 2HNO3 (aq) + K2SO4 (s)


The sulfate salts I save for other uses.
Stump remover is usually either sodium metabisulfite, or potassium nitrate, depending on brands, KNO3 can also be found as fertilizer, check labels and MSDS, the sodium nitrate is fertilizer, these can usually be found locally or ordered online garden and seed centers.

Sulfuric acid 98% drain cleaner, or you can use new battery acid (32% sulfuric acid battery acid), (5gallons fair price NAPA auto parts), the 32% battery acid can be concentrated up to about 98%, heat below boiling (after concentrated, if white fumes of sulfur dioxide gas (SO2), your concentrated and just wasting sulfuric acid).

You can use lab ware distilling glass, or use a home made setup like I do as long as you understand the safety and care of homemade distilling rig (see my post on killing two birds one stone), here I de-plate gold plated copper pins, collecting gold foils, and make nitric acid (distilling), and copper sulfate all at once in a homemade pickle jar distilling rig.
 
Thanks Butcher! I won't be trying this this week but soon. After i attempt AP - HCL/Cl. Safely Ofcourse!

By the way I was only asking if that was the method you were refering to. But you just saved me alot of time and lost sleep!

Thanks again!
 

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