Sciencemadness Discussion Board

N2O3 extraction in dichloromethane

woelen - 19-12-2021 at 07:17

I did a little experiment with making of N2O3 and checked how concentrated one can get this without decomposition, at room temperature. This compound can be extracted into DCM, which is quite interesting and also looks nice.

I added this to my electronic logbook, where I enter many experiments, which I do, which do not make it into my website:

https://woelen.homescience.net/expviewer

Check out experiment 653 (use "Experiment by ID" and then enter 653 in the form).

The dissolved N2O3 in CH2Cl2 can probably be used for other interesting reactions. I think, however, that it also contains some water, as demonstrated by the reaction with methanol.

teodor - 21-12-2021 at 00:52

It is a very nice experiment and the color of the solution is appealing.

I am thinking about

1) N2O3 + 2 H2SO4 -> 2 NOHSO4 + H2O, then getting other salts of NO+ with barium salt.
2) N2O3 + 2 NaClO4 (aq) + 2 H2SO4 -> NOClO4 + 2 NaHSO4 + H2O
and NOClO4 is a stable compound, similar to NH4ClO4 (see in the Comprehensive Inorganic Chemistry V, p.66)

I would try to repeat the experiment but I should get the nitrite salt first. I found a nice article about getting very pure nitrites, and I plan to try that.

woelen - 21-12-2021 at 04:30

Yes, I know the compound NOClO4, and I already made this.

It works much better with HClO4. Just bubble a mix of NO and NO2 (made by adding luke-warm dilute acid to solid NaNO2) through 60 - 70% HClO4. After a while, you see that a solid separates and the whole liquid turns in a white/glassy "mud". This mud is NOClO4, with some adhering water. Drying is not easy, but can be done over H2SO4. Many interesting experiments can be done, however, with the mud.

If you have NaClO4, then you can first make HClO4 by adding conc. HCl to a hot concentrated solution of NaClO4. NaCl precipitates and the remaining liquid can easily be boiled down. HClO4 is quite stable, as long as the concentration remains below 70%, it even withstands boiling hot temperatures well over 100 C.

HClO4, however, is easier to obtain. NaClO4 and KClO4 are forbidden in the EU, but you can legally obtain HClO4 (and NH4ClO4, but the latter is less useful if you are not into pyrotechnics or rocketry).

teodor - 21-12-2021 at 04:52

The compound NOClO4 is decomposing to a mixture of oxidizers of all kinds: chlorine, oxygen, nitric oxides. Does it have any pyrotechnic applications?

Update: oh I see (I found Chemical Force's video about this compound).

[Edited on 21-12-2021 by teodor]

Bedlasky - 22-12-2021 at 10:51

Nice report Woelen. This definitely go to my to do list.