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Author: Subject: Nitrosyl Perchlorate
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[*] posted on 13-4-2008 at 04:08


I have done the experiment of leading NOx over H5IO6. Nothing happens at all. The H5IO6 remains a dry powder.

Next, I heated the H5IO6, such that it just melts, while having it under un atmosphere of mostly NO2 (and some NO). Again, nothing happens. The solid melts, a clear colorless liquid is formed, and no NO2 or NO is absorbed in it.

I left the whole thing alone for an hour and when I came back, the white liquid had solidified again, and now it was covered with a thin layer of elemental iodine. Most likely, the periodate has oxidized some of the NOx to HNO3, itself being reduced to I2.

I also read some literature about the nitryl and nitrosyl ions. These ions need very strong acidic conditions and H5IO6 simply is not sufficiently strong, in fact, it is a fairly weak acid, even for its first proton. So, nitrosyl- or nitryl periodate is not possible, at least not along this route.




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Anders Hoveland
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[*] posted on 8-7-2010 at 23:07


madscientist:
"I wouldn't be suprised if nitrosyl perchlorate could be prepared from nitric acid and perchloric acid. That reaction may be dangerous if concentrated reactants are used!
HNO3 + HClO4 ----> H2O + O2NClO4
O2NClO4 + 2HClO4 ----> ONClO4 + HClO4 + HClO3 "


There is no reaction, only some equilibrium.
2HClO4 + HNO3 <--> H3O(+)ClO4(-) + NO2(+)ClO4(-)
your second reaction does not balance
14oxygens ---> 12oxygens , you would not get any NO(+)





[Edited on 9-7-2010 by Anders Hoveland]
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[*] posted on 9-7-2010 at 08:27


Nitric and perchloric acid can be used to get some nitronium perchlorate.

A substance (H3NO3)[ClO4]2, was made by Hantzsch (Ber. 58 [1925] 946) by adding anhydrous HClO4 into conc. nitric acid. Described as an exothermic, stable, non-explosive compound, recrystallizable from absolute perchloric acid. Later work by Goddard, Hughes, Ingold (J. chem. Soc. [1950] 2559) has found this material could be separated into nitronium perchlorate and hydroxonium perchlorate by fractional recrystallization from nitromethane. NO2ClO4 being obtained pure and structure verified by X-ray crystallography by Cox, Jeffrey, Truter (Nature, Lond. 162 [1948], 259).

Hantzsch also claimed to have made (H2NO3)ClO4 by adding conc. nitric acid into anhydrous perchloric acid. Describing this as stable, exothermic, non-explosive compound, recrystallizable from absolute nitric acid. But work from the first previous authors could not make this compound, they say he got a mixture.
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[*] posted on 9-7-2010 at 16:45


Quote: Originally posted by Theoretic  
Hmmm... Quote: "Nitrosyl perchlorate can be prepared by passing a mixture of

[snip]



I am a little late upon this. I would mention in passing that
Quote without the source .....

Another source (I am not going to quote it so I don't have
to tell you what it is, however, I'll give you a hint. Volume2
p.484) sez. essentially the same thing and references :—

K.A. Hofmann and A. Zedtwitz, Ber, 2031 (1909).
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[*] posted on 7-9-2010 at 12:15


Using equal volumes, and adding red fuming nitric acid (d= 1.52g/cc) to azeotropic conc. HClO4 under agitation gave me a white precipitate and left the liquid colorless. The resulting mixed crystals and liquid which weren't separated was very violently reactive against turpentine in very small amounts (but not towards DMSO, DMF which both just gave off white fumes at the same amounts). I'm not sure what this material is (comparisons in spectra can narrow down if it is a crystal mixture). It would be interesting to use spectra to compare these and see what it really is. One drop of the white crystals suspension on contacting about 2 drops turpentine which were spread out on a flat iron plate immediately thumped violently producing a very visible orange fireball accompanied by thick carbon/soot smoke rings and a horrible smell. It looked as something out of Hollywood on a minature scale. (Warning! Don't use more than a few drops or a very dangerous violent explosion can occur!). This violent reaction and rapid rate is in strong contrast to experiments with a bit larger amounts of moist NOClO4 solid which had added to it dumped in an excess of turpentine (hypergolics thread).
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[*] posted on 8-9-2010 at 07:58


Nitronium perchlorate, NO2ClO4, also known as nitryl perchlorate and nitroxyl perchlorate, is an inorganic chemical, the salt of the perchlorate anion and the nitronium cation. It forms colorless monoclinic crystals. It is hygroscopic, and is a strong oxidizing and nitrating agent. It may become hypergolic in contact with organic materials.

Nitronium perchlorate was investigated as an oxidizer in solid rocket propellants. Thomas N. Scortia filed for patent on such propellant in 1963.However its reactivity and incompatibility with many materials hindered such use. Coating of nitronium perchlorate particles with ammonium nitrate, prepared in situ by passing of dry ammonia gas over the particles, was investigated and a patent was awarded.

Decomposition rate of nitronium perchlorate can be altered by doping with multivalent cations.

Nitronium perchlorate and ammonium perchlorate do not produce smoke when burned with fuels. Potassium perchlorate and other metal perchlorates generate smoke as the metal chlorides are solid materials creating aerosols of their particles. Of all perchlorates, nitronium perchlorate is the most powerful oxidizer. However it can be easily detonated.

Fierce compound,hehehe:D
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[*] posted on 8-9-2010 at 10:30


Quote: Originally posted by kuro96inlaila  

Nitronium perchlorate and ammonium perchlorate do not produce smoke when burned with fuels.




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[*] posted on 12-9-2010 at 00:45


"this material could be separated into nitronium perchlorate and hydroxonium perchlorate by fractional recrystallization from nitromethane"

Would that not mean that nitronium ions (the source of HNO3's oxidizing power) were not attacking the nitromethane? Why is this?
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