Sciencemadness Discussion Board

Liquid Nitrogen Dioxide

subsecret - 17-8-2013 at 18:59

Have any of out members tried to condense NO2? It looks pretty awesome, just take care not to break the vial..

http://www.youtube.com/watch?v=ikNVn8P4h2E

plante1999 - 17-8-2013 at 19:07

I case you wondered, a member have mad liquid NO2 and taken picture of it, there is picture of it somewhere on the forum.

The_Davster - 17-8-2013 at 19:10

Yup, it is not too difficult. I never tried to ampoule it though....

plante1999 - 17-8-2013 at 19:18

I forgot to say the member was me, anyhow, it is very easy, and very fun to do so. Would do more ofttimes if rubber tubing was not destroyed in the process.

subsecret - 17-8-2013 at 19:26

I wouldn't like to be around if a bottle of liquid NO2 broke... Do you still have the sample?

plante1999 - 17-8-2013 at 19:29

Not about the bottle, but liquid NO2, never had a vial of it, I stirred it outside for the day I needed it, it was like -30 outside.

The picture is somewhere around...

[Edited on 18-8-2013 by plante1999]

Pulverulescent - 18-8-2013 at 01:26

Quote:
]Have any of out members tried to condense NO2? It looks pretty awesome . . .

It also looks very impure ─ the green colour suggests the sample consists of mixed NOx!
Possibly N2O3, . . . ?

Mailinmypocket - 18-8-2013 at 05:08

Check this out

kristofvagyok - 18-8-2013 at 05:16



In pure form it looks like this. If it's green or blue (as on that video) it contains a lot N2O3 instead of N2O4.

Pyro - 20-8-2013 at 11:18

Kristof, do you keep the sample cold? is the ampule special (thick walled)?


[Edited on 20-8-2013 by Pyro]

Pulverulescent - 20-8-2013 at 11:40

Quote:
is the ampule special (thick walled)[sic]?

It should be obvious to all but the meanest of intellects and the dimmest of eyes that the pictured ampoule is of the regular variety . . .

BromicAcid - 20-8-2013 at 13:11

Made a nice mix of liquefied nitrogen oxides once upon a time. Before I knew better I tried to atmospherically distill a mix of NaNO<sub>3</sub> with concentrated sulfuric acid. Nearly 50 mL of deeply colored distillate that refused to behave like nitric acid. Took me sometime to realize the folly of my ways.

I Like Dots - 20-8-2013 at 17:50

ME TOO BromicAcid. It was before I had a proper hotplate. It was not hot enough to boil the acid, only produce lots of NOx! Iit was redish and im thinking "hmm it must have a lot of nitrogen oxides dissolved.":D

But kristofvagyok You always post the best pictures and i envy whatever it is you do :)

Pyro - 20-8-2013 at 17:58

oh fuck you pulverulescent! :)
his ampule just looks nothing like mine, thats why I ask

Pulverulescent - 21-8-2013 at 00:58

So! Yours is one the that's thick?

jock88 - 21-8-2013 at 03:57

Quote: Originally posted by Pulverulescent  
Quote:
is the ampule special (thick walled)[sic]?

It should be obvious to all but the meanest of intellects and the dimmest of eyes that the pictured ampoule is of the regular variety . . .


What exactly is a 'regular variety' of ampule?



Pulverulescent - 21-8-2013 at 11:05

Well, let's see ─ 'the type most commonly encountered' . . . ?
'Hope that helps?

kristofvagyok - 21-8-2013 at 11:56

Quote: Originally posted by Pyro  
Kristof, do you keep the sample cold? is the ampule special (thick walled)?

Hi,

It is not a "sample", it is a commonly used reagent for nitration, so we have a bunch on these. The ampule is normal, not thick wall, no special glass, nothing, it's a common glass ampule. The only thing to note that it should be chilled when sealed.

Pyro - 21-8-2013 at 13:52

How did you make it? did you distill,...?

kristofvagyok - 21-8-2013 at 22:36

I have no idea where it came from, circa 30 year old ampules, so it could be from Russia, but there is also a chance that someone made it.

Oscilllator - 21-8-2013 at 23:50

I would like to point out that 5 seconds of internet searching reveals NO2 has a boiling point of 21 degrees, so there is no reason to use a thick-walled ampule.

Jylliana - 17-12-2014 at 03:07

*UTFSE*

I have this idea of ampouling some gaseous nitrogen dioxide by leading it into the ampoule through a rubber tube, clamping the tube and then flame sealing the ampoule right before the connection tube-ampoule.. I'll lose some of the gas, but in theory it should also trap some gas in the ampoule.

Does my idea sound reasonable or completely ridiculous? I don't want to do things that are very dangerous, so I ask first before doing anything stupid... :)

hissingnoise - 17-12-2014 at 03:32

Quote:
I don't want to do things that are very dangerous, so I ask first before doing anything stupid.

Nitrogen dioxide must not be allowed contact with organics, period!

Mixtures of NO2 and liquid hydrocarbons are sensitive, powerful explosives in their own right!

No contact with rubber/plastic ─ all glass apparatus must be used!


Jylliana - 17-12-2014 at 03:56

Okay. No-go, then. Good thing I asked before trying. I didn't know about the explosives-part. Thanks for your answer.

diddi - 17-12-2014 at 04:03

I would be condensing the NO2 gas from your reaction vessel in ice/water slush bath and sitting your ampoule in similar conditions. the liquid NO2 will just drip into the ampoule and when full enough, you can seal her up! don't go too cold (eg salt/ice) as NO2 freezes at around -10C

woelen - 17-12-2014 at 04:16

Jylliana, you can make an ampoule of NO2 in that way. I made ampoules of NO2 and Cl2 that way. I had a gas generator, used a mix of P4O10 and CaCl2 to dry the gas and flooded the ampoule with a lot of gas, while slowly retreating the PVC tube from which the gas was streaming. Then I quickly sealed the ampoule.

The result is shown here (for the Cl2-ampoule, the NO2 ampoule is not on wikipedia):

http://en.wikipedia.org/wiki/Chlorine#mediaviewer/File:Chlor...

There is no need to fear explosions or other nasty things with NO2, when you lead some of it through a plastic tube. The issues, mentioned by hissingnoise only become serious if there is prolonged contact with rubber, plastics and so on. E.g. if you perform a reaction with gaseous NO2 and you lead the gas through plastic tubes for hours, then there may be a problem, but not if you make some gas, suck it in a 100 ml syringe, filled with some P4O10/CaCl2 mix and then slowly blow it in a glass ampoule of 20 ml.

Jylliana - 17-12-2014 at 06:12

The method worked like a charm!
My setup:


My ampoule:



Thanks for your answers :)

Zyklon-A - 17-12-2014 at 08:37

I've condensed some N2O4 using a GG distillation setup and dry ice acetone bath for a coolant.
Worked like a charm, but I unfortunately didn't have a working torch at the time (7-8 months ago) so I couldn't ampule any of it.

neptunium - 17-12-2014 at 08:41

NO2 condenses at arround 20 C with a vapor preassure of less than 1 atm..(approx)
its not supprising it can be contained in a weak regular ampoule...
unlike Chlorine or other gases requireing too much preassure, NO2 can be kept liquid sealled if it does nt get too hot ...

hissingnoise - 17-12-2014 at 09:50

Quote:
The issues, mentioned by hissingnoise only become serious if there is prolonged contact with rubber, plastics and so on.

Indeed woelen, I'm guilty of what I accused Bert of doing . . .

And I fed NO2 through plastic tubing from a Jacob's Ladder years ago, without incident . . .

An amorphous, yellow powder which deflagrated weakly, was found within the tubing . . .

But you know how it is; you read enough about panclastites and next thing you know . . .


Jylliana - 17-12-2014 at 12:23

I appreciate your warnings and thoughts about it, hissingnoise.
I flushed the tubing with a bucketload(let my vacuümpump run for 20 minutes) of air and water directly after usage. That should prevent anything dangerous from depositing on the insides of the tubes. Without knowing what could happen, I might have not done that.

[Edited on 17-12-2014 by Jylliana]