Sciencemadness Discussion Board

nitric acid syntesis go very wrong

plante1999 - 4-1-2011 at 17:43

reactant

flask:
40g copper
85g ammonium nitrate
150ml 20% HCl

test tube:
5ml 3%H2O2

picture at 13h00 10minute after the starting of the reation.



14h00 the reaction go very very rapid the H2O2 is now yellow(why is it, nitrogen oxide?)


14h10

the stopper litteraly explode and splach arround 100ml of HCl everyware.

15h00 testing of the nitric acid, very reactive.

(I wear all the safaty equipement needed so I dont ave any burn)

(it is based about the nurdrage video tutorial)

[Edited on 5-1-2011 by plante1999]

[Edited on 5-1-2011 by plante1999]

[Edited on 5-1-2011 by plante1999]

[Edited on 5-1-2011 by plante1999]

plante1999 - 4-1-2011 at 18:17

edit: the wall is plated with a aluminium oxide coated sheet.
and the table is made from glass.(its look like wood or steel but its is only the support of the glass)

[Edited on 5-1-2011 by plante1999]

not_important - 4-1-2011 at 18:18

NH4NO3 + HCl <=> NH4Cl + HNO3

HCl plus HNO3 is aqua regia http://en.wikipedia.org/wiki/Aqua_regia

which rapidly forms NOCl and Cl2 along with various nitrogen oxides.

Thermal run-away, giving overheating with rapid gas formation and boiling, seems to be likely unless you monitor and control the temperature; and/or use the proper concentrations to prevent run-away.

The intent would seem to be to react NO3(-0) with H+ and Cu to form NO2, then dissolve that in the dilute H2O2 to form HNO3. I suspect you can get some HNO3, but it will dilute and contain chlorine in one state or another.

Arthur Dent - 5-1-2011 at 04:15

Just out of curiosity, is your Ammonium Nitrate reagent grade or is is coming from cold pack compresses?

I ask because usually the Ammonium Nitrate in those packs is quite pure, but some brands have urea mixed in. That might produce an "unexpected" result!

Robert

plante1999 - 5-1-2011 at 04:48

it is from cold pack but i dont think it have impurity.

Random - 5-1-2011 at 06:08

Did you put that plastic tube directly on the test tube without any space for the gas to escape? If yes, the pressure built up from undissolved gas and maybe that caused it to explode.

plante1999 - 5-1-2011 at 06:11

no i put a 1/4poly tube in a 1/2inch tyest tube.

Random - 5-1-2011 at 07:19

Maybe a small amount of NCl3 formed or something like that, or maybe that poly tube was nitrated by no2.

plante1999 - 5-1-2011 at 07:45

yes i think it is someting like that because the explausion have destroyed th stopper and splash HCl at 14feet high

syntesi of 65% nitric acid from simple apparatus

plante1999 - 5-1-2011 at 09:22

I am thinking to test this apparatus i ave made, heating the large beaker at 50degree Celsius.




[Edited on 5-1-2011 by plante1999]

plante1999 - 5-1-2011 at 10:11

so after talking, working.

result: verry verry verry pur nitric acid no yellow, white fumming nitric acid.

reactan 20ml 95%sulfuric acid
30g of ammonium nitrate

result 10ml acid

(I test it with copper an no reaction adition of small ammount of watter and very vigourus reacdion with emition of nitrtogen dioxide.

i will post a picture latter.

[Edited on 5-1-2011 by plante1999]

metalresearcher - 5-1-2011 at 12:36

Nice trick to make HNO3 !
But how does it react ? Vigorously or slowly ?
No NO2 fumes appearing ?
How concentrated is the HNO3 ?

According to the picture much vapor will leak out between the dish / watch glass and the rim of the beaker .

How did you get NH4NO3 ?

EDIT: It cn be done by any nitrate, but will result in red fuming HNO3 @normal pressure.

Look here:
http://en.wikipedia.org/wiki/HNO3#Laboratory_synthesis

[Edited on 2011-1-5 by metalresearcher]

plante1999 - 5-1-2011 at 12:45

only a verry small ammount of nitric acid escape.
when heated at 50-60 degree centigrate the reaction is slow and any NOx are evident(if it have some the gas will becaume brown because of the air acces bi the beaker rim.

I think it is at 70-95% purity.

I get my NH4NO3 from instan cold pack.

I will post a photo of the acid furter.

[Edited on 5-1-2011 by plante1999]

[Edited on 5-1-2011 by plante1999]

plante1999 - 5-1-2011 at 13:00

the nitric acid chiled at 0 degree centigrade.




sorry for the bad cality picture take by a 3 boxe camera....

Mixell - 5-1-2011 at 13:54

If its white fuming nitric acid as you claim (if excess water wan't involved in the process) so it should be 97%+.
I have also made fuming nitric acid using a condenser, it is a bit yellowish, but I assume it is at least 95%+

hkparker - 5-1-2011 at 17:00

Nice product! But I would be extremely carful with ammonium nitrate. Ive done this synthesis many times and did a video on it, and many people said, I think it was on NurdRage's video too, that ammonium nitrate will decompose to ammonia and this can be very dangerous. could be what happened?

plante1999 - 6-1-2011 at 04:45

it is at 210-250 degree celciuc and i heat at 50-60 degree celciuc so....

hkparker - 6-1-2011 at 16:26

K I looked it up. According to some things I read in a NurdRage video ammonium nitrate will of course make nitric acid in situ with HCl but decomposes when distilling. Id imaging you can still get a product, but its better to use sodium or potassium nitrate. its easy to convert with sodium or potassium hydroxide.

starch - 6-1-2011 at 19:03

hmmmm i have ran this experiment a few times

never thought the nitric acid obtained was ne where near that strenghth, it was still quite reactive with copper

time to have another go this weekend i think :)

i got 50% h202 and some KNO3 to play with as well

hkparker - 6-1-2011 at 19:10

50% H2O2??:o from where?

And yea the nitric acid produced by frac. distillation of a nitrate with conc. H2SO4 is fuming (~96%, 20M), greater concentration then azeotropic distillation (70%, 15.6M)

starch - 6-1-2011 at 19:57

hkparker in australia 50% H2O2 is very OTC, ya just need to know where to look :)

hkparker - 6-1-2011 at 19:59

darn, people have gotten arrested in the states for buying large quantities of 12%-30% from hair stores, though I manages to get 35% online :)

plante1999 - 7-1-2011 at 09:47

I have tested 2 time my technic end each time it work , i will test it in 2 day.

Somniferrous - 20-1-2011 at 14:12

Quote: Originally posted by hkparker  
darn, people have gotten arrested in the states for buying large quantities of 12%-30% from hair stores, though I manages to get 35% online :)


Hi.

If you live in the US, there is a very convenient source of 12% and 27% H2O2 that is everywhere and easy to get with no problems at all. it's cheap too, about $15/gallon. Of course it is a commercial product with a specific use. But if I state it openly on the net that might change things. Email me and I will reveal it to you.

[edit: fixed formatting]

[Edited on 22-1-2011 by madscientist]

Steve_hi - 14-2-2011 at 07:15

Hope I'm posting in the right place. If not I'm sorry. I need to have some nitric acid for an experiment I will do in my book which I bought to learn chemistry. I have very little experience but I want to learn Chemistry for a hobby. Anyways I can buy a 4litre jug of nitric acid that is combined with phosphoric acid for 24$ and I thought I could buy it and maybe distill it to seperate it, like I did with ethanol and water. I can also buy a similar product for 34$ that lists the phosphoric acid first and then nitric acid.
Do chemical companys list the ingredients in order of quantity like the food Industry?
Do you think I can distill the acids to seperate them? or is there a better or easier way to do it. Its not just for the acid I want to do this but also the learning of how.
Thank you for any help.
Ps the acid mixture source is concrete etching from Rona hardware store

HHammerHeadD - 27-3-2011 at 04:59

thats a sign there is copper in the acid, too much nitrite and too much copper and looks like too much sulfuric...but its' your pet project. I just hate getting in over my ability. Makes Jack a Dull Day on oxygen while undergoing inhalation therapy with ISOPRIL

Edenite - 22-6-2011 at 19:10

This is probably an over-optimistic question, but I gotta ask:
Is there a way to make nitric acid (however weak) without using chems like HCL, or sulfuric acid? Maybe Weaker, yet easier to obtain acids, or something else that would enable the conversion from nitrate to nitric acid?

Mixell - 23-6-2011 at 00:39

Decomposition of metallic nitrates, for example Cu(NO3)2, they give off NO2 fumes that will be passed into hydrogen peroxide.
2NO2 + H2O2 --> 2HNO3.
Or just passed into water: 3NO2 + H2O--> 2HNO3 + NO.

Zelot - 23-6-2011 at 11:27

Would it be possible to distill nitric from a mixture of KNO3 and KHSO4?
KHSO4 is easily obtainable for pools to decrease pH. I have read that KHSO4 acts in solution like a mixture of H2SO4 and K2SO4, but I am not entirely sure if that is true or not.

redox - 23-6-2011 at 11:53

Quote: Originally posted by Zelot  
Would it be possible to distill nitric from a mixture of KNO3 and KHSO4?
KHSO4 is easily obtainable for pools to decrease pH. I have read that KHSO4 acts in solution like a mixture of H2SO4 and K2SO4, but I am not entirely sure if that is true or not.


Yes this is possible, I have done it myself.

KHSO4 + KNO3 = K2SO4 + HNO3

entropy51 - 23-6-2011 at 12:31

Quote: Originally posted by Zelot  
Would it be possible to distill nitric from a mixture of KNO3 and KHSO4?
Yes, but it must be heated to a higher temperature than necessary when using H2SO4 and so some of the HNO3 will decompose. But it does work.