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Antiswat
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[*] posted on 24-3-2013 at 10:14
Ammonium Nitrite


today i cleaned a 0.5 L PVC bottle with NO2 from Cu + HNO3..
i decided to open a bottle of 25% NH4OH aswell
NO2 + NH4OH > NH4NO2
or am i wrong?
the brown gas went very fast into white smoke alike other acid reactions in air with ammonia..
but... i have searched around on here to see if anybody have been wanting to make ammonium nitrite.. apparently not, seemingly its ''acute toxic'' that doesnt sound very pleasant..
anyways my thought about NH4NO2 is that it should be possible to make quite easily by NO2 + NH3 or even NH4OH
it could then be used to make other nitrites as i also read that it very quickly goes into H2O and N2...

NH4OH + NO2 > NH4NO2
NH4NO2 + Na2CO3 > (NH4)2CO3 + NaNO2
i really love ammonium carbonate's property to decompose in hot water..
what do you guys think.. useful or trash? the Na2CO3 could be dissolved in weak NH4OH btw




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[*] posted on 24-3-2013 at 11:12


Quote: Originally posted by Antiswat  

NO2 + NH4OH > NH4NO2
or am i wrong?


It's nitrate (NH4NO3), not nitrite (NH4NO2), that is being formed.




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[*] posted on 24-3-2013 at 13:14


'Sure the nitrite in equimolar mixture with nitrate isn't formed?
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[*] posted on 24-3-2013 at 13:17


i see the problem with NH4OH, but NH3 dissolved in water is referred to as NH4OH tho the NH3 is still just whats in there..
but still if using sodium carbonate to get sodium nitrite wouldnt it still be relatively useful? there must be some way to seperate NaNO3 from NaNO2 if NO3 would be formed..




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https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 24-3-2013 at 13:34


There's a very long nitrites thread, that's your best starting point...



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[*] posted on 25-3-2013 at 05:28


I suspect that you get a mixture of ammonium nitrite and ammonium nitrate;

2NO2 + 2NH3 + H2O -> NH4NO2 + NH4NO3

Nitrites are only acutely toxic if swallowed and even then they are a lot less poisonous than sodium azide, sodium cyanide, etc.
Sodium nitrite is a constituent of Prague powder aka curing salt.

http://en.wikipedia.org/wiki/Curing_salt
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[*] posted on 25-3-2013 at 08:08


Quote: Originally posted by blogfast25  
There's a very long nitrites thread, that's your best starting point...


yes.. i searched on SM for it but i didnt find anything.. only that ammonium nitrite was mentioned very few times and nothing really about synthesis




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 25-3-2013 at 08:11


Quote: Originally posted by ScienceSquirrel  
I suspect that you get a mixture of ammonium nitrite and ammonium nitrate;

2NO2 + 2NH3 + H2O -> NH4NO2 + NH4NO3

Nitrites are only acutely toxic if swallowed and even then they are a lot less poisonous than sodium azide, sodium cyanide, etc.
Sodium nitrite is a constituent of Prague powder aka curing salt.

http://en.wikipedia.org/wiki/Curing_salt



but yes a mixture.. still alot more safe to do that to start boiling sodium nitrate with charcoal in it
even after NaNO3 + C you should still have an amount of NaNO3 in it, so it should be useful, if anybody would care to attempt getting nitrites this way




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 25-3-2013 at 08:20


I suppose that sodium nitrite + ammonium perchlorate would form ammonium nitrite and sodium perchlorate.



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[*] posted on 25-3-2013 at 08:43


ammonium nitrite is not stable past -20C if i remember correctly so, it is likely even if you did form any that it is all gone.
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[*] posted on 25-3-2013 at 08:52


It seems that ammonium nitrite is stable as long as you look after it;

http://en.wikipedia.org/wiki/Ammonium_nitrite

But I tend to agree that the major component of the reaction product would be the nitrate and it would gradually tend to be the only component due to oxidation and decomposition of the nitrite.

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[*] posted on 25-3-2013 at 10:25


An interesting experiment would be to mix a concentrated solution of KNO2 and a concentrated solution of NH4ClO4. KClO4 will precipitate and form a fairly compact crystalline solid and NH4NO2 remains in solution. Maybe this is a possible way to make NH4NO2 (contaminated with only a very limited amount of KClO4). I have lots of NaNO2, but only a very limited amount of KNO2 (the latter is hard to find and expensive, while NaNO2 is easy to find and very cheap). I'll try on a test tube scale and see if I can get the solution to evaporate in a warm place and obtain solid NH4NO2, I do not have enough KNO2 to test on a somewhat larger scale. Besides that, NH4NO2 is said to be very unstable and may decompose explosively.



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[*] posted on 25-3-2013 at 10:44


It looks like you can make ammonium nitrite but heating it is a bit of a no no;

http://pubs.rsc.org/En/content/articlelanding/1911/ct/ct9119...

And it seems that we have chewed over this one before;

http://www.sciencemadness.org/talk/viewthread.php?tid=6650

:D

And another reference to a preparation;

http://www.ias.ac.in/resonance/Jan2001/pdf/Jan2001p42-49.pdf

I do not like patents but this looks workable

http://www.freepatentsonline.com/2285843.pdf

[Edited on 26-3-2013 by ScienceSquirrel]
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[*] posted on 26-3-2013 at 02:11


@ScienceSquirrel Please, be careful about triple-posting.

@woelen NaClO4, which would form, is highly soluble in water, so getting NH4NO2 out will certainly be difficult. Try to use the ammonium nitrite generated to do something interesting, such as hydroxylamine synthesis or some organic chemistry.




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[*] posted on 26-3-2013 at 02:26


Quote: Originally posted by Eddygp  
@woelen NaClO4, which would form, is highly soluble in water, so getting NH4NO2 out will certainly be difficult.
That's why I want to do the experiment with KNO2 instead of NaNO2. Because I only have a little amount of KNO2 I have to stick to test tube scale experiments and can only use a few hundreds of mg in my experiments.

I hope that the NH4NO2 does not immediately decompose to water and N2. The experiment will give the answer.


[Edited on 26-3-13 by woelen]




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[*] posted on 26-3-2013 at 08:54


Quote: Originally posted by Eddygp  
I suppose that sodium nitrite + ammonium perchlorate would form ammonium nitrite and sodium perchlorate.


sounds about right.. but the problem is if you dont have any source of NaNO2 in first place..




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 26-3-2013 at 08:55


Quote: Originally posted by ThatchemistKid  
ammonium nitrite is not stable past -20C if i remember correctly so, it is likely even if you did form any that it is all gone.


thats why you should add Na2CO3 to the solution, so the freshly formed NH4NO2 would react with the Na2CO3 to create NaNO2 and (NH4)2CO3, which decomposes very easily




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 26-3-2013 at 08:59


Quote: Originally posted by woelen  
An interesting experiment would be to mix a concentrated solution of KNO2 and a concentrated solution of NH4ClO4. KClO4 will precipitate and form a fairly compact crystalline solid and NH4NO2 remains in solution. Maybe this is a possible way to make NH4NO2 (contaminated with only a very limited amount of KClO4). I have lots of NaNO2, but only a very limited amount of KNO2 (the latter is hard to find and expensive, while NaNO2 is easy to find and very cheap). I'll try on a test tube scale and see if I can get the solution to evaporate in a warm place and obtain solid NH4NO2, I do not have enough KNO2 to test on a somewhat larger scale. Besides that, NH4NO2 is said to be very unstable and may decompose explosively.


we could call it interesting properties aswell..
i think you might wanna leave the NH4NO2 solution in a large surface thing to evaporate below 60*C and then dessicate the rest off.. if you manage to isolate NH4NO2 you could basically make any nitrite, by reacting it with a carbonate.. (NH4)2CO3 is becoming my favorite chemical..




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 26-3-2013 at 09:21


Quote: Originally posted by ScienceSquirrel  
It looks like you can make ammonium nitrite but heating it is a bit of a no no;

http://pubs.rsc.org/En/content/articlelanding/1911/ct/ct9119...

And it seems that we have chewed over this one before;

http://www.sciencemadness.org/talk/viewthread.php?tid=6650

:D

And another reference to a preparation;

http://www.ias.ac.in/resonance/Jan2001/pdf/Jan2001p42-49.pdf

I do not like patents but this looks workable

http://www.freepatentsonline.com/2285843.pdf

[Edited on 26-3-2013 by ScienceSquirrel]



i did search up for ammonium nitrite tho.. they dont really describe the idea i have for it, tho..
but its interesting that its still seen as a very unstable compound nearly impossible to create when it has been researched about and found out, and also published to be more stable than thougt before..
a problem with the NO2 might be that it would be needed to be anhydrous, but that is easily done by decomposition of Cu(NO3)2, where the CuO leftover from the reaction can be made into Cu(NO3)2 again with HNO3.. Cu(NO3)2 can also be purchased on some sites.. think ive seen 1kg for sale on a art site for 22€




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 26-3-2013 at 09:26


Quote: Originally posted by woelen  
Quote: Originally posted by Eddygp  
@woelen NaClO4, which would form, is highly soluble in water, so getting NH4NO2 out will certainly be difficult.
That's why I want to do the experiment with KNO2 instead of NaNO2. Because I only have a little amount of KNO2 I have to stick to test tube scale experiments and can only use a few hundreds of mg in my experiments.

I hope that the NH4NO2 does not immediately decompose to water and N2. The experiment will give the answer.


[Edited on 26-3-13 by woelen]


according to sciencesquirrels link, a indian scientist stated that it wasnt really as unstable as thought of before, but it wouldnt be a very good thing to find out it was much more unstable than he thought, anyways.
the best would be to isolate it, then you could measure out some for some other reactions, such as suggested organic
perhaps it would be insoluble in ethanol, methanol or some other solvents, and could more easily be isolated by precipitating it with something its insoluble in, such as the procedure for TACS and TACN (IIRC i did this with TACN aswell to ppt the TACN out)




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 26-3-2013 at 09:33


NH4NO2 is definitely unstable, but not as unstable as some other compounds. I don't know if I have read it here or in other place, but a conc. solution of NH4NO2 is more prone to explode than crystalline, solid NH4NO2.
By the way, [SPOILER]Looks like everyone is more-than-double-posting here today, eh?[/SPOILER]





[Edited on 26-3-2013 by Eddygp]




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[*] posted on 26-3-2013 at 13:33


I dissolved 470 mg of NH4ClO4 in a few ml of water and 340 mg of KNO2 in another small amount of water. Then I mixed the two liquids. Qucikly a fine crystalline precipitate is formed. This precipitate fairly quickly settles at the bottom and the clear colorless liquid could be taken away from the precipitate with a pasteur pipette. The white solid is KClO4. Appr. 70% of the liquid could be recovered with the pipette, the rest sticks to the KClO4.

I transferred the clear liquid to a petri dish and put this in a warm place (around 40 C, not warmer than that). After 3 hours, at least half of the liquid is gone, still no crystals. At the glass there were many bubbles, somewhat like the bubbles of a soft drink which stick to the glass. I suspect partial decomposition to N2 and water. Tomorrow I will see what remains.




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[*] posted on 26-3-2013 at 16:21


Quote: Originally posted by Eddygp  
NH4NO2 is definitely unstable, but not as unstable as some other compounds. I don't know if I have read it here or in other place, but a conc. solution of NH4NO2 is more prone to explode than crystalline, solid NH4NO2.
By the way, [SPOILER]Looks like everyone is more-than-double-posting here today, eh?[/SPOILER]

its hard to reply to more than one using only one comment (;



[Edited on 26-3-2013 by Eddygp]




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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[*] posted on 27-3-2013 at 00:08


Yes, I know and I read this, but I just wanted to try it myself. I too often have read something in books and on Wiki-pages and then found out that reality is at least more subtle than the books and sometimes the books are plain wrong.

I now am at work, but this evening I'll have a look at it again and then I'll see whether there is solid NH4NO2 or just nothing left.




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[*] posted on 27-3-2013 at 01:56



You may prepare NH4NO2 by reaction of (NH4)2SO4 (or NH4Cl, I think) and NaNO2 in 95% ethanol. Details can be found in orginal article (in German): Z. Elektrochem. 11, 409-413 (1905).
Purification is described in the same journal, but it is not very interesting - by fractional precipitation with ether (from ethanol).
By the way, solubility of NH4NO2 in water is ~200g/100g (20 C)

[Edited on 27-3-2013 by kmno4]




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