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menchaca
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HNO3????
i dont know what i did when i was child or how i did it but this is what happened to me:
i took a large bottle and i added quantity of ammonia and a large quantity of comercial H2O2(3%) suddenly it´s colour turned red and white fumes
appeard in the mouth of the bottle. Could that generate nitric acid? i dont know what to to think because nitric acid isnt easy to obtain oxidying
ammnia but this was what happened to me and.........
well that´s all, i hope somebody can help me
thanks again!
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DeusExMachina
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no, that's not the way it works. You make HNO3 from ammonia with electrolisys. With platinum wires that is. I made a topic on this (I think it
was me  )
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menchaca
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can you tell mi more about this?
about production of HNO3 electroliticly i mean......
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Darkfire
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H2SO4 + (X) NO3 = HNO3 + ....
You will need to distill of the nitric acid under low temps to avoid decomposition.
CTR
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DeusExMachina
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there has been a topic on this I have been told it is nearly impossible to do this with a home lab.
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Darkfire
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No way, its not hard at all with even a basic lab.
CTR
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Rhadon
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DeusExMachina: If you are referring to what I said in another topic: I was talking about the oxidation of ammonia back then (which I
do now think should be possible to do at home as well, after BASF gave me details about the process to convince me  ). What Darkfire is talking about will be possible to do at home, although a
considerable amount of the HNO3 will decompose if you distil at atmospheric pressure. I'd suggest extracting the HNO3 with CH2Cl2 instead and
avaporating the latter (b.p. of CH2Cl2 is only about 40 °C), that should be possible to do with hardly any decomposition of the HNO3. This method has
already been covered well, at least in an older thread on the E&W forum. You might check this out when it's back up. There is also a patent
about this process which should be worth reading. It's on the FTP in Xoo's Folder.
[Edited on 1-4-2003 by Rhadon]
[Edited on 1-4-2003 by Rhadon]
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menchaca
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will electrolitic oxidation of NH3 only posible with platinum electrodes? if other materials can be used what materials?
thanks again!
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Cappy
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My guess is that platinum is used because it is not very reactive with HNO3. Gold could probably be used, but still cost a lot. Aluminum could
probably be used, but would lose more energy as heat (higher resistivity).
I'm not positive. Could someone confirm or deny this?
[Edited on 4/3/2003 by Cappy]
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Theoretic
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An answer on the original question: H2O2 reacts with ammonia to give NH4NO2:
2NH3+3H2O2=>NH4NO2+4H2O.
The red probably was NOx evolved from a side reaction. The white...?
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Blind Angel
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NH4NO2, wouldn't this be usefull to form nitrite (Sodium Nitrite and all)
NaCl + NH<subb>4</sub>NO<sub>2</sub> -> NH<sub>4</sub>Cl + NaNO<sub>2</sub>
NaOH + NH<subb>4</sub>NO<sub>2</sub> -> NH<sub>4</sub>OH + NaNO<sub>2</sub>
?
Any of those reaction possible (yes i'm pretty tired)
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BASF
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NH4NO2? - Sounds too good to be true.
Anodical oxidation of NH3 ? This would be very cool. Maybe there is a patent on this?
BTW, platinum wire is not that expensive.
The bigger problem is that the electrodes have to have a big surface to get the desired current density.( if the current density is too high, only
tiny gas bubbles are generated)
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BASF
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I was once thinking of making my own platinum-coated electrodes by dissolving it in aqua regia, then just let it dispose on a less noble metal.
This is also a cool way of detecting noble metals: for example, you can take a coin of copper(has to be pre-cleaned, of course), then place a drop of
silver- quicksilver- or maybe also platinum- solution on it. After 5 mins or so, the coin turns silver.    
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Theoretic
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Getting nitrites via the chloride route is impossible, NH4NO2 decomposes at low temperatures (hot water). The alkali route seems all right to me,
don't see why it might not work.
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Mephisto
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The NH4NO2 decomposes at 20 °C. So maybe it’s possible to make it at 5 °C and get then the alkali nitrites by mixing with other alkali salts
(like Blind Angel said).
[Edited on 3-10-2003 by Mephisto]
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Theoretic
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So, anyway, I think the white fumes were fumes of H2O2/concentrated NH3 solution/whatever - the heat of reaction is supposed to be considerable.
Now, THAT helped, didn't it?
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Blind Angel
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If the heat of the reation was considerable then NH<sub>4</sub>NO<sub>2</sub> would decompose instantly...
By cooling we would be able to get some NH<sub>4</sub>NO<sub>2</sub> in H<sub>2</sub>O<sub>2</sub> and
water (considering that Peroxyde was used in excess to oxyde all the NH<sub>3</sub> then you could catalyst the H<sub>2</sub>O<sub>2</sub> decomposition in water with Zn, Mg or another metal which
you would be able to filter off to get a solution of Water and NH<sub>4</sub>NO<sub>2</sub> add NaOH and you got
NH<sub>4</sub>OH and NaNO<sub>2</sub> solution. NaNO<sub>2</sub> melt a 271ºC so you can boil off the water,
NH<sub>4</sub>OH will simply decompose into NH<sub>3</sub> and water at high temp. Sodium Nitrite from Household ammonia and
Hydrogen Peroxyde, someone to try it (my peroxyde stock is a bit low lol ) ?
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Mephisto
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It´s worth trying
Unfortunately I haven’t enough time for more exact tests with bigger amounts, now. But I tried to do this just with some millilitres, some months
ago. I’ve add 27.3 g (0.2 mol) of ice-cold NH3 (25%) to 68 g (0.3 mol) ice-cold H<sub>2</sub>O<sub>2</sub> (30%). Both
liquids had a temperature of -8 °C. During the mixing, there wasn’t any fume-evoltution or rising of temperature noticeable. Then I added 8 g NaOH
in ~30 ml distilled water and heated the whole mixture for 45 minutes at 60 °C with continuously magnetic stirring. A lot of bubbles evolved and
NH<sub>3</sub>-smell was noticeable, but no nitrous fumes have been formed.
To test the presence of NO<sub>2</sub><sup>-</sup> or NO<sub>3</sub><sup>-</sup> I added a mixture of
sulfanilacid and alpha-naphthylamine (in German “Lunges Reagenz”). The test was positive. But it is very very sensitive, so maybe just some
milligrams of NaNO<sub>2</sub> have formed. I don’t know. I let the liquid dry, but never tested the residue.
But even if this give only bad yields, it could be possible to synthesise a nitrite, by passing nitrous fumes from
H<sub>2</sub>O<sub>2</sub> and NH<sub>3</sub> (see first post) through a NaOH solution.
… start on research
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Theoretic
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Hmm... The reaction of H2O2 and ammonia can lead to different outcomes, depending on the stochiometry. The main reaction that probably happened at
such low temperatures was the formation of HYDRAZINE! The hydrazine could probably go to hydrazoic acid if there was enough H2O2 present. If there was
more H2O2 and more vigorous reaction conditions, nitrogen could have been evolved. And of course, yet more H2O2 yields nitrite and nitrate. Just like
chlorine, going in order from smaller to bigger amounts of chlorine in the stochiometry, the products of its reaction with ammonia are:
Hydrazine
Chloramine
Nitrogen
Dichloramine
Nitrogen trichloride.
Going back to NH3/H2O2... More vigorous reaction conditions are required, in my opinion.
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Acid Test
fruitcake
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Hydrazine From Peroxides?
Hydrazine from ammonia and H2O2.It sounds to good to be true!!!
The formula would have to be
2NH3 + H2O2
That is two parts ammonia to one part of hydrogen peroxide.Hydrazine requires 2 Nitrogen and four hydrogen.The extreme reactions are caused by the
excess hydrogen and oxygen being released from the reaction
.....
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Theoretic
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Hmmm...
Mephisto: how do you expect nitrous fumes (acidic) evolve after you've added strong alkali? Hydrochloric acid might be a better test. I even
think that ammonium chloride could be used, so as to remove nitrous fumes from the reaction zone as soon as formed
[Edited on 9-1-2004 by Theoretic]
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Acid Test
fruitcake
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Actually in the presence of a ketone you
would probably get indole.This of course
will set the way for psychedelic chemistry.
Indole is the main component to all
tryptamines including 5-MT(serotonin)
I have always wanted to try to synthesis
5-MT and take a dose of it
.....
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Levi
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I wonder whether or not nitrogen trichloride and peroxide will form nitric acid. Working with NCl<sub>3</sub> isn't a good idea on a
large scale, but if it works it would be a tempting route to nitrates. I don't have a fume hood so I won't be trying this, has anyone else been brave
(read: stupid) enough?
Assuming this method works, are the following equations correct?
NH<sub>3</sub> (aq) + 3HCl (aq) --> NCl<sub>3</sub> + 3H<sub>2</sub>
2NCl<sub>3</sub> + 5H<sub>2</sub>O<sub>2</sub> --> + 2HNO<sub>3</sub> + 3Cl<sub>2</sub>
(g) + 4H<sub>2</sub>O
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The_Davster
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My only experiance involving NCl3 was accidental and mildly amusing...
The first reaction will not work, the following will happen.
NH3 +HCl -->NH4Cl
IIRC, NCl3 is prepared by bubbling chlorine into an ammonium nitrate solution, or electrolysis of ammonium chloride.
The second reaction I really could not say...
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Levi
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| Quote: | Originally posted by The_Davster
My only experiance involving NCl3 was accidental and mildly amusing...
The first reaction will not work, the following will happen.
NH3 +HCl -->NH4Cl
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Ah, thanks for pointing that out! NH<sub>4</sub>Cl in a solution of HCl in excess should form NCl<sub>3</sub> when NaOCl is
added. Without the bleach nothing happens.
I guess what the question boils down to is will hydrogen peroxide oxidize nitrogen trichloride from +3 to +5?
[Edited on 24-4-2007 by Levi]
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