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Easy Fuming HNO3 90%+, and Electro-Azide Fun

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LutzH

Tue Jan 05 2010, 07:49PM

Registered Member #1721 Joined: Sat Sept 27 2008, 08:44PM
Location:
Posts: 136

Hello:

Due to the subject of fuming nitric acid always causing a lot of discussion I just wanted to present my solution to the problem of making it which I worked out about 20 years ago, I have yet to see a better more easy method presented anywhere. It of course hinges on the availability of common industrial 65-72%HNO3. I figured I would also throw in a HV electro-chemical experiment which can be fun, and legal to boot. This way if you want a bigger bang then just get a bigger capacitor, this is legal, and it will not get you in trouble. My feeling is that fuming HNO3 is not a good thing to play around with, but if you must do it then you might as well do it correctly. So I am presenting this for informational purposes only.

Basic Chemistry Review:

H2SO4 and H2O form a constant boiling mixture at about 78% max, so by boiling a water solution of H2SO4, the best that you can hope to achieve is 78%, I believe the term was azeotrope.

H2SO4 drain cleaner sold at Ace is about 92%, so it is much more easy to just buy it. If you want to make white fuming HNO3 90%+ just mix equal volumes 90%+ H2SO4 and commercial 65-72% HNO3, then distil the mixture until 2/3 of the original volume of the 72%HNO3 used, distils over. Bingo you are done. I once made 3 liters of it in a day. This is a hobby that I gave up way before 9/11, it is just to hot of an item to have in a legal sense, especialy post 9/11. This is a simple dehydration reaction, the H2SO4 retains the water from the HNO3 solution, then HNO3 then distils over easy due to its low BP. The leftover now about 70-78% H2SO4 can be added to NaNO3 to make even more HNO3.

I have done the H2SO4 + NaNO3 and KNO3, Na works better, but it tends to clog your condensor and form frothy boiling mixures at the middle to end. Using conc. 90-98% H2SO4 to dehydrate commercial 72 or 68% HNO3 is sooo much better.

If you are using the fuming nitric to clean glass and quartz for high vacuum and plasma tubes for laser work then fine, but if you are tempted to go in the "boom" direction my advice is JUST DONT DO IT. A long, long, time ago when the world was a different place it was fun to build a fat single layer magnetic coil, with a piece off copper pipe in the center hole filled with PETN, or EDNA (Ethylenedinitramine) You did not need fuming nitric for EDNA). The capacitor which energized the main coil was in the same circuit as the exploding wire assisted initiator at one end of the copper tube. What happens next is the interesting part:

The magnetic flux in the outer coil is shorted by the expanding copper pipe causing the magnetic flux to compress towards the end until it builds to levels that are un-imaginable. When the end of the coil is connected to an antenna, or a special microwave tube you have an EMP device which will fry anything within several hundred meters to 1KM, so this is not something which can be done anywhere near civilization!!! Also you need to obtain the needed permits and licenses. Believe it or not it can be done, and they do get approved. This is also far cheaper also than the attourney bill for your first hearing, just fill out the forms, put in the check, and talk to the guys in suits, then go have fun legaly :) It would be interesting to see if this magnetic pulse could be used for a mini fusion energy pop in some way. Maybe these kind of experiments could be combined with avalanche control opperations? If you talk to the right folks, maybe they would not mind a wire coil around their charge in the interest of science. You could even throw out the idea that all the iron bearing rocks in the area will "pulse" to help enhance the avalanche control effort :) Yahhh Right, but who knows, no one has tried it.

What can also be fun is working with legal amounts of initiators, like lead and silver azide. Sodium Azide can be harvested from old style air bags by just recrystalization once soluabilized. The lead salt when formed without Dextrin in the solution, can form large crystals which can detonate upon fracture. Forget the copper salt also, it can go off with a feather touch. The silver salt is interesting, we used to make legal amounts, and put about 50mg on electric Estes rocket engine ignitors, then place it between two electrodes which were connected to a large 50KV .1mfd HV capacitor. When the Silver Azide detonated the cloud of now ionized metalic silver acted as a good conductor and wow!!! This was good fun because it was all one big bang with most of the energy coming from the capacitor. You have to respect the silver azide, it is an even more efficient detonator than the lead salt, more stable and safer to boot, its just to expensive for commercial use. Do not try this with sterling silver as a starting material, it has copper in it! Check the law, but you used to be allowed to have up to 100mg of explosive materials without a permit / license, a quick call to the BATF could comfirm this.

I think it would be fun to try this same setup, with just a air "puffer", and a tiny glass funnel below the electrodes filled with aluminum powder. Puff the funnel and bang! This should give on heck of a UV pulse also. I just wanted to present this a safer legaly firm alternative. This way you can enjoy your bang free from worry :)

MinorityCarrier

Tue Jan 05 2010, 09:47PM

Registered Member #2123 Joined: Sat May 16 2009, 03:10AM
Location: Bend, Oregon
Posts: 312

Unlicensed manufacture of explosive metal azides in the U.S. is a felony. This is probably not a permitted subject for discussion in this forum, I'll let the moderator make that call.

rp181

Wed Jan 06 2010, 01:30AM

Registered Member #1062 Joined: Tue Oct 16 2007, 02:01AM
Location:
Posts: 1529

you described a Explosively pumped flux compression generator.

I will stay away from the chemistry portion :)

Steve Conner

Wed Jan 06 2010, 10:45AM

Registered Member #30 Joined: Fri Feb 03 2006, 10:52AM
Location: Glasgow, Scotland
Posts: 6706

MinorityCarrier wrote ...

Unlicensed manufacture of explosive metal azides in the U.S. is a felony. This is probably not a permitted subject for discussion in this forum, I'll let the moderator make that call.

I'll let the government agents that browse 4hv in their lunch breaks make the call.

My only gripe would be that the post is a classic example of grandstanding. It seems to me that LutzH just wants to boast about the dangerous stuff he's done rather than contribute anything useful.

Bored Chemist

Wed Jan 06 2010, 12:22PM

Registered Member #193 Joined: Fri Feb 17 2006, 07:04AM
Location: sheffield
Posts: 1022

"H2SO4 and H2O form a constant boiling mixture at about 78% max, so by boiling a water solution of H2SO4, the best that you can hope to achieve is 78%, "
Just plain wrong.

radiotech

Wed Jan 06 2010, 03:51PM

Registered Member #2463 Joined: Wed Nov 11 2009, 03:49AM
Location:
Posts: 1546

Kartsev. V.P. Three Thousand Years of magnets -Mir- Publishers Moscow (translated from the Russion by Ann Feltham 1975 from the 1971 Russian Edition.) On page 82, the magnetocumulative techniques described by LutzH in the thread post are diagrammed and described. A careful read of this book might be interesting the the rail gun people especialy concerning magnetic stampers.

LutzH

Wed Jan 06 2010, 07:38PM

Registered Member #1721 Joined: Sat Sept 27 2008, 08:44PM
Location:
Posts: 136

Hello:

Just to clear up a few points...

On the H2SO4, I stand corrected, yes its 93% if you have a sophisticated industrial setup with fractioning columns, and with pressure control. In a simple home set-up the basic 70-80% figure stands, see the cut and pasted notes below, direct from a H2SO4 industry publication. I suppose with a fractioning column, which can be done at home, you could maybe get 85+ %. I would however not want to be any where near 330 deg. C sulfuric acid. This stuff is bad enough at room temp. This is one acid to respect because the reaction products with tissue are toxic, so the burns heal very slow, and are nasty. At 300+ deg. it would be worse than blister agent, no thanks, I will just buy the tiny amounts that I use to pickle gold at Ace!

My intent is not to "grandstand" we have enough folks doing this already when they for example display large arcs coming from conventional big tesla coils etc, here there is plainly no new, or useful scientific information to be learned. When these same coil designs are repeated over and over, and even shown arcing into body parts, this is "grandstanding".

I have over the years learned tollerance, so I will not judge these folks, or label them with such terms. Let them have their fun, its ok, if it brings them a smile and makes them happy, then fine more power to them. I will refrain from being a self appointed expert on what is "Useful" or Scientific". Instead I will try to shift my perspective towards where they are, then maybe if I am lucky then I can even share a little of their excitement.

Danger, yes in large amounts energetic substances can be a very real hazard. But letâ€™s put this into perspective:

Remember the label on the capacitor that you have which reads: "Warning the charge stored in this capacitor is lethal" I could go on and on here, ending a ten page list with the gasoline can in the garage.

In my case this experimentation led to my becoming an EOD technician, which then in turn led to college and a productive life. I would like to offer my sincere apology if I did not stress enough in the posting: "not to do this". I understand at the same time the reality of the attraction of this area of experimentation, so my point in the posting was to offer some constructive guidance towards science in this area, away from blowing up garbage cans, and other stupid stuff. This is why I repeated several times the need to work with the government, and not against it.

The bottom line is that everything has its place, and we all have to use good judgment. In youth this judgment is often lacking: It was in my case, I had no guidance in this area, I am just one of the lucky ones with all of my fingers and hands. Sometimes it can be beneficial for the younger folks to read about the mistakes made by us older guys. This is in part why I suggested sticking to very tiny mg amounts if you have to, or if you feel a need to go there.

When I read the chemistry thread in this forum, it quickly became very clear to me, that quite a few folks were doing kind of experimentation. Yes they were being "politically correct" and they danced around the issue, in a feeble attempt to hide what they were doing. It is precisely these folks, who I wished to get through to, not as a scolding parent or authority figure, but as someone who has been there and seen that non scientific experimentation here, is not going to bring you anything but trouble.

Magnetic flux compression is science, and it still holds the world record for the most powerful magnetic field ever generated (Other than some nSec marx bank events). This forum is dedicated to HV and the related science, and like it or not it overlaps in some areas with energetic events and substances. So if you are one of the folks experimenting in this area: I will repeat it again since it seems that it was missed in the original posting:

I DO NOT THINK THAT THIS IS AN AREA WHERE YOU SHOULD BE EXPERIMENTING!!!!

If you however choose to ignore this advice, then please: DO IT IN A LEGAL WAY, GET THE PERMITS, and most important the guidance.

Please do not insult the intelligence of the readers with posts on "Fuming Nitric Acid" and then claim some bizarre use, all the while intending to "pull the wool over the forum moderatorâ€™s eyes". The moderator is allowing the posting not because you fooled him, but rather because he is extending trust, which is an admirable character trait, and a sign of integrity. I will end this post with a quote from Frank Zappa:

The single most important lesson that I have learned in my life is: "That in all of my battles, between myself and the world, I have learned to back the world."

H2SO4 Industry Notes:

The System Sulfuric Acid / Water
The sulfuric acid / water system displays a maximum azeotrope at 93.3 wt% sulfuric acid concentration and a temperature of 338Â°C at ambient pressure conditions. A large separation factor exists as may be seen in illustration 1. Furthermore, almost no sulfuric acid is contained in the vapour up to a concentration of about 70 wt%. The vapour concentration of the sulfuric acid increases very strongly only from a fluid phase concentration of about 85 wt%.

The following notes for the concentration of sulfuric acid may be derived from the equilibrium data and the vapor pressure curves:

One cannot achieve 100% concentration by performing water dehydration due the azeotrope. Yet, it is more economical to perform concentration only up to a maximum sulfuric acid concentration of 96 wt% due to the possibility to increase the concentration by adding SO3.

One may operate with simple-design evaporator facilities up to a final concentration of about 70 wt%, due to the low partial pressure of sulfuric acid in the vapor phase.

In the so-called range of high-concentration displaying concentrations higher than 70 wt%, supplementary measures are necessary in order to reduce the proportion of sulfuric acid in the distillate.

PS: Has anyone tried magnetic flux compression by electromechanical means instead of explosive? If for example you placed an exploding wire inside of a water filled Cu tube, would it, or could it be made to expand it in the same way? If this pulse were fed into a HV pulse transformer it could be interesting.

MinorityCarrier

Wed Jan 06 2010, 09:55PM

Registered Member #2123 Joined: Sat May 16 2009, 03:10AM
Location: Bend, Oregon
Posts: 312

You neglected to mention that sodium azide is extremely poisonous, can be absorbed through moist skin, etc.

LutzH

Thu Jan 07 2010, 12:10AM

Registered Member #1721 Joined: Sat Sept 27 2008, 08:44PM
Location:
Posts: 136

Good Point!!!

Sodium Azide is very toxic, about 1/2 of Cyanide, and 1/3 of Nicotine. Since there are some other things about it like adding acid liberating toxic gasses ect, a thorough review of an MSDS sheet would be in order before using it in any way. Also the azide salts of some elements like Strontium are neat. Sr azide will not detonate unconfined in small amounts, but it will give a nice deep red spectral flash. One thing to keep in mind with the alki azides is that upon decomposition the metalic alki element is the by-product, which can be nasty. This is also the reason they trigger spark gaps so well, the metal vapor.

In airbags the sodium azide was mixed with other chemicals so as to finaly form sodium silicate. this prevented the vehicle occupant from getting hit with a cloud of sodium vapor, or lye dust. The air bag units themselves are also a major hazard if they were to be triggered while in someones hand ect. Maybe better to just stay away from this period. Fulminates are however even worse, especialy Mercury. Releasing puffs of mercury vapor is nasty period anywhere. Currently even the government is looking for a replacement for lead azide due to the enviornmental aspects of lead. Silver azide is in the running for this. For a triggered spark gap, only 10mg was enough. We got our sodium azide a long time ago when it was used as a buffer in several medical lab solutions. This was about 20 years ago, so I have no idea if it is still used this way.

Well enough chemistry for a while, now days the only chemistry I do relates to precious metals. Refining gold can be fun and constructive.

Proud Mary

Sat Jan 09 2010, 10:15AM

Registered Member #543 Joined: Tue Feb 20 2007, 04:26PM
Location: UK
Posts: 4992

Reckless, irresponsible, dangerous, illegal, and likely to end in lengthy imprisonm,ent in the United Kingdom, for both the unlicensed production of explosives, and possession of articles likely to be of use to terrorists, which is anything the terror police say it is.

Let's hope that self-appointed jihadis, or the type of nutcase that blows up gay pubs, and clubs for people of colour, hasn't read and understood this foolishness.

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