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Author: Subject: anhydrous liquid ammonia
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[*] posted on 31-12-2007 at 21:39
anhydrous liquid ammonia


I hopped down to the Sheriff's to pick up my concealed carry renewal and while I waited picked up the local methlab threrat pamphlet. Lots of hysteria and photos (I'd be happy to scan it). Implicit in part of was that liquid anydrous amonia could be made from (NH2)2SO4 fertilizer. I couldn't find a thread but would like to know how and whether it makes economic sense for the legal experimenter.
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Sauron
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[*] posted on 31-12-2007 at 21:56


What pray tell is (NH2)2SO4 ?

Do you mean (NH4)2SO4 ?

Because that is what is in UAS fertilizer (urea-ammonium sulphate).

One of these days the narcs are going to read about fixation of atmospheric nitrogen and they will want to declare air a List One chemical.

Clearly, the most faile way to obtain anhydrous ammonia is to remove it from commercial ammonium hydroxide solutions, preferably 28% reagent NH4OH, or if you can't get that, 10% hosehold ammonia.



[Edited on 1-1-2008 by Sauron]




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evil_lurker
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[*] posted on 1-1-2008 at 12:07


Sauron is correct, ammonia solution will disproportionate rather easily by bringing the temp up in the 90-95ºC range (all the ammonia is gone when boiled, but that brings over water which isn't a good thing).

And, as a bonus, 28% ammonium hydroxide solution is ORM-D in gallon quantities and rather cheap @ $15-20 or so USD per gallon.

Ok, so its not politically correct, ethical, and only slightly illegal, but the absolute best way to get it is to find a "white buffalo" nurse tank left out in a farmer's field overnight and go raid it.

[Edited on 1-1-2008 by evil_lurker]




Not all chemicals are bad. Without chemicals such as hydrogen and oxygen, for example, there would be no way to make water, a vital ingredient in beer.
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MagicJigPipe
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[*] posted on 1-1-2008 at 12:13


I often thought about buying my own anhydrous ammonia tank, going to a farmers field, taking some NH3 and leave some cash on it with a note. But I ulitimately decided not to (first because if you are caught you are guilty until proven innocent of meth manufacture) because, assuming the farmer called the cops (very likely) it would only hurt the cause of the home chemist. I guess if I need it I will stick to NH4Cl + Base or the boiling ammonia solution method mentioned above.

The only thing I don't like about that method is the MASSIVE amount of water that needs to be removed. It takes an impressive drying apparatus.

[Edited on 1-1-2008 by MagicJigPipe]




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Mr. Wizard
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[*] posted on 1-1-2008 at 17:58


Don't think farmers are unaware of the potential and possibility of theft of their ammonia. They are not stupid. They also know of the many times ammonia thieves have left a tank leaking or damaged causing injury or death to them or their employees. I would advise against any such foolish actions.
BTW have you ever seen what an ammonia vapor cloud can do to a person's eyes? It will blind you in seconds. This doesn't even include the damage done to other slightly moist regions normally protected by clothing. If you are messing around with a fitting and you get an unexpected leak, you will have no other option but to leave, leaving the tank leaking, and a danger to everyone around. Don't touch other peoples' stuff.:mad:
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Sauron
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[*] posted on 1-1-2008 at 19:42


That's the sort of extremely good advice that simply can't be repeated often enough.

We tend to take NH3 rather lightly compared to Cl2, NOx etc. but we should not. I would not much care to have a cylinder much larger than a lecture bottle of NH3 on hand in my lab. As has been discussed in another thread, there are alternatives, such as NH3 on ammonium thiocyanate and various other salts, which have a rather low vapor pressure at ordinary temperatures and are relatively easy to store, but which can release dry NH3 on demand when warmed.

There's a big difference between a few hundred CCs of NH3 liquid in a dewar or in a solution as described, compared to a high pressurized cylinder.

I would not deal with any of them except in a good hood, and wearing goggles, face shield, gloves etc. and possibly only after applying petroleum jelly to potential target areas of the body and/or wearing protective apparel. It's simply not a good time to cut corners about safety.




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[*] posted on 1-1-2008 at 21:06


On the other hand, if you're feeling a bit wild and crazy, there's some lower pressure synthesis routes to ammonia these days. Feed them water and air/N2 and electric power, and get o2 and NH3 out. Just on the edge of what amateurs might pull off.

Solid State Ammonia Synthesis
http://www.energy.iastate.edu/Renewable/ammonia/ammonia/2007...


Science 2 October 1998:
Vol. 282. no. 5386, pp. 98 - 100
Ammonia Synthesis at Atmospheric Pressure
George Marnellos, Michael Stoukides
DOI: 10.1126/science.282.5386.98

Journal of Catalysis
Volume 193, Issue 1, 1 July 2000, Pages 80-87
Synthesis of Ammonia at Atmospheric Pressure with the Use of Solid State Proton Conductors
George Marnellos, Stergios Zisekas and Michael Stoukides
doi:10.1006/jcat.2000.2877

Solid State Ionics
Volume 178, Issues 1-2, 31 January 2007, Pages 153-159
Catalytic and electrocatalytic synthesis of NH3 in a H+ conducting cell by using an industrial Fe catalyst
George Marnellos, Stergios Zisekas and Michael Stoukides
doi:10.1016/j.ssi.2006.11.019


Meterials Science Forum
Vols. 561-565 (2007) pp 1597-1600
Ammonia Synthesis Using Atomic Hydrogen Supplied From Silver-Palladium Alloy Membrane
M. Itoh, M. Saito, N. Tajima, K. Machida


EP0972855
United States Patent 6712950 Electrochemical synthesis of ammonia
United States Patent 6881308
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[*] posted on 1-1-2008 at 22:00


Mix slaked lime and ammonium sulphate, both from the hardware store, heat in a steel can, and condense the vapour. The result is 50% w/w ammonia solution. Add NaOH from the same hardware store and distil out the ammonia, passing thru a -10C trap (chiller at hardware store) to freeze out water, and consensing in a steel cartidge -33C (that can also be readily obtained). I cant believe anyone could think of ammonia as a controled substance, its just too common a thing.
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[*] posted on 1-1-2008 at 22:03


Quote:
Originally posted by len1
I cant believe anyone could think of ammonia as a controled substance, its just too common a thing.


Parts of the US government might disagree. As I have some lithium metal, the simultaneous possession of anhydrous ammonia would likely get me tossed in jail.

And consider the status of iodides in Australia, a country with a lot of coastline and seaweed.
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[*] posted on 1-1-2008 at 22:14


Quote:

And consider the status of iodides in Australia, a country with a lot of coastline and seaweed.



Kelp of course grows all along the southern coastline - but its only about 0.1% iodine.

It seems every country goes crazy in its own original way. While ammonia is fine here, iodine, it has been decided is not. Most chemicals for work I can just drop in and get - same day - I2 has to go through accounts, which introduces a 3 week delay. Fortunately Ive never needed it.

Now the crazy part. Those who need it for drug manufacture dont need to wait. I2 is sold as 3% tincture in pharmacies. From what I read on this forum, its only a catalyst in one particular mode of meth manufacture, if thats true then what is the point? I wish people would leave the elements alone, and keep the banned substances list rational.

[Edited on 2-1-2008 by len1]
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[*] posted on 2-1-2008 at 00:10


Actually, the best method may be to disproportionate 10% ammonium hydroxide solution.

If one were to simply boil 10% hardware store concentration aqueous ammonia and then bubble the wet gas into a concentrated solution of ammonium hydroxide in an ice cold champagne bottle, one could come up with a solution of ammonia in the 40% range.

Then by stoppering with some sort of valve system and the application of mild heating such as that of a water bath to 50ºC or so, the ammonia could be easily metered out, dried, and condensed.

Then the whole process could be repeated again.

There is a whole table of aqueous ammonia concentrations and boiling points in the document below:

http://www.tannerind.com/PDF/green-aqua-amm.pdf




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[*] posted on 2-1-2008 at 16:24


Yes, NH3 is very dangerous. Everytime I go to my grandfather's house I see at least one huge tanker of it and often find myself wondering what would happen if there was a massive leak or rupture.

Even a very small leak can cause your cause your lips, eyes and nose to burn even with adequate ventilation. Just imagine opening a bottle of household ammonia and sticking your nose in it. Then mulitiply that feeling by 100. Even household ammonia makes me recoil in horror when sniffed directly.

However, I don't think I'm as stupid as your typical methhead that steals NH3 and puts it in a propane tank. I have used a nurse tank before and am very familiar with it.

Yes, it would be wrong to steal NH3 but not really stupid if you knew exactly what you were doing and were using the right equipment and safety procedures. (well, it would be stupid because of legal risk.) At least no more so than using a nurse tank to nitrogenate the soil. The connection that you hook up to the applicator is the same as the one that is used to fill cylinders.




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[*] posted on 3-1-2008 at 01:05


Quote:
Originally posted by MagicJigPipe
Yes, NH3 is very dangerous. Everytime I go to my grandfather's house I see at least one huge tanker of it and often find myself wondering what would happen if there was a massive leak or rupture.

Even a very small leak can cause your cause your lips, eyes and nose to burn even with adequate ventilation. Just imagine opening a bottle of household ammonia and sticking your nose in it. Then mulitiply that feeling by 100. Even household ammonia makes me recoil in horror when sniffed directly.


Even the 28% ACS ammonium hydroxide that I have is not nice to work with, just taking the cap off can stink up the whole area for a little while. It also sure as hell clears a stuffed up nose even a few feet away.
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