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MagicJigPipe
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[*] posted on 7-4-2008 at 10:00
Ammonium Nitrate


I called some local fertilizer suppliers in hopes of finding some ammonium nitrate in a decent quantity (i.e. A 50lb bag that would basically last me forever). Ammonium nitrate is no longer sold in my area in anything but "ton amounts to authorized purchasers". Most of them said, "you're not going to be able to find any of that around". Only one mentioned the large quantity purchases being allowed. Obviously, no more 50lb bags here.

A few of them had "calcium ammonium nitrate" and they said that was the closest I was going to get to NH4NO3. What's funny is, most didn't even know what potassium nitrate was.

Surely this calcium ammonium nitrate can be used to make HNO3. But it really doesn't sound to practical to convert other nitrates to NH4NO3 through nitric acid.

Damnit this sucks. I should have ordered that 50lb bag off that trinitylabs site when it was still up. SHIT!




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[*] posted on 7-4-2008 at 10:40


Don't you guys have instant cold packs in the US? If yes, they can't be that expensive...?



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MagicJigPipe
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[*] posted on 7-4-2008 at 10:52


They are VERY expensive for how much NH4NO3 you get out of them. Something like $3 for 25-100 grams. That's $300 for 2.5-10kg. THAT SUCKS. I suppose you have to do what you have to do, though.

Potassium nitrate is cheaper than that here. Even at pharmacies it is $2.75 per 170g.

Apparently trinitylabs still carries it but check this shit out:

AMMONIUM NITRATE PRILLED 5 LBS.....$29.17
AMMONIUM NITRATE PRILLED 25 LBS.....$99.12
AMMONIUM NITRATE 50 LBS PRILLED......$198.24

Still pretty damn expensive. Not to mention the probably outrageous shipping fees.

[Edited on 7-4-2008 by MagicJigPipe]




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[*] posted on 7-4-2008 at 10:55


That is quite expensive.

But the KNO3...to give it some perspective: here in Norway, 90g of KNO3 at the pharmacy is approx. the equivalent of $20.




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[*] posted on 7-4-2008 at 11:38


Quote:

Don't you guys have instant cold packs in the US? If yes, they can't be that expensive...?


Yes, but, as I understand it, nowadays many of them are filled with urea.
Since cold packs typically don't state their ingredients, one could be on
a wild goose chase buying different types and testing their contents.

With those prices and availability, it looks like a scaled down Ostwald process
may be worth considering . . .

http://www.physicsdaily.com/physics/Ostwald_process
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[*] posted on 7-4-2008 at 11:47


How much ya want?

Pleny of fertilizer dealers around here sell it.

Apparenlty the folks round here got more common sense than they do fear of terrorism.

[Edited on 7-4-2008 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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[*] posted on 7-4-2008 at 11:47


Quote:
Originally posted by MagicJigPipe
What's funny is, most didn't even know what potassium nitrate was.
Surely this calcium ammonium nitrate can be used to make HNO3!


If you'd said Nitre or Saltpeter they might have twigged!
I have calcium ammonium nitrate, or C.A.N. as it's called here.
It's cheap, too!

I dissolve it in water, a few pounds at a time.
When the clay(?) settles it can be decanted, or filtered if you're in a hurry.
The NH4N03 isn't very pure (various phenolics?) but crystallised from a cooled saturated solution it's not bad!

If its solution is evaporated a cream-coloured cake is left, which if heated to its decomp temp will slowly whiten to something like packed snow; reasonably pure.

Just don't inhale the fumes!!!

Oh, and careful heating is advised!

Alkali-nitrates are best for HN03; hot concentrated H2S04 is a good enough oxidiser to oxidise NH4N03 to N2 + H2O.
The distillation will start OK but when the temp approaches 120*C your HN03 will be seriously diluted.

Eventually only water and N2 will come over!

To get other nitrates you could try metathesis with a K or Na salt, but check solubilities so you'll know which precipitates first.

P
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[*] posted on 7-4-2008 at 11:51


It's the same deal here; you can't buy it in bags, period. I had the good fortune of having a friend in Florida who made the 2000 mile road trip up here once, and he brought me 3 50lb bags, but I still feel like I don't have enough to last a lifetime. It seems ironic, but there in Florida where they have some of the strictest laws and crackdowns in the country, you can still buy it at feed stores. Some day I may have to make my own from scratch via calcium nitride or urea and Ostwald processes. Maybe someone here who can still buy it would be willing to ship you some, but like anything I wouldn't expect it to be available to the public anywhere for long (of course you know this as well as I, where most people don't seem to realize the severity of the problem). You've simply either got to buy it from a willing farmer or other individual who can still get it, or make your own.

Converting calcium ammonium nitrate to ammonium nitrate via nitric acid and ammonia wouldn't be too bad really. You wouldn't need anything fancy, since just the wet ammonia and raw wet nitric you'd get out would work fine for making ammonium nitrate. The biggest expense would be the alkali and the sulfuric acid needed to do that, but it beats the hell out of $200 plus shipping don't you think? Maybe you could even use an electrolytic process with addition of ammonia and precipitation of calcium hydroxide off the cathode to convert it more directly and cheaply (at the expense of time no doubt). Beyond that the Ostwald process would be my only other suggestion, and it should not be too hard (just really slow) if you get yourself an old catalytic converter.

[Edited on 7-4-2008 by kilowatt]




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[*] posted on 7-4-2008 at 12:13


Around here, Calcium Ammonium Nitrate (CAN) is about a 20% blend of Calcium Carbonate (limestone) with ammonium nitrate. I bought a 25Kg bag as a source of ammonium nitrate. The carbonate is easily separated by dissolution and filtering. The big drawback is getting the ammonium nitrate out of solution and in a dry form. If you just want it for nitrate metathesis reactions (like I did) it's fine!

It's mentioned in several threads on this site, or Google "CAN".
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[*] posted on 7-4-2008 at 12:16


Sodium and i believe calcium nitrate can be bought unsuspiciously from pottery suppliers. Even if you can't find a well stocked store in your area, combined with a few other useful reagents, the cost of shipping should be worth it.
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[*] posted on 7-4-2008 at 12:17


Oh, well that makes it easy then. Ammonium nitrate is not that hard to dry either, again just time consuming. I have recrystallized some of my AN fertilizer before just to make it more pure. It does not form any hydrates as far as I know. Are you just referring to the tedium of boiling off the water?



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[*] posted on 7-4-2008 at 12:27
NH4NO3


Ca(NO3)2 + (NH4)2SO4 --> 2NH4NO3 + CaSO4

Both readily available and cheap at the local agricultural supply where I live.

The CaSO4 precipitates out instantly. Filtering can be a pain but it can be done.




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[*] posted on 7-4-2008 at 13:55


Once, when I needed some NH4Cl, I mixed AN and ordinary granular table-salt (stoichiometrically) in a metal dish and heated the mixture.

NH4Cl sublimed from the mix, condensing on a large cold glass parabola over the dish in high purity.

Had the stuff been finely ground and well mixed, it would probably have gone all the way to NaN03, with all the NH4Cl on the glass.

Temperature control might be needed to prevent reduction of the nitrate to nitrite!
Careful slow heating is called for, in any case.

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[*] posted on 7-4-2008 at 14:06


Quote:
Originally posted by MadHatter
Ca(NO3)2 + (NH4)2SO4 --> 2NH4NO3 + CaSO4

Both readily available and cheap at the local agricultural supply where I live.

The CaSO4 precipitates out instantly. Filtering can be a pain but it can be done.


I'm sure I can find some calcium nitrate, too. It's twice the nitrate per mole (compared to NH4NO3), as well!

Have you tried this MadHatter? If so, is there any more you can tell me before I try?

I found this info on "CAN" while searching google.


Quote:

CAN contains 27% nitrogen and 8% Calcium as Calcium Carbonate (lime). It consists of dust-free, white free-flowing granules.


Quote:

Calcium ammonium nitrate (CAN) contains 27 % N and 20 % of ground limestone. Nitrogen is half in the nitrate form and half in the ammoniacal form. This results in rapid as well as permanent effect. The granulation of this fertilizer ensures a quick and exact dosing.


Quote:

Calcium Ammonium Nitrate (CAN 17) is a versatile fertilizer that contains 8.8% calcium and 17% nitrogen. The nitrogen is one-third ammonic form and two-thirds nitrate form. CAN 17's largest market currently is among California and Arizona vegetable growers, although that is changing as growers in the Pacific Northwest discover the advantages of offering both an available and a reserve form of nitrogen in addition to soluble calcium


Is this really just a calcium salt and Ammon. Nitrate mixed together? Does the compound 5Ca(NO3)2.NH4NO3.10H2O actually exist? If so, is that what CAN is? I suppose what I am asking is-- what is it exactly?

[Edited on 7-4-2008 by MagicJigPipe]




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[*] posted on 7-4-2008 at 14:19


How do you dry ammonium nitrate? I put it in the oven (slightly open to allow water to escape) and heat it to around 120-150 C (it starts to smoke heavily if overheated) for some hours. Then I pour it from the dish on some Al foil. When it cools I break it up and dry it for an hour or two with a hot air blower. I noticed that my ammonium nitrate melts at a lower temperature than it should. And when heated with the hot air blower it doesn't melt but still some smoke is produced (smells the same as when AN decomposes). Well it contains some magnesium nitrate (around 5%). Perhaps that is the reason?



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[*] posted on 7-4-2008 at 14:25


If it melts before it's supposed yo that usually means it's hydrated but since NH4NO3 doesn't complex with water I'm not sure what your prob is.



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[*] posted on 7-4-2008 at 14:33


Well it is possible that it is hydrated but I don't think so as it worked great in APAN, MEKPAP/AN and various pyrotechnic mixtures.



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[*] posted on 7-4-2008 at 14:42


It seems that there is indeed such a double salt, which has its own CAS number (15245-12-2) :

http://ctd.mdibl.org/detail.go;jsessionid=2BCA76D75A8DF0BD7D...

http://www.bibra-information.co.uk/chemlist-C.html

However, it seems that the fertilizer may not be the double salt, but a
mixture of two salts according to our friends at Homeland Security:

http://64.233.169.104/search?q=cache:68Po-TIRUCoJ:www.fwaa.org/Hot_Topics/TFI-Memo1.pdf+%22calcium+ammonium+nitrate%22+%22double+salt%22&hl=en& ;ct=clnk&cd=5&gl=us&client=firefox-a

Basically, they can't figure out whether CAN fertilizer is a watched
chemical because their list only includes ammonium nitrate; presumably,
terrorists have no use for the double salt ;)
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[*] posted on 7-4-2008 at 14:46


Hello MagicJigPipe ,

I remember one time not_important saying that using this procedure (calcium nitrate + ammonium sulphate) will not give a very pure product since the Ca++ ions will tend to be more soluble in presence of ammonium ions..

Another idea from N.I. is that you can also mix (NH4)2SO4 and KNO3 solutions and cool well (K2SO4 is the least soluble), remaining NH4NO3 that is easily further purified..




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[*] posted on 7-4-2008 at 14:53


CAN-17 is a solution of calcium and ammonium nitrates
http://www.simplot.com/agricultural/plant/cal_ammon_nitrate....

CAN in solid form usually is CaCO3 + NH4NO3, from the EU:
Quote:
However, in practice, products containing limestone and/or dolomite and with nitrogen content <28% are designated as Calcium Ammonium Nitrate (CAN).

but check the spec sheet and MSDS on the specific product.

In the case of limestone + AN, solution in warm water quickly followed by filtration should give decent recovery. Too long of contact with hot water will drive off NH3 and CO2, leaving you with mixed nitrates.

Hot methanol should dissolved nitrates away from carbonates and sulfates.

If your raw materials lead you to precipitating CaSO4 from mixed nitrates, note that CaSO4 is slightly soluble in water and more so in solutions of ammonium salts or mineral acids. The later causes a little trouble when making HNO3 from H2SO4 and Ca(NO3)2. For making AN, the filtered solution can be treated with ammonium carbonate to precipitate much of the calcium as CaCO3. Alternatively the solution can be evaporated on a water or steam bath, then the AN can be extracted with methanol; if you do this use a slight excess of ammonium sulfate as calcium nitrate is also soluble in methanol.

Calcium and magnesium nitrates are fairly hygroscopic, in attempting to take them to dryness you can end up with a mush formed from melted hydrates of the nitrates. Mixed ammonium+(calcium,magnesium) nitrates do not dry well, as the Ca/Mg nitrates tend to 'melt' in their own water of crystallisation, so the product always is moise appearing. Even if you get a mixed ammonium+(calcium,magnesium) nitrate dry, it readily picks up moisture again.

table of solubility of CaSO4 in various water+acid mixtures here:
http://www.sciencemadness.org/talk/viewthread.php?tid=9848&a...
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[*] posted on 8-4-2008 at 11:21
Calcium Nitrate


The calcium nitrate I use is the mixed NH4NO3/Ca(NO3)2. The trick is to precipitate and
filter the CaSO4 as much as possible. NH4NO3 is highly soluble even in cold water.
I can't find the solubility curves for CaSO4 in ammonium salt solutions.

One other thing: That mixed Ca(NO3)2 is usually coated with wax for time release.
So I put it in a filter and pour ice water through to leave the wax behind before proceeding.
Don't use hot water for that step. The wax gets soft and clogs the damn filter.




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[*] posted on 8-4-2008 at 13:15


I have a problem. My AN starts to smoke heavily when I dry it before it melts. The smoke is white, thick and has the smell of decomposing AN but AN doesn't decompose on such a low temperature. I heat it at around 80 C. It does contain around 5% of (MgNO3)2. Does anyone know why it smokes like that?



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[*] posted on 8-4-2008 at 13:56


Does NH4NO3 sublime readily at elevated temperatures? I always thought it started to decompose a little below it's melting point.



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[*] posted on 8-4-2008 at 16:40


Any organics or transition metal nitrates could be accelerating the decomposition. It likely is best to attempt to crystallise the AN, remembering that in crystallisation you are not going to get 100% of the substance - you must leave liquid. Filter off and drain the crystals, dry them at low heat - 40 C or so. If they don't go dry then it is magnesium salts causing the problem, you'll have to remove the Mg by precipitation with ammonium carbonate or strong aqueous ammonia.

Attached is a PDF that contains just an image file, showing solubility of CaSO4 in the presence of several ammonium salts. Ammonium nitrate can increase the solubility as much as 5 times, with means a gram of CaSO4 in 100 cc of liquid.

Attachment: CaSO4_sol_ammonium.pdf (93kB)
This file has been downloaded 559 times

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[*] posted on 15-4-2008 at 06:32


Yes we discussed this before, the thing is that the sulphate has the equilibrium

SO4- + H+ -> HSO4-

and this means CaSO4 is going to be more soluble in acidic solutions.

Ammonium salts tend to be acidic, hence calcium sulphate dissolve more readily in them. If you make the solution basic by adding ammonia - that aspect of the problem will solve, and the NH3 will not contaminate the product
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