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Author: Subject: N2O5 from NO2 and Ozone?
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[*] posted on 27-4-2021 at 15:35
N2O5 from NO2 and Ozone?


Hey everyone, I've recently managed to ampoule liquid N2O3 and NO2 using dry ice baths, borosilicate ampoules, and resin (for ampoule reinforcement in safekeeping). The process of ampouling these nitrogen oxides is fairly simple and very similar to the ampouling of liquid chlorine in terms of temperature of the condensation and vapor pressure of the condensed liquid. Though I haven't finished my video on making these ampoules yet, the process I used to make them is very similar to that used in this video:
https://www.youtube.com/watch?v=udf-KSMd8yw
Here's my question.
It's well known that a gaseous mixture of ozone and NO2 can form dinitrogen pentoxide at a wide range of temperatures. Similarly, NO reacts with ozone though similar steps, yielding NO2 first, and then N2O5 through formation of the nitrate radical. I recently purchased an industrial ozone generator that claims a production of 60 grams per hour (hardly believable) but reviews of the generator are largely positive. Among other things, I'd like to try synthesizing N2O5 by direct oxidation of NO2/N2O4 with Ozone at ~ -10 degrees Celsius. My plan is to build a plastic housing (might break down over time) in which I can feed pure O2 into the Ozone generator and let it accumulate until around a 10% gaseous concentration. At this point I'd have a aquarium pump bubble the Ozone into the liquid NO2/N2O4, oxidizing any present N2O3 and hopefully some NO2 as well.
If this method works, it could be a relatively simple method of N2O5 preparation, however I don't have any clue if it would definitively work quite yet. I can only hope that being a mega-oxidizer the Ozone will do its job even at these low temps.
If anyone has any guesses of whether or not this will work, I'd be happy to hear them.

Here's a picture of some of the N2O3 ampoules in resin that I sell.


N2O3.jpg - 1.7MB




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[*] posted on 27-4-2021 at 23:04


NO2 and ozone indeed are said to react with each other, giving N2O5 (some textbooks even claim further oxidatin to NO3, but the latter is questionable). I do not know, however, how fast this reaction is. I have no personal experience with it.

Another route to N2O5 is reaction of fuming white nitric acid with P4O10 and distilling at reduced pressure. N2O5 is not very stable and I have read somewhere that it decomposes in a month or so, when stored at room temperature. Are you planning to ampoule this solid? If so, I strongly advice you not to do so. N2O5 decomposes to NO2 and O2 and especially the O2 will give a very high pressure in the ampoule.

Of course, if you want to make N2O5 for certain syntheses or for chemical demonstrations, then that would be great and I would love to see your results shared over here.

[Edited on 28-4-21 by woelen]




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[*] posted on 28-4-2021 at 03:00


Reaction of NO and ozone is used in analytical chemistry to measure amount of nitrogen oxides through chemiluminescence. NO react with ozone to produce NO2 in excited state, which than goes to the ground state and produce visible light.

https://en.wikipedia.org/wiki/Chemiluminescence#Gas-phase_re...




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[*] posted on 28-4-2021 at 05:59


Quote: Originally posted by woelen  
NO2 and ozone indeed are said to react with each other, giving N2O5 (some textbooks even claim further oxidatin to NO3, but the latter is questionable). I do not know, however, how fast this reaction is. I have no personal experience with it.

Another route to N2O5 is reaction of fuming white nitric acid with P4O10 and distilling at reduced pressure. N2O5 is not very stable and I have read somewhere that it decomposes in a month or so, when stored at room temperature. Are you planning to ampoule this solid? If so, I strongly advice you not to do so. N2O5 decomposes to NO2 and O2 and especially the O2 will give a very high pressure in the ampoule.

Of course, if you want to make N2O5 for certain syntheses or for chemical demonstrations, then that would be great and I would love to see your results shared over here.

[Edited on 28-4-21 by woelen]


Yeah, I gave up on the idea of potentially ampouling the N2O5 several weeks ago after seeing the rate of decomposition on storage. Not entirely sure how much pressure the resin blocks can hold but testing them to the vapor pressure of oxygen is not something I want to try out.
A friend of mine who goes by “ReactiveChem” on YouTube has produced N2O5 in the manner you illustrated with dehydrating agents and vacuum distillation. I believe his video is still up on either YT or his BitChute. Personally, if this ozone reaction works at the temps I’m hoping for, this would be a lot easier for me to synthesize the N2O5. No need to destroy a vaccumn pump if I can buy dry ice in abundance.
There’s certainly a plethora of highly technical nitrations I could try with the N2O5, with many in pursuit of energetic end products. For now I’m mainly looking at the synthesis as a video idea with not too much else planned.
Thanks!




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[*] posted on 28-4-2021 at 06:12


Quote: Originally posted by Bedlasky  
Reaction of NO and ozone is used in analytical chemistry to measure amount of nitrogen oxides through chemiluminescence. NO react with ozone to produce NO2 in excited state, which than goes to the ground state and produce visible light.

https://en.wikipedia.org/wiki/Chemiluminescence#Gas-phase_re...


Ah, that’s very interesting! I had no clue that there was such a reaction. I’ll definitely have to try that out and get some footage of it.
I guess that would also confirm my assumption that ozone would first oxidize NO to NO2, and then to the NO3 radical. From there I believe the NO3 reacts with NO2 and directly forms the N2O5 endproduct.




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