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Author: Subject: help make white fuming nitric acid.
Luftwaffe
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[*] posted on 1-10-2011 at 23:28


I do not believe distilling nitric using HCL would be possible considering Aqua Regia is the mixture of HCL and Nitric Acid.

Consider the reaction,

HNO3 (aq) + 3 HCl (aq) → NOCl (g) + Cl2 (g) + 2 H2O (l)

As well as,

2 NOCl (g) → 2 NO (g) + Cl2 (g)

I believe your yields would be bad and would require a very good scrubber or ventilation to deal with all the toxic and corrosive gasses. Even if you tried to distill nitric from a mixture of HCL and a nitrate salt it would take so much time to get a reasonable amount of product. Time is money, and I think spending a few extra bucks on some drain cleaner is better than a few days of frustration.


Sources: Wikipedia, personal knowledge.

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AndersHoveland
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[*] posted on 2-10-2011 at 01:22


Quote: Originally posted by Luftwaffe  
I do not believe distilling nitric using HCL would be possible considering Aqua Regia is the mixture of HCL and Nitric Acid.

HNO3 (aq) + 3 HCl (aq) → NOCl (g) + Cl2 (g) + 2 H2O (l)



Actually, that reaction is an equilibrium reaction. It tends to go to the right when the acids are very concentrated, but more often the reverse reaction happens when the reactants are more dilute. NOCl actually hydrolyses with water to nitrous acid and hydrochloric.

NOCl + H2O --> HNO2 + HCl

In the presence of water, chlorine easily oxidizes nitrous acid.

HNO2 + H2O + Cl2 --> HNO3 + (2)HCl

So the net reaction is just the reverse, assuming of course that the acids are dilute. Even in 30% concentrated acids, the equilibrium primarily exists in the form of HNO3 and HCl, although there is enough equilibrium to attack gold.

All too often, seamingly simple reactions are actually much more complicated. Most of the time, for convenience, we like talking about the simple net reaction, but these types of generalisations do not hold true for all conditions.




I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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Steve_hi
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[*] posted on 2-10-2011 at 09:57


Just checked in on my nitrica acid today Ive been keeping it in a small fridge that wasnt turned on when I opened the door I stunk the whole place up. The nitric acid ate all the rubber seal and turned it to mush and was eating the steel bail that keeps the lid down. I think the first thing to do in the synthesis of Nitric acid is to have a suitable container to store it in.

[img]C:\Users\Steve\Pictures\2011-10-02\1.jpg[/img]

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quicksilver
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[*] posted on 2-10-2011 at 11:55


Teflon (type) seals / stoppers or "glass to glass" (roughened glass stoppers)..... Few other materials will appropriately seal HNO3 for any period of time. But keeping it cool and away from UV (dark amber glass) IS a smart idea.





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Steve_hi
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[*] posted on 2-10-2011 at 15:30


I had an idea this afternoon I was thinking to use a brown beer bottle and machine a flat piece of aluminum the size of the OD of the beer bottle neck and put it inside the bottle cap since Aluminum is not reacted by nitric acid it should suffice as a seal ?? Not that I dont want to buy a proper bottle but pro lab scientific wants 15 dollars for a bottle and it is only hdpe cap plus the shipping
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AndersHoveland
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[*] posted on 2-10-2011 at 21:06


Quote: Originally posted by Steve_hi  
... since Aluminum is not reacted by nitric acid it should suffice as a seal ??


Aluminum is actually resistant to nitric acid if the acid concentration is over 95%, but if the concentration is below 80%, or if the nitric acid is heated above 40degC, the corrosion rate is much faster.
This is only for handling nitric acid. If the nitric acid is to be stored for long lengths of time, aluminum is probably not advisable, as it no doubt would gradually corrode over time.




I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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Luftwaffe
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[*] posted on 2-10-2011 at 21:45


Instead of aluminum, just line the cap with teflon tape. I intend on storing my nitric with glass perfume bottles with teflon tape lining the plastic cap. I buy my reagents from prolab, I was quite dissapointed over there reagent bottles so I have to improvise. :(
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AndersHoveland
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[*] posted on 3-10-2011 at 00:07


would like to share an interesting reaction from the literature of Marcellin Berthelot, dry ammonia gas reacts with the nitrogen dioxide and nitric oxide, at room temperature,

(2)NO2 + (2)NO + (4)NH3 --> (2)NH4NO2 + (2)H2O + (2)N2

Solid ammonium nitrite inside a tube explodes if heated on a water bath to between 60-70degC. And the substance gradually decomposes at room temperature, slower if cold, or faster in aqueous solutions, forming nitrogen gas.





I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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Steve_hi
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[*] posted on 6-10-2011 at 12:27
Nitric acid from CAN


Someone mentioned that CAN "Calcium Ammonia nitrate" could not be or would be difficult to use as the nitrate for this synthisis but to day i repeated my previous distillation with NH4NO3 that I got from CAN fertilizer and I had no problem with it, it worked fine.

[img]C:\Users\Steve\Pictures\2011-10-06\1.jpg[/img]

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hissingnoise
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[*] posted on 7-10-2011 at 01:11


Hot, concentrated sulphuric acid is a good oxidiser and will oxidise the ammonium ion, introducing water and diluting the distillate!
Use an alkali-metal nitrate for the highest concentration of HNO<sub>3</sub> . . .


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Steve_hi
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[*] posted on 7-10-2011 at 01:25


I have a number of different nitrates can you mix the nitrates and do this synthesis. like KNO3 and CaNO3 and I have BaNO3 I ordered by mistake just curious bout all these diffent nitrates I have and dont know what I will do with them

Got overexxcited about learning chemistry when I was ordering chemicals:D


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hissingnoise
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[*] posted on 7-10-2011 at 03:50


The sulphates of barium and calcium being insoluble will complicate things.
K and Na nitrates are ideally suited for preparing HNO<sub>3</sub>.

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Luftwaffe
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[*] posted on 7-10-2011 at 04:24


If you use CAN fertilizer, make sure you know the percentages of each nitrate or you may be using too much of an excess or too little sulfuric acid in your nitric synthesis. Basic stoichiometry I know, just making sure! :D
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[*] posted on 7-10-2011 at 06:14


hissingnoise :

Some interesting idiosyncratic elements about CAN. The Yara product may have been one of the few ammonium nitrate products to halt the use of a FGAN to be used as an ANFO or energetic. A great deal of research was put into the final Norwegian export product. When exposed to water the Yara product yields a "Glue like material" that clogs a filter. It's a Carboxylate polymer [and] is somewhat a generic term as it could mean China Clay and oil or a synthetic. It is obviously a “trade secret” as it’s not totally spelled out in their patent. The original is Norwegian and I couldn't get an English copy. The US was 6,930,139 and gave enough info to develop two mechanical methods of extraction. And there may be a chemical method of extraction but the recovered material would be KNO3 rather than the original nitrates. The mechanical processes work well but one is somewhat slow and the other requires a moderate amount of tools in construction. I had some fun figuring out workable extraction techniques: however I take my hat off the Yara as their prilled product (IMO) would be safe for sale unless the user to some real time in examining the techniques to isolate the original NH4NO2.

From a utilitarian stand-point, Yara may have stopped the common abuse of NH4NO3 from dangerous, unskilled use as a blasting agent. The market they have at this time is very large. NH4NO3 will only be sold [in configuration similar] as a bagged product. It is still available to agriculture via truck (unbagged- delivery) but there will be a minor registration process - all laws available via the DHS page, etc.
This IS a multi billion dollar market, when all is said and done.

The interesting thing was that many people have attempted to put the breaks on bagged ammonium nitrate access by the public and the Yara company may have been the first to come close. They have succeeded in grabbing the US/CA market of bagged FGAN, which is quite an accomplishment.
The Dept. of Homeland Security (DHS) has proposed ('08) & got enacted into law a national focus on NH4NO3. If you ever do want to check out what lengths the DHS had gone to so as to grab a headline or two and give themselves a little promotion check out: "the Secure Handling of Ammonium nitrate Program" DHS, (see attached summery), the bulk can be Googled as well as the specifics.

The new laws for the US deal with bagged NH4NO3 and are already in effect. but as many people have said through out the years it would be consistently possible for a skilled / clever individual to be able to extract ammonium nitrate from a prill-based starting material. It's just that Yara had come the closest so far.

Attachment: AN_ANPRM.pdf (254kB)
This file has been downloaded 600 times






[Edited on 7-10-2011 by quicksilver]




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Steve_hi
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[*] posted on 7-10-2011 at 07:23


Interesting how goverment agencies and the general public can be so stupid.
How many people have been blown up by NH4NO3
How many people have died from tobacco
How many people have died from hand guns
How many people have died from alcohol and families ruined in the process
How many people have died from patent protection barring people from being able to afford life saving medications , simply to protect the wealth of the richest people in the world.\

Trudeau said "The public is an ass" HE WAS RIGHT
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hissingnoise
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[*] posted on 7-10-2011 at 08:08


Quote:
How many people have been blown up by NH4NO3

It's AN's potential for blowing people up rather than the numbers but historically AN does have a reputation.
State agencies can attempt making its extraction 'difficult' but that's all they can do!
Small hurdles for anyway committed terrorists!
And they know it . . .



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quicksilver
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[*] posted on 7-10-2011 at 11:11


Quote: Originally posted by Steve_hi  
I had an idea this afternoon I was thinking to use a brown beer bottle and machine a flat piece of aluminum the size of the OD of the beer bottle neck and put it inside the bottle cap since Aluminum is not reacted by nitric acid it should suffice as a seal ?? Not that I dont want to buy a proper bottle but pro lab scientific wants 15 dollars for a bottle and it is only hdpe cap plus the shipping




Teflon stoppers ARE available and are worth the effort to buy. As you know HNO3 absorbs water fairly quickly from almost any exposure. While amber glass is a good idea, I would do all I could to achieve a safe and air-tight seal. What's more you certainly don't want them to break & thin commercial glass may not be the best choice; more so because they are designed poorly and tip over easily.
Common "black rubber" stoppers simply can't be sealed effectively against a strong acid's fumes and the mess they make when decomposing is disgusting.
There are polyurethane stoppers that have been wrapped in Teflon tape and appear to last for a few weeks but they also decompose. Teflon stoppers are really the best choice. They aren't cheap but they will last for many years of active use in most common caustics.




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[*] posted on 7-10-2011 at 20:08


Remember this is bad stuff, they mix it wife jet propulsion kerosene to make ICBM rockets fly! My father dealt with this stuff in the US ARMY guided missile division.



History is repeating itself.
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Eyro9001
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[*] posted on 7-10-2011 at 21:21


I have yesterday manufacture of nitric acid by distillation way
The quantity = 17ml
weight = 27g
Density = 1.59
!!!!
(the color is very yellow)
How much is the concentration of the acid?
Is there a problem?
How do I know the presence of oxides of nitrogen in acid or not

Note
This my first experience in the manufacture of nitric acid

Thanx >>>

[Edited on 8-10-2011 by Eyro9001]
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Luftwaffe
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[*] posted on 7-10-2011 at 22:07


I shall give you the answer, UTFSF! Concentration can easily be found from density charts on the internet and oxides of nitrogen can be seen by mere visual observation. You can even use NOx scrubbers to rid of all traces of them which has been discussed in many posts on SM, search to ascertain the answers you seek.
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[*] posted on 8-10-2011 at 03:00


Luftwaffe :
Quote:

Concentration can easily be found from density charts on the internet

Yeah I know that, but the density is 1.59 ! not found in table of concentrations. (that mean up of 100%!!!)

Quote:

oxides of nitrogen can be seen by mere visual observation

Explain this point please, or give me the links
Thank you very much
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Steve_hi
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[*] posted on 8-10-2011 at 06:10


I think that the fact it is yellow in colour signifies NO because pure HNO3 is clear in colour
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hissingnoise
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[*] posted on 8-10-2011 at 06:56


Gaseous NO<sub>2</sub> is a dark reddish brown colour but the dimer N<sub>2</sub>O<sub>4</sub>, existing at low temperatures, is colourless . . .


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Luftwaffe
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[*] posted on 8-10-2011 at 14:30


Eyro, how precise and what volume of acid were you measuring? When calculating densities even a small inaccuracy is a big deal if your only measuring a few mL of acid. Perhaps scale up your measurement and see if your results change.

As for the equilibrium between NO2 and N2O4, you can shift the equilibrium towards making NO2 by chemically removing NO2 with a scrubber forcing the reaction to completion.

N204 --> 2 NO2

[Edited on 8-10-2011 by Luftwaffe]
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hissingnoise
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[*] posted on 9-10-2011 at 05:46


In this case, the equilibrium is solely temperature-dependent.

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