APO
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Nitronium Perchlorate
I can't find ANY synthesis what so ever on Nitronium Perchlorate,I can only find Nitrosyl Perchlorate synthesis. So does anyone Know how to make
Nitronium Perchlorate?
"Damn it George! I told you not to drop me!"
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plante1999
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I can find one easily by looking in references book. You shouldn't play with that if you don't want to use dangerous sulphuric acid. HA HA HA
Better to start with safer stuff, K3wl.
[Edited on 19-3-2013 by plante1999]
I never asked for this.
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AndersHoveland
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Quote: Originally posted by BromicAcid  | | Anyway, I can't seem to find nitrosyl perchlorate in my chemistry encyclopedia, no surprise but I do have nitronium perchlorate in here, NO2ClO4, it's
formed from ozone, nitrogen dioxide, and chlorine dioxide, highly reactive, soluble in water to nitric and perchloric acids, may explode, etc.
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| Quote: Originally posted by Formatik | 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. |
I am sure it could also be formed by dissolving N2O5 into Cl2O7, if there was not just an explosion.
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Motherload
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That stuff for me is theoretical ....
Energetics is one thing .... But that stuff is a breed of its own.
I ain't into pyrophorics and that.
I wouldn't recomend synthesizing that .... It will set literally any thing on fire (if your lucky) and explode in most cases.
"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
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AndersHoveland
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It would be a very powerful nitrating agent, however. Despite the instability and explosion hazard, it could still be a sufficient substitute in
procedures where nitronium tetrafluoroborate (NO2BF4) is called for.
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APO
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No synthesis?
"Damn it George! I told you not to drop me!"
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caterpillar
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How old are you? Ten? Or even eleven? I cannot give you more due to the nature of your questions. Try something like preparation of large carbon
crystals- chances to success will be the same.
Women are more perilous sometimes, than any hi explosive.
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Motherload
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APO. There is many other ways of hurting yourself.
Please don't pick science/chemistry or guns.
Stay away from that stuff. Most pro labs don't have the equipment
to handle and synthesize that.
"Chance favours the prepared mind"
"Fuck It !! We'll do it live !!"
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plante1999
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APO, you would be better to learn some chemistry, use strong acid and base, and after a few month/ year of intensive learning you could play with
energetics, and after a few year with energetic you could play with nitronium perchlorate.
I never asked for this.
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AndersHoveland
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There is a synthesis for nitronium tetrafluoroborate. My guess is that it could be reacted with sodium perchlorate to obtain the nitronium
perchlorate.
NO2BF4 + NaClO4 --> NaBF4 + NO2ClO4
As for how to separate the products, I am not entirely sure. My guess would either be (very) cautious vacuum "distillation" (read= sublimation), or
extracting with nitronium perchlorate with some solvent (nitromethane or methylene chloride might work).
You would likely kill yourself trying it, APO. The following information is being provided for information purposes only.
| Quote: |
Nitronium tetrafluoroborate can be prepared by adding a mixture of anhydrous hydrogen fluoride gas and boron trifluoride to a solution of either
highly concentrated nitric acid or nitrogen pentoxide dissolved in nitromethane.
WARNING: Rubber gloves, an apron, and a plastic face mask are strongly recommended. All operations should be carried out in a hood.
If hydrogen fluoride comes in contact with the skin, the contacted area should be thoroughly washed with water and then immersed in ice water while
the patient is taken to rushed to the emergency department. Burns caused by hydrogen fluoride may not be noticed for several hours, by which time
serious tissue damage may have occurred.
Note: Any operations involving liquid hydrogen fluoride must be carried out with equipment resisting hydrogen fluoride, such as fused
silica, polyolefin, monel steel, or teflon. Kel-F grease is recommended for ground-glass joints. Nitronium tetrafluoroborate slowly attacks silicone
stopcock grease, causing air to enter the flask. After completion of the reaction, all equipment should be washed with plenty of water.
A 1-L three-necked polyolefin flask is provided with a short inlet tube for nitrogen, a long inlet tube for gaseous boron trifluoride, a drying tube,
and a magnetic stirring bar. The flask is immersed in an ice-salt bath and flushed with dry nitrogen. Under a gentle stream of nitrogen and with
stirring, the flask is charged with 400 ml. of methylene chloride, 41 ml. (65.5 g., 1.00 mole) of red fuming nitric acid (95%), and 22 ml. (22 g.,
1.10 moles) of cold, liquid, anhydrous hydrogen fluoride. 5. It is convenient to condense anhydrous hydrogen fluoride, b.p. 19.5°, from a cylinder
into a small calibrated polyolefin flask immersed in a mixture of dry ice and acetone. As hydrogen fluoride is very hygroscopic, it should be
carefully protected from atmospheric moisture, preferably by maintaining an atmosphere of dry nitrogen over it, otherwise by means of a drying tube.
The hydrogen fluoride is then simply poured into the reaction flask.
Gaseous boron trifluoride (136 g, 2.00 moles) from a cylinder mounted on a scale is bubbled into the stirred, cooled reaction mixture. (The
temperature of the reaction is not critical, but the reaction is slower at higher temperatures because of the lower solubility of boron trifluoride in
the solvent). The first mole is passed in rather quickly (in about 10 minutes). When approximately 1 mole has been absorbed, copious white fumes begin
to appear at the exit, and the rate of flow is diminished so that it takes about 1 hour to pass in the second mole; even at this slow rate, there is
considerable fuming at the exit. After all the boron trifluoride has been introduced, the mixture is allowed to stand in the cooling bath under a slow
stream of nitrogen for 1.5 hours. The mixture is swirled, and the suspended product is separated from the supernatant liquid by means of a
medium-porosity, sintered-glass Buchner funnel. Note that since free hydrogen fluoride is no longer present, filtration can be carried out with glass
or porcelain equipment.
The gooey solid remaining in the flask is transferred to the funnel with the aid of two 50-ml. portions of nitromethane. The solid on the funnel,
nitronium tetrafluoroborate, is washed successively with two 100-ml. portions of nitromethane and two 100-ml. portions of methylene chloride. In order
to protect the salt from atmospheric moisture during the washing procedure, suction is always stopped while the salt is still moist. The moist salt is
transferred to a round-bottomed flask and dried by evaporating the solvent. At the end of the procedure the flask can be gently heated to 40–50°C
(Nitronium tetrafluoroborate is thermally stable up to 170°. Above this temperature it starts to dissociate into nitryl fluoride and boron
trifluoride.) The yield of colorless nitronium tetrafluoroborate is 85–106 g. (64–80%) It is stored in a wide-mouthed polyolefin bottle with a
screw cap. The edge of the cap is sealed with paraffin wax after it is screwed on. Nitronium tetrafluoroborate is very hygroscopic. It is stable as
long as it is anhydrous, but it is decomposed by moisture, and all transfers should be in a dry box.
Nitronium tetrafluoroborate slowly attacks polyethylene and polypropylene, but apparatus made of these materials will last for several preparations of
the salt.
The last part of the procedure can be used to purify nitronium tetrafluoroborate that has picked up water on standing. The impure salt is washed twice
with nitromethane, twice with methylene chloride, and is dried under reduced pressure.
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Boron Trifluoride BF3
Boron trifluoride is a very toxic gas, which readily reacts with water to form metaboric acid and Fluoroboric acid, which then can further hydrolyze
if excess water is present. It is a strong fluoride ion abductor, meaning it will pull a fluorine atom from many covalent compounds to form the
tetrafluoroborate anion (BF4-), while leaving a positively charged cation. However, boron trifluoride is not as powerful of an abductor as antimony
pentafluoride, as demonstrated by its unreactivity towards trichlorofluoromethane.
| Quote: |
Boron trifluoride may be prepared by heating a mixture of boric oxide and calcium fluoride with concentrated sulfuric acid. It may also be prepared by
mixing 5 parts of potassium borofluoride (KBF4) with 1 part finely powdered boric oxide, then heating with concentrated sulfuric acid. The boron
trifluoride, can be collected over mercury. Potassium borofluoride may be produced by heating together 2 parts boric acid, 5 parts CaF2, and 10
parts conc H2SO4. The liquid is then cooled and filtered, and a solution of a potassium salt is added. Potassium borofluoride precipitates out, and
may then be recrystallized from hot water. By this method it can be prepared as anhydrous hexagonal crystals. If it is prepared instead from
hydrofluoric acid, boric acid, and K2CO3, a gelatinous mass forms instead, which however forms cubic octahedral and cubic dodecahedral crystals when
heated to 100 degC.
Boron trifluoride also results from heating a mixture of boric oxide and calcium fluoride to a white heat in an iron pipe. Heating solid borofluorides
to red heat, boron trifluoride is evolved, leaving behind metal fluorides.
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[Edited on 20-3-2013 by AndersHoveland]
I'm not saying let's go kill all the stupid people...I'm just saying lets remove all the warning labels and let the problem sort itself out.
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Theoretic
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AndersHoveland that was WOW! i especially loved the 'fluoride ion abductor' part 
but... saying it is less powerful than SbF5 because it does not attack CCl3F implies that SbF5 DOES attack it 
have you any references pertaining to that?
w/regard to the NO2ClO4 synthesis wouldn't it be better to have nitronium sulfate as a starting material? From NaNO3 and SO3 it could be obtained
easily, and sodium sulfate would fall into the ppt reasonably well (it's known to be a tenacious and high-melting product when HCl is prepared from
salt and sulfuric acid, and the reason an excess of H2SO4 is used so NaHSO4 results instead, so we know it has a strong lattice)
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APO
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How accurate is this from an old Megalomania archive?
"Nitryl perchlorate can be prepared by distilling anhydrous perchloric acid, allowing the distillate to drip onto a large excess of dry dinitrogen
pentoxide chilled to -80 °C (yes that's negative) and some nitromethane. The mixture is allowed to warm to room temperature, then kept under vacuum
for 48 hours to remove any volatile contaminants."
He referred to Nitronium Perchlorate as Nitryl Perchlorate. Also my ignorance is a result of the public school system, but I assure you guys at this
point of my little knowledge of energetics, these are are just questions. I'm aware this is higher level chemistry, and that I come across quite dumb.
I won't do anything with the real stuff until I have a full hazmat suit.
"Damn it George! I told you not to drop me!"
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woelen
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Even with a full hazmat suit this procedure is madness when no other special precautions are taken. Did you ever read about the properties of
anhydrous HClO4? Do you really believe that you will play with that like you play with a toy? Even most professional labs do not have the facilities
to handle this beast in an only somewhat safe way. You need a special fume hood with slowly running water along the walls and suction system,
otherwise later (or sooner!) an explosion will occur. Anhydrous perchloric acid cannot be stored under normal conditions. Literature states that after
approximately 1 month of storage at room temperature it explodes! Distilling this stuff is next to insane.
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APO
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Well, would vacuum distillation help?
"Damn it George! I told you not to drop me!"
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