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weiming1998
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Nitrate salt synthesis
It is very hard to buy nitrate salts/nitric acid where I live (cold packs are urea and fertilizers have only a tiny amount of nitrate in them.) So
far, the only routes to nitrate salt/nitric acid I know of are these:
.Oxidation of ammonia, then bubble gases through water. (requires expensive catalyst tubes/etc)
.Arc furnace-produced nitrogen dioxide (don't have arc-furnace and likely to be extremely expensive
.Oxidation of ammonia by ozone (produces ammonium nitrate) (My ozone generator only produces 400mg ozone/hour)
.Nitrite salts (can't get them)
.Fermentation of urine/manure (very disgusting and will stink/take a long time)
So, does anyone here know how to make nitrate salt/nitric acid or even nitrite salts?
Disclaimer: I am not using nitrate salts for pyrotechnics/explosives (I already have potassium chlorate for pyrotechnics and I am never going to make
explosives)
I just want to explore some nitrate chemistry and possibly make some aqua regia for gold plating.
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Bot0nist
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Don't you have YouTube.
Check out making niter beds. IT was all the craze in Ye-ole days. It was even mandated by governments in some wartime eras when black powder was in
high demand.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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phlogiston
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I recently experimented a bit with ammonia oxidation, and I think the resulsts suggest that plain copper wire may also work as a catalyst.
I just stuffed some fine copper wire (from mains electrical wiring) into a glass tube (pasteur's pipette), through which I drew a flow of air. As soon
as I held the inlet over a concentrated ammonia solution, the copper would glow white hot, eventually melting the glass and copper wire. It was
necessary to preheat the tube/copper a bit with a torch to get the reaction started but as soon as the ammonia entered the tube it was
self-sustaining.
I also did the same experiment with a small diameter (about 3 mm) titanium-platinum alloy tube which behaved similarly (but did not melt). These tubes
are rather expensive, though.
-----
"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer |
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weiming1998
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Quote: Originally posted by Bot0nist  | Don't you have YouTube.
Check out making niter beds. IT was all the craze in Ye-ole days. It was even mandated by governments in some wartime eras when black powder was in
high demand. |
Niter beds requires manure. I don't have manure. I suppose I could buy manure from garden supply stores, but it's going to stink my backyard real bad.
Also, it takes months and years to generate a little bit of impure potassium nitrate.
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weiming1998
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| Quote: Originally posted by phlogiston | I recently experimented a bit with ammonia oxidation, and I think the resulsts suggest that plain copper wire may also work as a catalyst.
I just stuffed some fine copper wire (from mains electrical wiring) into a glass tube (pasteur's pipette), through which I drew a flow of air. As soon
as I held the inlet over a concentrated ammonia solution, the copper would glow white hot, eventually melting the glass and copper wire. It was
necessary to preheat the tube/copper a bit with a torch to get the reaction started but as soon as the ammonia entered the tube it was
self-sustaining.
I also did the same experiment with a small diameter (about 3 mm) titanium-platinum alloy tube which behaved similarly (but did not melt). These tubes
are rather expensive, though. |
The equipment on actually oxidizing the ammonia, then bubbling it through water, are going to be hard to find. I could substitute an iron tube for the
glass tube part. Then I need something to contain ammonia, then bubbling the substance through water, etc...
I'll have a hard time building this, but I might do it anyway
Thanks for the help though.
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Pulverulescent
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Can't you just buy it on ebay?
P
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AirCowPeaCock
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| Quote: Originally posted by weiming1998 | | Quote: Originally posted by phlogiston | I recently experimented a bit with ammonia oxidation, and I think the resulsts suggest that plain copper wire may also work as a catalyst.
I just stuffed some fine copper wire (from mains electrical wiring) into a glass tube (pasteur's pipette), through which I drew a flow of air. As soon
as I held the inlet over a concentrated ammonia solution, the copper would glow white hot, eventually melting the glass and copper wire. It was
necessary to preheat the tube/copper a bit with a torch to get the reaction started but as soon as the ammonia entered the tube it was
self-sustaining.
I also did the same experiment with a small diameter (about 3 mm) titanium-platinum alloy tube which behaved similarly (but did not melt). These tubes
are rather expensive, though. |
The equipment on actually oxidizing the ammonia, then bubbling it through water, are going to be hard to find. I could substitute an iron tube for the
glass tube part. Then I need something to contain ammonia, then bubbling the substance through water, etc...
I'll have a hard time building this, but I might do it anyway
Thanks for the help though. |
The equipment is very minimal..you ought to be able to pick all of it up from a surplus store for less than 20$...depending on your scale.. Glass
tubes, stoppers, flask, beaker..that's all you need! whats so hard about that? And in my experience cold packs have at-least an ounce of NH4NO3, and
as I've heard mix that with a little hydrochloric acid and you have a NH4Cl-HNO3 solution, easy to distil if you have glass on glass distillation.
Check out Nurdrages video on nitric acid, he shows a crude distillation process only involving three beakers and a bit of distilled water and copper.
[Edited on 1-19-2012 by AirCowPeaCock]
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Bot0nist
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"And in my experience cold packs have at-least an ounce of NH4NO3, and as I've heard mix that with a little nitric acid and you have a NH4Cl-HNO3
solution, easy to distil if you have glass on glass distillation." ~ APCP
I get between 50-55g of ammonium nitrate from cold packs (dried weight) on average. (It's the "Large size.)
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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neptunium
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i dont know about the cold packs anymore ...5 or 6 years ago maybe but in the US today...i doubt the quantity and quality...
there is a video on youtube this dude makes nitric acid with an old neon transformer and hydrogen peroxide..i tried it with an old bottle of Jack
Daniel and a fridge compressor continuously bubbling NO2 in the H2O2... 3% works but get the 12% (40volume) clairoxide (hair bleach)from the beauty
supply store
after letting it run overnight (make sure it wont overheat though..) you`ll get a descent quality HNO3 depand on your set up you can let it run a week
and get a good quantity
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Bot0nist
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You shouldn't generalize. I bout 170g of NH<sub>4</sub>NO<sub>3</sub> last weekend at the dollar store in cold packs and I'm
in SE USA. Only lost 6% after recrystallization. It is very pure ammonium nitrate. The urea one are out there. That's why we read ingredients and
MSDS's though. There are a few threads on this. One I posted in is called "cold pack disappointment." I believe.
[Edited on 19-1-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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AirCowPeaCock
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sorry guys, I ment HCl! but you probably realized that...
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AirCowPeaCock
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I got alot from a cold pack last year and I'm definitely in the US. I'm not that interested in NH4NO3 unless I need N2O, but I don't usually have
much use for that--oxygen works just fine. You can also get KNO3 stump remover by the pound for less than 5$ a pound, and mix it with some sulfuric
acid drain cleaner (mines 95%). Don't be so pessimistic..
BOLD
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entropy51
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| Quote: Originally posted by neptunium | i dont know about the cold packs anymore ...5 or 6 years ago maybe but in the US today...i doubt the quantity and quality...
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You aren't shopping in the right store. Ive been getting CVS cold packs that have 120 grams each of very
good NH4NO3, two cold packs per box.
But I just scored 3 pounds of good KNO3 stump remover so I won't need cold packs for a while.
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S.C. Wack
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http://www.sciencemadness.org/talk/viewthread.php?tid=11388
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weiming1998
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As I said before, I am not allowed to buy things off Ebay, plus the police might track the order to my house and search my lab, and they'll find a lot
of interesting things or maybe claim me as try to make illegal fireworks.
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weiming1998
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| Quote: Originally posted by AirCowPeaCock | | I got alot from a cold pack last year and I'm definitely in the US. I'm not that interested in NH4NO3 unless I need N2O, but I don't usually have
much use for that--oxygen works just fine. You can also get KNO3 stump remover by the pound for less than 5$ a pound, and mix it with some sulfuric
acid drain cleaner (mines 95%). Don't be so pessimistic.. |
I asked for stump remover at Bunnings and another shop, and all they gave me is this weird tree killer that had some obscure ester of some sort. Also,
no sulfuric acid drain cleaners. They are all (impure) sodium hydroxide ones. Some of them are even enzyme drain cleaners.
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weiming1998
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| Quote: Originally posted by AirCowPeaCock | | Quote: Originally posted by weiming1998 | | Quote: Originally posted by phlogiston | I recently experimented a bit with ammonia oxidation, and I think the resulsts suggest that plain copper wire may also work as a catalyst.
I just stuffed some fine copper wire (from mains electrical wiring) into a glass tube (pasteur's pipette), through which I drew a flow of air. As soon
as I held the inlet over a concentrated ammonia solution, the copper would glow white hot, eventually melting the glass and copper wire. It was
necessary to preheat the tube/copper a bit with a torch to get the reaction started but as soon as the ammonia entered the tube it was
self-sustaining.
I also did the same experiment with a small diameter (about 3 mm) titanium-platinum alloy tube which behaved similarly (but did not melt). These tubes
are rather expensive, though. |
The equipment on actually oxidizing the ammonia, then bubbling it through water, are going to be hard to find. I could substitute an iron tube for the
glass tube part. Then I need something to contain ammonia, then bubbling the substance through water, etc...
I'll have a hard time building this, but I might do it anyway
Thanks for the help though. |
The equipment is very minimal..you ought to be able to pick all of it up from a surplus store for less than 20$...depending on your scale.. Glass
tubes, stoppers, flask, beaker..that's all you need! whats so hard about that? And in my experience cold packs have at-least an ounce of NH4NO3, and
as I've heard mix that with a little hydrochloric acid and you have a NH4Cl-HNO3 solution, easy to distil if you have glass on glass distillation.
Check out Nurdrages video on nitric acid, he shows a crude distillation process only involving three beakers and a bit of distilled water and copper.
[Edited on 1-19-2012 by AirCowPeaCock] |
I am very short on professional glassware. I don't have anything to distil with (you know the glass tube?) And I can't buy any, chemistry supply
stores won't sell to individuals.
Also, I don't have a neon sign transformer. I'll be looking for one, but don't have one right now.
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entropy51
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| Quote: Originally posted by weiming1998 | | I asked for stump remover at Bunnings and another shop, and all they gave me is this weird tree killer that had some obscure ester of some sort. Also,
no sulfuric acid drain cleaners. They are all (impure) sodium hydroxide ones. Some of them are even enzyme drain cleaners. |
It's getting harder to find chemicals everywhere. I looked for about two years for that KNO3 stump remover before I finally found
it, and I bought the last 3 pounds on the shelf. None of the hardware stores carry muriatic acid or Rooto anymore, although they still have a
sulfuric based drain opener that is OK for making HCl or HNO3, but not much else. I was formerly able to buy KMnO4 by the pound locally, but that's
disappeared as well. The grocery stores used to have pure NaOH, but no more. THe hardware stores still carry it though, for now. It's been said
before: if you find something good in the store, stock up!
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AirCowPeaCock
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Wow, life must suck for you guys, I can pick up all the technical grade ammonia(10%), sulfuric acid (95%), powdered sodium hydroxide I want from
menards. And all the sodium metabisulfate and potassium nitrate I want from an obscure gardening store, all the NH4NO3 from the drug store..no
problem..
But maybe I should stock up...
[Edited on 1-20-2012 by AirCowPeaCock]
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weiming1998
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I can buy relatively pure sodium hydroxide just a few months ago, now it's drain cleaner crap that is contaminated massively with aluminum, etc.
Ammonia is only 2-4%, cold packs all urea, and some times I can't even find them. Absolutely no nitrate fertilizers without a ton of contaminants,
only 3-6% hydrogen peroxide can be found, iodine supplements all kelp instead of sodium/potassium iodide, Hydrochloric acid can only be found in a
specialized pool shop, in Bunnings they don't even sell sodium bisulfate (pH down) anymore. Can't buy freaking POOL CHEMICALS without the workers
asking questions and saying how buying sodium thiosulfate is a waste of money. Sulfuric acid is nowhere to be found, etc. Chemicals in China, the
country I used to live in, is not even as strictly regulating chemicals as Western Australia. I imagine in a few years, not even baking soda and
vinegar is going to be found, and everything in the hardware store is heavily contaminated on purpose. This is no different than outright banning
amateur chemistry.
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weiming1998
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| Quote: Originally posted by entropy51 | | Quote: Originally posted by weiming1998 | | I asked for stump remover at Bunnings and another shop, and all they gave me is this weird tree killer that had some obscure ester of some sort. Also,
no sulfuric acid drain cleaners. They are all (impure) sodium hydroxide ones. Some of them are even enzyme drain cleaners. |
It's getting harder to find chemicals everywhere. I looked for about two years for that KNO3 stump remover before I finally found
it, and I bought the last 3 pounds on the shelf. None of the hardware stores carry muriatic acid or Rooto anymore, although they still have a
sulfuric based drain opener that is OK for making HCl or HNO3, but not much else. I was formerly able to buy KMnO4 by the pound locally, but that's
disappeared as well. The grocery stores used to have pure NaOH, but no more. THe hardware stores still carry it though, for now. It's been said
before: if you find something good in the store, stock up! |
The problem is, I can't even seem to find good chemicals anymore, and if it is good, it is hell expensive (50g potassium permanganate for $10
dollars!)
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AirCowPeaCock
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I wouldn't call 50g KMnO4 hella expensive, due to its oxidation properties its somewhat expensive to ship. Id spend 10$ for 50g KMnO4, but maybe
that's just me. I think maybe, hopefully, eventually they'll give up on the chemical restriction because they will realize given enough effort meth
and RDX can be made from shit. And I don't think they're going to be taking my shit away anytime soon..but maybe not, I see a disturbing trend
towards totalitarianism in the US...I keep thinking 1984--if you know what I mean. It's honestly scary, especially the tea party and the GOP..
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weiming1998
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Or maybe not, and they're going to even ban chemistry experiments in school. All that is left for students to learn is theory. Anyway, back to the
main subject:
From this post, I can see there's only 5 routes for me to make/get a nitrate salt/nitric acid:
:Niter beds, which aren't very convenient and will take a long time.
:Oxdation of ammonia. Seems to work at first, but How do I get enough oxygen for the ammonia to combust, even if there is a catalyst?
: Neon sign transformer+ air: This is the only plausible one, but I can't find a neon sign transformer. Does any of you know where to get one/buy one?
:Searching for more stores, or
:Buying off Ebay (I have to persuade my parents then)
[Edited on 20-1-2012 by weiming1998]
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Bot0nist
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| Quote: | The process for making saltpeter is very similar to that for making potash, the chief difference being the starting material. The soluble part of wood
ash is mostly potassium carbonate and so when we purify it by recrystalization, the resulting product is purified potassium carbonate. The soluble
part of these manurial soils are mostly mixed nitrates. The reason for this is that while the original animal waste may have had a wide variety of
soluble materials, as the water wicked up through the soil and evaporated, the less soluble parts fell out of solution as it became more and more
concentrated. Only the most soluble parts, in this case the nitrates, made it to the top of the soil and when the last bit of moisture evaporated,
they were deposited as a white crust on the surface.
So the beginning of primitive saltpeter production is to collect this white crust leaving behind as much as possible the underlying soil. Of the three
nitrates present, potassium nitrate is the one we need. To extract it, we use a metathesis reaction in much the same way that we have previously
produced lye:
Ca(NO3)2(aq) + K2CO3(aq) -----> CaCO3(s) + 2 KNO3(aq)
This removes all the calcium as insoluble calcium carbonate leaving mostly potassium nitrate and a little sodium and potassium carbonate which can be
further separated out by repeated recrystalizations in much the same way that we produced potash.
Saltpeter has been mined in Virginia, particularly in the dry caves of the Shenendoah valley. Most of the nitrate mined today comes from Chile and is
called "Chile Saltpeter," which is chiefly sodium nitrate. However, most of the nitrate used in explosives and agriculture is today derived from
nitrogen in the air
~ http://www.cavemanchemistry.com/oldcave/projects/gunpowder/i...
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| Quote: Originally posted by Bot0nist | | KNO<sub>3</sub> can be extracted from manurial soil using wood ash(for potassium carbonate I think). A useful purity can be obtained by
recrystallization using ethanol to precipitate out the less soluble salts. Make sure the soil has been protected from direct rainfall.
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| Quote: Originally posted by Bot0nist | I once found an old collapsed barn in an overgrown pine grove. The barn had collapsed in such a way that the roof (Tin I guess) was suspended about
1/1/2 to 2 feet off the ground. It looked to be at least 50-70 years old, at least. Underneath the roofing was a bunch of dusty soil and decomposed
hay and it all had a fine layer of visible salts on the surface. I used the 55 gal drum method and got a good bit of nitrate salts when I was
finished. I assume the barn had housed horses or livestock, which must have contributed to the large deposits of nitrates. The finished product worked
great in ball milled black powder after a few recrystallizations. I had to increase the proportion of it to obtain suitable burn speeds though. I
attributed this to impurities that I couldn't (with my current know how ) purify it
any further. [Edited on 3-3-2011 by Bot0nist] |
[Edited on 21-1-2012 by Bot0nist]
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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weiming1998
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So pouring soil into a barrel and dissolving all the solubles in it, then precipate with K2CO3? No problem, I can make K2CO3 from K2SO4 and Na2CO3.
I'll try this.
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