Anyone here know how to make nitric acid from oleum?

[True Sounds]

Because I know Oleum is Sulfuric acid but do not have a source for the Nitric unless I can convert it somehow. Any help on this project would be greatly appreceated. oleum is Sulfuric acid as a gas and I was wondering if there was a process that would tell or teach me how to make nitric acid from this Oleum.Any ways Nitric Acid is neeeded in a bunch of synths of explosives. Thank you For encouraging me to type more Th0r.
:amish:

[Th0r]

Give us more information. Odin warned you that if you continued not to give more information in the OP then your threads and posts would be deleted, since both he and I view you are attempting to boost your post count.

[death11284]

Yes this is possible, though oleum is not necessarily a gas. First, let me tell you, use the fucking search engine, it's not my job to punish or preach, but I'm still going to preach.

However, I will help you, this one time.
http://www.roguesci.org/theforum/showthread.php?t=1778

[crazy white guy]

Roguesci is down atm. How to make nitric acid in a nutshell:

Get either a retort or round bottom flask. for the RB flask, put it on an angle so that the spout is at a 1 or 2 degree angle. If you have a retort simply put it on a ring stand above your heating element. You mix the sulfuric acid in with Ammonium nitrate or any other stable chemical with many nitrogen atoms compared to other atoms. Once this starts to bubble and change state you heat it to Nitric's boiling point. The acid will pour in gass form into your end receptacle. Its good to have a cooling apparatus between your flask/retort's mouth and your end container.

edit due to bitching on specifics:

Heat evenly over an oil bath if you don't have a Bunsen burner or similar lab grade equiptment that can be used. Urea and Ammonium Potassium (best) Nitrates are the only I recommend but there are many others that you can use.

also, Fuck safety. If you aren't taking the appropriate precautions every time you monitor a reaction, you life is going to be very short and uncomfortable.

[odin_dax]

I don't know if True is just a kid or extremely retarded, but after reading all his recent posts I'll say the latter.

[death11284]

Please, don't follow what CWG said..
There is A LOT more involved in the process, such as deadly fumes...you must have an oil bath, only certain types of material may be used for seals...Yeah..LOTS more

[crazy white guy]

To determine the proper amount of nitrate to use with any given amount of acid, you divide the weight of the acid by 98. Multiply the results by twice the molecular weight of the nitrate that you are using.

For instance, you have 98 grams of sulfuric acid. You also have potassium nitrate. Potassium nitrate has a molecular weight of 101. So, double 101 = 202. Thus, you'd use 202 grams of potassium nitrate with the 98 grams of sulfuric acid.

Though, in actual practice, you'd want to use a slight excess of acid to ensure a complete reaction.

Ideally, when distilling the acid, you'd be using laboratory grade glassware, but even 2 beer bottles could be used in dire circumstances.

To start, place the concentrated sulfuric acid in the container that's going to be heated. Next, add with swirling or stirring with a glass/plastic rod, the dry powdered nitrate. If there's any visible fuming, STOP! Get upwind and wait a few minutes for it to stop. Then continue until all the nitrate is added and well wetted by the acid. There should be no clumps.

If you have lab glass, you already know what to do for a distillation. If you're using a beer bottle still, place the bottle with the nitrate/acid paste in a larger can with a layer of sand on the bottom. Fill the remaining space with more sand the filled, and slide the cut out lid with a hole for the bottles neck over the can. Wire the lid in place.

(The purpose of the sand can is to prevent the glass bottle from shattering from uneven heating.)

Now lay the can on it's side. If you've measured it correctly, then no paste will come out the neck. If any does, catch it in a bowl or such and save it for your next batch.

Now line up the second bottle exactly parallel to the first one, and seal them together using Teflon tape (if possible) or damp cotton cloth (bandages work). The second bottle is the condenser that the nitric acid will be collected in. If using tape, poke a very small hole in the gap between the two bottles to provide pressure relief so the tape doesn't rupture.

Keep this second bottle well cooled. You can do this by wrapping it in a small towel and having a constant stream of cold water from a hose flowing over it. Or wrap it in ice. However you do it, keep it as cold as possible.

Proceed to gently heat the bottle using a gas or charcoal fire. You don't want to overheat the paste which would cause some to carry over into the receiving bottle.

You'll know the reaction is done when no more fumes are seen to be in the bottles.

At this point, remove the heat and allow the assembly to cool down while keeping the receiver cool.

Carefully seperate the two bottles, being careful to wear acid resistant gloves and staying upwind of the assembly.

This is what I got from the archive, Its my version with a bit more detailed into.

[Anders Hoveland]

Oleum is not just sulfuric acid. It is SUPER-concentrated sulfuric acid. Usually around "120%".
This is because if more water is added, pure 100% sulfuric acid is formed.
However, adding plain water to oleum should NEVER be done. As soon as a drop of water was added, it would cause the oleum to dangerously spray upward. Normally, oleum would be slowly and carefully added in small ammounts to 70% concentrated sulfuric acid to dilute it.

Oleum can be considered a mixture of pure sulfuric acid and PYROsulfuric acid, with a structure HOSO2OSO2OH.
Oleum is made by reacting sulfur trioxide with concentrated sulfuric acid. Oleum can be useful to perform nitrations. Nitrations usually require 98% acid, but during a nitration water is generated that quickly dilutes the acidity. This means that a large volume of 98% sulfuric acid is required to do a nitration on a very small ammount of whatever is being nitrated. However, oleum is a strong dehydrating agent (stronger than pure sulfuric acid) and so it quickly absorbs water. It takes several times less oleum to do a nitration than the ammount of sulfuric acid that would be required.

[madscientist]

Also, since hydration of oleum is more exothermic than that of sulfuric acid, it allows nitrations to be effected that are otherwise unworkable, such as that of DNT.

[digermane]

It's more accurate to say that oleum is a sulfuric acid generator than concentrated sulfuric acid...

[Leshrac]

Because I know Oleum is Sulfuric acid but do not have a source for the Nitric unless I can convert it somehow. Any help on this project would be greatly appreceated. oleum is Sulfuric acid as a gas and I was wondering if there was a process that would tell or teach me how to make nitric acid from this Oleum.Any ways Nitric Acid is neeeded in a bunch of synths of explosives. Thank you For encouraging me to type more Th0r.
:amish:

Sulfuric acid + Ammonium/Potassium Nitrate + heat = Nitric Acid.

http://www.youtube.com/watch?v=2yE7v4wkuZU
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[Anders Hoveland]

Well, actually NH4NO3 is not the best source of nitrate when using with concentrated sulfuric acid. Nitroglycerin can be made from NH4NO3 and sulfuric acid, the advantage is that NH4NO3 is much more soluble than KNO3, but there is also an undesirable side reaction. The concentrated H2SO4 dehydrates the NH4NO3 and N2O is produced.

[digermane]

Did you seriously just say that producing NO2 in vivo is a bad thing when the reaction is attempting to produce nitric acid?

[Anders Hoveland]

That is N2O (nitrous oxide), not NO2 (nitrogen dioxide).
But, yes, nitrogen dioxide is not considered desirable for the nitration of alcohols, because it promotes further oxidation of the alcohol into carboxylic acids.
However, a nitration on an alcohol can be performed using only NO2 with only moderately concentrated acid (20% HCl), there will just be lower yields, and organic byproducts.
The reaction proceeds by the formation of nitrous acid from the NO2, and then the nitrous acid forms an nitrite ester under the moderately acidic conditions (nitrate esters require much more acidity to form). The nitrite ester must then be removed from the solution (it is will be oil soluble). Finally, nitrogen dioxide can be bubbled into a solution of the nitrite ester in a hydrocarbon solvent, oxidizing the nitrite to a nitrate. The formation of nitrate cannot be done when the alcohol is dissolved in water, otherwise the the nitrate ester will quickly react with water, even in 20% HCl solution.

You may be wondering about some of the NO2 oxidizing the nitrite ester when it is still forming in the 20%HCl solution. There is an equilibrium.
CH3OH + HNO2 + NO2 <--> CH3ONO + H2O + NO2 <-->
CH3ONO2 + H2O + NO <--> CH3OH + HNO3 + NO <--> CH3OH + (2)HONO

[madscientist]

References?

[Anders Hoveland]

see shadow RX forums, where there are pictures of a procedure using sodium nitrite and HCl to make isopropyl nitrite from the alcohol.

also see http://pubs.acs.org/doi/abs/10.1021/jo00863a019 where it is described that NO2 forms nitrite esters with cellulose

To quote from a patent: "When nitrogen dioxide is reacted with the alcohol in the presence of water at temperatures below 250° C., equimolar proportions of the nitrite ester and nitric acid are formed. By increasing the temperature of the reaction to 350° C., the formation of nitric acid was almost eliminated, and the conversion to nitrite ester increased."

[madscientist]

Finally, nitrogen dioxide can be bubbled into a solution of the nitrite ester in a hydrocarbon solvent, oxidizing the nitrite to a nitrate.

That's the part I want to see a reference on.

[Anders Hoveland]

Here are two quotes from the literature:

"oxidation of nitrite ester to nitrate ester by hydroperoxides"
Mechanisms of antioxidant action: The photo-antioxidant behaviour of nitroalkanes S. Al-Malaika, Aston University, UK

"the nitrite ester being oxidized to the nitrate ester in the presence of excess dinitrogen tetraoxide"

Obviously dinitrogen tetraoxide is just cold NO2. "hydroperoxides" almost certainly refers to organic peroxides, it is doubtful that plain H2O2 could be used because an organic solvent is required to avoid hydrolysis of the nitrate ester.

[digermane]

"the nitrite ester being oxidized to the nitrate ester in the presence of excess dinitrogen tetraoxide"

Obviously dinitrogen tetraoxide is just cold NO2. "hydroperoxides" almost certainly refers to organic peroxides, it is doubtful that plain H2O2 could be used because an organic solvent is required to avoid hydrolysis of the nitrate ester.

You do realize that "dinitrogen tetraoxide is just cold NO2." is a very significant statement about the reaction conditions, right? You cannot make a significant change in the reaction conditions and expect a reaction to still work.

As to your statement about hydrogen peroxide... kinetics kinetics kinetics.

[Anders Hoveland]

Throughout the literature, they refer to NO2 and N2O4. The cold form is just more conventient to work with, since NO2 solutions give of irritating fumes.

[digermane]

The form is a function of temperature and pressure. Endergonic reactions are not done in a slush bath for a reason.

[Leshrac]

see shadow RX forums, where there are pictures of a procedure using sodium nitrite and HCl to make isopropyl nitrite from the alcohol.

Isopropyl nitrite is made using sulfuric acid.

Don't bother arguing, I made and sold liters of this stuff :-)

[-=HeX=-]

Lehsrac: You may have sold liters of the stuff, I myself made a large amount for use in fuel-air munitions and found the HCl method FAR easier to use. Probably because HCl was cheaper and easier to control temp-wise than the H2SO4, but I digress. Any decent acid would work...