symboom
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Ammonium Nitrite Isolation
Ammonium phosphate is dissolved in water then frozen a solution of sodium nitrite is also made and the both freezing mixtures are mixed no reaction
and no bubbles form as ice is present helping keep the reaction from becoming to warm
Option 1
boiling the water off with reduced pressure I should be able to isolate dry ammonium nitrite that or extract it with a solvent only problem if sodium
phosphate is insouble to not knowing which solnts to use im guessing vacuum distillation. Leaving ammonium nitrite behind
Reduced pressure is used so at near freezing water can boil off
Because at room temperature ammonium nitrite decomposes
It reminds me of copper peroxide both are temperature sensitive reactions they both provide great practice in temperature control some chemical
reactions are done good in the winter and some in the summer
So the tempture must remain around 0C until ammonium nitrite is removed from solution snd a desicant is used to remove moisture and dry it then the
dry smmonium nitrite can be returned to room temperature.
Option 2 percipitate it out
Liquid ammonia
Dioxane??
Methanol
Ethanol
Isopropanol
Sodium nitrite soubility
Not sure if liquid ammonia could be used with sodium nitrite
soluble in methanol (4.4 g/100 mL)
ethanol
slightly soluble in diethyl ether (0.3 g/100 mL)
Insouble in solvent in which sodium percipitates out
And driving the reaction forward
Ammonium compounds
Ammonium chloride
Solubility in methanol
3.2 g/100 g (17 °C)
3.35 g/100 g (19 °C)
3.54 g/100 g (25 °C)[2]
Solubility in ethanol 6 g/L (19 °C)
[Edited on 12-7-2017 by symboom]
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woelen
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Solid ammonium nitrite is very unstable, especially if it is not perfectly dry. I do not believe you will be able to isolate this salt. Even the dried
mix with sodium phosphate will not be stable. It slowly decomposes to give water and nitrogen gas. At elevated temperatures it may decompose very
violently and exothermically.
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PHILOU Zrealone
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The solubilities you list are all arround the ambiant T°...
If you go arround 0°C or below...nearly all (if not all) will drop down and be even less soluble.
You have more chance to work with a metathetical reaction..prior to the concentration sublimation step...
NH4NO2 must be close to NH4NO3 in terms of solubility...and must thus be quite high vs other salts...
The simple following reactions should be good ones...
2 KNO2 + NH4O2C-CO2NH4 --> KO2C-CO2K(s) + 2 NH4NO2
With as driving force the precipitation of potassium oxalate...
2 Mg(NO2)2 + (NH4)2CO3 --> MgCO3(s) + 2 NH4NO2
With as driving force the precipitation of magnesium carbonate...
Ca(NO2)2 should work aswel with precipitation of Ca oxalate...or Ca carbonate
Probably other metals will do the job too since oxalates and carbonates are usually unsoluble...but the difficulty will be to find or metathetically
synthetise the nitrite first...
As exposed NH4NO2 is about the same as NH4ClO3 onto the stability and dangerousity levels...so due cautions must be taken when handling the material
as solid or concentrated solutions
==> Tiny amounts
==> Avoid hard confinment (glass, metal, hard plastic) in case of unwanted explosion less dangerous schrapnells.
==> No screw on top caps (pressure build up may occure)
==> No standing near flamable solvents
==> No long storage without control (never left alone).
[Edited on 12-7-2017 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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symboom
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It was here some where that magnesium nitrite also decomposes just attempted that sodium nitrite mixed with magnesium sulfate then heated no
decomposition occured
Also ammonium chlorate is more stable than ammonium nitrite ammonium nitrite decomposes in room temperature water although it is stabilized with
ammonia maybe that will keep it from decomposing at room temperature im tired of always keeping the temperature around freezing
[Edited on 12-7-2017 by symboom]
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woelen
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I think that NH4NO2 is less stable than NH4ClO3. It is not more explosive, it simply decomposes while being prepared.
I once made NH4ClO3 in small quantities (there is an experiment about this on my website). It can be prepared without too much difficulty. A solution
with NH4ClO3, when allowed to evaporate, leaves behind dry white crystals of NH4ClO3. A solution with NH4NO2, when allowed to evaporate, simply
decomposes and nothing is left behind on long standing. The liquid concentrates, and then it starts to produce nitrogen slowly. Finally nothing is
left behind.
This experiment can be done easily. Dissolve some KNO2 in water. Dissolve some NH4ClO4 in water. Use equimolar amounts. Mix the two solutions, while
cold. KClO4 precipitates and quite pure NH4NO2 remains in solution. When this solution is allowed to evaporate, then a minor amount of white solid
remains. This is a tiny fraction of the KClO4 or NH4ClO4, which remains dissolved or some leftover reagent, because it is impossible to have exact 1 :
1 stoichiometric amounts (an error of 1% is easily made). You can easily see though, that from 1 grams of KNO2 you get well over 1 gram of KClO4,
while you only get milligrams of solid from the evaporated liquid.
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PHILOU Zrealone
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When thinking about ways to obtain directly NH4NO2 into a discrete dry form...
I came to insane genius ideas...that following me deserved a tread on their own...so I did it...
==> Dry state binary explosive mixes with transcient ammonium nitrite generation
[Edited on 13-7-2017 by PHILOU Zrealone]
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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symboom
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And also a use for ammonium nitrite
Ammonium Cobalti-nitrite, 4(NH4)3Co(NO2)6.3H2O, reaction of ammonium nitrite upon cobalt chloride solution with acetic acid. It may also be obtained
by adding semicarbazide to a solution of sodium cobalti-nitrite and by double decomposition of solutions of ammonium chloride and sodium
cobalti-nitrite; orby addition of nitrous acid to a suspension of cobalt carbonate in the requisite quantity of ammonium nitrite the salt is
precipitated out.
Ammonium cobalti-nitrite is a yellow powder, almost insoluble in cold water, yielding on warming a yellow solution, which simultaneously decomposes.
When dry the salt is quite stable, and may be kept for months without decomposition.
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PHILOU Zrealone
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Quote: Originally posted by symboom  | And also a use for ammonium nitrite
Ammonium Cobalti-nitrite, 4(NH4)3Co(NO2)6.3H2O, reaction of ammonium nitrite upon cobalt chloride solution with acetic acid. It may also be obtained
by adding semicarbazide to a solution of sodium cobalti-nitrite and by double decomposition of solutions of ammonium chloride and sodium
cobalti-nitrite; orby addition of nitrous acid to a suspension of cobalt carbonate in the requisite quantity of ammonium nitrite the salt is
precipitated out.
Ammonium cobalti-nitrite is a yellow powder, almost insoluble in cold water, yielding on warming a yellow solution, which simultaneously decomposes.
When dry the salt is quite stable, and may be kept for months without decomposition. |
I wonder if it has energetic properties if heated/shocked confined or actuated by a primer?
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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