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MadHatter
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Ferrous Sulphate
Can you get FeSO4 from an agricultural supplier ? That'll take care of the chlorate problem
for you and it's very cheap(at least here in the US).
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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hashashan
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Never seen it in an agricultural supply here .. but I believe It wont cost too much in a chem shop.
btw ... im not so good in potential chemistry ... can anyone please write down the full reaction of reduction of chlorate with FeSO4?
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12AX7
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6 Fe(2+) + ClO3- + 6H+ ---> Fe(3+) + Cl- + 3H2O
Notice the equilibrium is heavily dependent on H+ -- an excess of Fe(II) is desirable, with enough acid to react all chlorate and dissolve all
Fe(III), which requires a low pH. You will want to wash the product with dilute HCl to remove traces of Fe2O3 (although as it acts as a catalyst, it
might be considered a beneficial impurity in pyrotechnia?), then mildly basic or neutral water until the pH is neutral.
Tim
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hashashan
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That I already seen
but i meant a more specific formula
as i understand the Cl- is the NaCl but what is the Fe(III) (is it coming in the form of the ferric sulfate?)
and the H+ will be HCl right?
I just never done this procedure and would like some details.
Im sorry if im making a fool out of myself
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12AX7
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Doesn't matter, sulfate, chloride and alkaline ions are all spectators. You must add them to the reagents when calculating stoichiometric proportions
(which is kind of odd to do anyway, unless you know the amount of chlorate to begin with -- you could titrate a sample to determine this). What's
left doesn't matter, unless you want to like, evaporate down the solution and recover whatever all was in it. In that case, you'll get a mixture of
Na2SO4, NaCl, Fe2(SO4)3, FeCl3, FeSO4 and FeCl2.
Tim
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hashashan
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I wanted to know the final products to know if they are soluble or not.
and to know how to extract the AP out of all that mess. for example the Na2SO4 is one of the guys I wouldnt like to have in my solution... and as I
see there is no way to prevent him from coming to the party... right?
So as I see there is no way to get some NH4ClO4 without HClO4 ... right?
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12AX7
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Well, no... you use enough water to wash everything else out.
If that's more water than the NH4ClO4 dissolves in, then you should consider an aqueous process instead.
I would go with HCl, heat and a big fan. ClO3- gives ClO2 or Cl2 in acidic solution. Basify with your choice cation (NH4+, etc.) and precipitate.
Personally, I am currently collecting crude KClO4, which I will boil with mild HCl in a pyrex vessel, neutralize and wash with cold H2O. This should
leave little chlorate and sodium among the low-solubility KClO4, hopefully spectrally pure to the eye.
Ammonium perchlorate isn't as insoluble, but you could start with NaClO4 (solution or crystallized) and work on that. The remaining perchlorate will
precipitate, with concentration if needed.
Tim
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hashashan
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HCl is nice ... but it is absolutely unacceptable if the chlorate levels are high.
and all other methods involve N2SO4 in the end?
If so then probably LiClO4->NH4ClO4 would be the ok... however their solubilities are not too different .... anyway guys .. I'm desperate.
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12AX7
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Then keep running until chlorate levels are acceptable. You might even run until it precipitates NaClO4 on cooling, which appears to be within reach
(I don't know how much NaClO3 can be dissolved in the reheated liquor without falling out on cooling).
Tim
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hashashan
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Yes this is a good idea, but I don't have NaClO3 also  I make the perchlorate
right out of NaCl.
I might try to precipitate the chlorate.... but I don't believe that NaClO4 can precipitate out of the solution because it is much more soluble then
the chlorate and it will salt out the chlorate
[Edited on 29-1-2008 by hashashan]
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12AX7
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Ah, but there's still a chlorate intermediate. I isolate it; you don't.
I believe I have precipitated NaClO4, such that chlorate concentration is small enough not to precipitate, while perchlorate concentration is high
enough to precipitate on sufficient cooling. I don't think I've precipitated it by forcing the equilibrium with additional chlorate, which does work
to some extent in the NaCl-NaClO3-H2O system. The excess chlorate precipitates preferentially.
Tim
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MadHatter
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Solubilities
Hashashan,
The solubilities of NH4ClO4 and LiClO4 are wide enough for the metathesis and precipitation
provided there is a high quantity in the solution to start with.
From CRC, 62nd Edition(1981-1982):
KClO4 ____________0.75 @ _0 C________21.80 @ 100 C
LiClO4 ___________60.00 @ 25 C________150.00 @ 89 C
NaClO4+H2O_____209.00 @ 15 C________284.00 @ 50 C
NH4ClO4 _________10.74 @ _0 C_________42.45 @ 85 C
The potassium cation is useless and the sodium cation provides the widest potential
precipitate range depending on which anion is used.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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hector2000
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whatis your idea about this method:
http://www.geocities.com/CapeCanaveral/Campus/5361/chlorate/...
and
http://www.wfvisser.dds.nl/EN/perchlorate_EN.html
Chemistry=Chem+ is+ Try
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