Sciencemadness Discussion Board - HNO3..

HNO3..

vlassen - 14-3-2011 at 14:05

Hello,

I just found this way of making nitric acid..

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t...

It looks like this

http://www.sciencemadness.org/talk/viewthread.php?tid=401

this method (1st link) seems to work quite well (and cheap)...

What do you think?

[Edited on 14-3-2011 by vlassen]

ScienceHideout - 14-3-2011 at 17:05

Quote: Originally posted by vlassen

Hello,

I just found this way of making nitric acid..

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t...

It looks like this

http://www.sciencemadness.org/talk/viewthread.php?tid=401

this method (1st link) seems to work quite well (and cheap)...

What do you think?

[Edited on 14-3-2011 by vlassen]

I have my own way of making HNO3. I adapted it from the 2nd part og the following NurdRage video. Even though it is not pure or concentrated, it works.

http://www.youtube.com/watch?v=2yE7v4wkuZU

vlassen - 15-3-2011 at 06:26

I tried this method and the yield was low IMO. Do you get a good yield with your process?

ScienceHideout - 15-3-2011 at 11:41

Quote: Originally posted by vlassen

I tried this method and the yield was low IMO. Do you get a good yield with your process?

I use peroxide like nurdrage, and I use lots of copper and heat it. I never titrated it, but as long as it eats copper it can serve most of my purposes.

Formatik - 15-3-2011 at 17:43

Quote: Originally posted by vlassen

...
What do you think?

It would be very impure. Despite that silver treatment, and though Ag2SO4 has slight solubility it is much more soluble than AgCl. Also, Ag2SO4 has increased solubility in acids, HNO3 enhances solubility. This can become a lethally problematic impurity if the acid was mixed with organics, and a detonating silver compound forms. The acid will also have some sodium contamination. Distillation is needed.

Another way to make it from NaHSO4 is by heating. NaHSO4 heated with KNO3 will drive off some nitric acid, or CuSO4.5H2O mixed KNO3 at modestly low heat (65 to 235 C) drive off HNO3 and NO2. The vapors can be captured in cool H2O (better is moderate H2O2 since it oxidizes nitrogen oxides). But I would always use H2SO4 and do the regular distillation. Besides good for sheer experimentation, I don't like roundabout methods.

plante1999 - 16-3-2011 at 03:29

you should chec the way i use , it is a the end of the page (yellow picture).

http://www.sciencemadness.org/talk/viewthread.php?tid=15211

vlassen - 16-3-2011 at 08:07

ScienceHideout, Formatik: Thank you for your help

plante1999: you say in your topic that you got ammonium nitrate from instant cold pack.. How? (In 2009, it was banned along with nitric acid, some nitrates/chlorates etc. I guess you know the "Explosive Act"..)

[Edited on 16-3-2011 by vlassen]

[Edited on 16-3-2011 by vlassen]

hissingnoise - 16-3-2011 at 09:14

Quote: Originally posted by Formatik

Besides good for sheer experimentation, I don't like roundabout methods.

And since said roundabouts produce nothing worth the effort they're mostly just a waste of time!

Bot0nist - 16-3-2011 at 10:25

Quote: Originally posted by vlassen

ScienceHideout, Formatik:

plante1999: you say in your topic that you got ammonium nitrate from instant cold pack.. How? (In 2009, it was banned along with nitric acid, some nitrates/chlorates etc.

I still get it in cold packs in the USA. Just bought some last Friday. Ingredients: Ammonium nitrate and water. Some have urea in them instead though. You have to watch out for that.

vlassen - 16-3-2011 at 12:21

Quote: Originally posted by Bot0nist

Quote: Originally posted by vlassen

ScienceHideout, Formatik:

plante1999: you say in your topic that you got ammonium nitrate from instant cold pack.. How? (In 2009, it was banned along with nitric acid, some nitrates/chlorates etc.

I still get it in cold packs in the USA. Just bought some last Friday. Ingredients: Ammonium nitrate and water. Some have urea in them instead though. You have to watch out for that.

But what about Canada? Especially Quebec.. That's what I can get there

http://www.formedica.com/en-ca/produits/premiers-soins/gel-p...

but it doesn't say anything about ingredients..

Bot0nist - 16-3-2011 at 12:37

I'm not sure about Canada. If the product is a 'gel' like it says then I doubt it would be useful. The ones I use are just a white bag filled with little beads (prills?) of NH4NO3 and a little brittle bag of water inside. The ingredients state only dihydrogen monoxide and ammonium nitrate. The NH4NO3 prills are very hygroscopic, so I pulverize them with a rolling pin, and then heat it between paper towels at 110F in the oven for 20 minutes. I then seal immediately in a water tight container.

vlassen - 16-3-2011 at 12:55

It's not a gel, it's exactly like your white bag (white beads and a bag of water). But, I fear that it might be urea.

Bot0nist - 16-3-2011 at 13:08

Some simple tests could determine if its urea I imagine. Is it pure white? Does it smell of ammonia when heated?

plante1999 - 16-3-2011 at 13:16

in live in qc and you could get easily ammonium nitrate cold pack

vlassen - 16-3-2011 at 13:46

Quote: Originally posted by Bot0nist

Some simple tests could determine if its urea I imagine. Is it pure white? Does it smell of ammonia when heated?

Yeah it's white.. I have never heated it, but it stinks anyway*. I'll try to determine the solubility, I think it might be a good way to determine if it's ammonium nitrate or urea (or anything else)

*In fact, I think the smell comes from the bottle..

plante1999: which brand?

[Edited on 16-3-2011 by vlassen]

cyanureeves - 16-3-2011 at 14:07

urea also smell of ammonia.walmart has a prilled cold pack that says non-toxic and its urea.50/50 prills and baking soda boiled should get you sodium nitrate,you can then evaporate and mix with sugar(a la nurd rage)and burn it or just make gun powder if its ammonium nitrate prills. i got an oldie cold pack and the water pack has a green liquid and the powder looks like baking soda.never seen this before.

vlassen - 16-3-2011 at 14:32

So if I mix a solution of ammonium nitrate and sodium bicarbonate it should make bubbles.. I'll try that

vlassen - 16-3-2011 at 15:03

It didn't work, I didn't see any bubbles.

Bot0nist - 16-3-2011 at 15:14

I meant the Urea smells like HN4 not the AN. I don't know if the 'bubble' test will work. Its not an acid. Does the metathesis create CO2 or something?

If it smells like HN4 its urea IIRC.

vlassen - 16-3-2011 at 15:36

Quote: Originally posted by Bot0nist

I meant the Urea smells like HN4 not the AN. I don't know if the 'bubble' test will work. Its not an acid. Does the metathesis create CO2 or something?

If it smells like HN4 its urea IIRC.

It's not an acid, but:

NH4NO3 + NaHCO3 -> NH3 + CO2 + H2O + NaNO3

bbartlog - 16-3-2011 at 17:07

Why wouldn't you get ammonium bicarbonate if this reaction were conducted at room temperature, i.e.
NH4NO3 + NaHCO3 -> NH4HCO3 + NaNO3 ?
Granted ammonium bicarbonate is itself pretty unstable and would easily decompose (even if it formed) to the products you list, but I'm not sure it just happens right away.

cyanureeves - 16-3-2011 at 17:45

bubbles? you mean because baking soda fizzes in water?i never paid no mind to the bubbling, but ammonium nitrate and sodium bicarbonate make a bunch of ammonia when boiling. take advantage of the ammonia.just dry your yield and add sugar then burn it.

vlassen - 16-3-2011 at 17:55

bbartlog: what do you mean? If 2 gases and water are produced, then I think it's spontaneous

cyanureeves: well I thought that if it produces NH3 (gas), then I would see bubbles or something like that o.0.. I'll try to boil it then.

Formatik - 16-3-2011 at 18:39

Urea boiled with bicarbonate will also form NH3. I would mix conc. aq. NaOH with the suspected NH4+ salt, if it gives off NH3 at room temperature, then it's NH4+.

Quote: Originally posted by hissingnoise

And since said roundabouts produce nothing worth the effort they're mostly just a waste of time!

Mostly true. But reagents may be harder to get in some areas, and increased restrictions can make one or the other harder to obtain. The versatility is good.

[Edited on 17-3-2011 by Formatik]

Bot0nist - 16-3-2011 at 18:41

Now there's an idea...

Still, this will only tell you if it contians an NH4_, not if its contaminated with urea i suppose.

[Edited on 17-3-2011 by Bot0nist]

[Edited on 17-3-2011 by Bot0nist]

Formatik - 16-3-2011 at 18:47

Quote: Originally posted by Bot0nist

Now there's an idea...

Still, this will only tell you if it contians an NH4_, not if its contaminated with urea i suppose.

Right, but why would they mix NH4NO3 with urea? I just don't think that happens. Urea is intended as a replacement to the more hazardous substance.

Note: it looks like there are some cold packs that do have a mixture of the two, but do indicate it is a mixture: http://www.sciencemadness.org/talk/viewthread.php?tid=14525 This is rare, though, from all I've seen and heard of cold packs is that they are either one or the other.

[Edited on 17-3-2011 by Formatik]

Bot0nist - 16-3-2011 at 19:24

Your right. Sorry, I wasn't thinking

. It is most likely either, or.

hissingnoise - 17-3-2011 at 06:16

Why not just buy cheap, fertiliser-grade NaNO3 . . .

Bot0nist - 17-3-2011 at 07:12

I agree, if HNO3 distillation is the goal, then there are a ton of cheaper and easier to get nitrate salts out there. I just use cold packs when I really need some NH4NO3, as it can be hard to get thanks to McVeigh and pals.

It works better for my cellulose nitrate synthesis than any other nitrate salt I have used, which is why I'm often hunting for cheap first-aid kits.

[Edited on 17-3-2011 by Bot0nist]

hissingnoise - 17-3-2011 at 07:38

Quote:

It works better for my cellulose nitrate synthesis than any other nitrate salt I have used, which is why I'm often hunting for cheap first-aid kits.

NC by prolonged immersion in strong, mixed acid will make your improvised NC look tame by comparison.
So, if you have nitrate salts and H2SO4 you just need some glass?

Bot0nist - 17-3-2011 at 07:49

I know using nitric is better. I have an all glass distillation setup, and have tried making HNO3 with it. I had trouble condensing the acid, and a little leak caused me to get a nice taste of orange. Not fun indeed! I buy my nitric when I need it now, which is rarely.

I nitrate my cellulose twice in the nitrate salt/acid mix for 3 hours each time, and I agitate the mix constantly, which I think helps replenish the nitronium ions in the solution. I wouldn't call it tame. I have even had luck detonating it once, though I should make some with 70% HNO3 and compare it.

[Edited on 17-3-2011 by Bot0nist]

hissingnoise - 17-3-2011 at 08:08

I must be missing something here - you're afraid of a little NO2 leaking during distillation but the room-filling cloud of HNO3 vapour produced when NH4NO3 is mixed with H2SO4 doesn't seem to bother you . . . ?
WTF!

Bot0nist - 17-3-2011 at 09:05

First, I don't 'fill a room' with any harmful gasses.

When I add my AN to my sulfuric, I do it in a slow, controlled way and keep things cool. Gas production is pretty minimal, and a little ventilation doesn't hurt. When I was trying to distill HNO3, I falsely assumed that my setup was sealed and it was not. This resulted in me breathing in some gasses that made my life hell for a few days, so I really just don't have a desire to try and distill HNO3 any more. Not to mention I had trouble getting a yield anyway. ( probably because of the leak.)

It is not fear of toxic gasses that deter me, but the general inconvenience makes it unnecessary for me to try and obtain HNO3 by any other means than paying absorbent prices for 70% bottles, given the limited amount of uses I have for it. I'm not saying making it is a bad idea that shouldn't be attempted, just that I prefer not to try it anymore. The NC I make works well for my uses and when I need HNO3, I simply pour some from the bottle.

I meant no offense or confusion to you. I apologize if it seemed otherwise.

[Edited on 17-3-2011 by Bot0nist]

hissingnoise - 17-3-2011 at 12:47

I'm just puzzled BotOnist - almost to the point of wondering if we're talking about the same procedures . . .

Bot0nist - 17-3-2011 at 13:20

The only procedures I was talking about were the distillation of HNO3 from a nitrate salt and H2SO4, and the nitration of cellulose using a nitrate salt and H2SO4. If you would care to be more clear on the cause of your puzzlement, than maybe I can further clarify myself to you.

hissingnoise - 17-3-2011 at 13:31

Well, I find the distillation of HNO3 to be problem-free essentially and the use of nitrate salts with H2SO4 to be unappealing because nitric acid mist is produced however carefully the reactants are mixed . . .

Bot0nist - 17-3-2011 at 13:48

I see. I am glad that you have had an easy time in distilling HNO3. I, however, did not. I have no doubt that all of my problems with that synthesis were the direct result of my own ignorance/negligence, and I do not discourage anyone from attempting to run that synthesis, as long as they take proper precautions, as it seams to be a really useful and fun procedure.

When I make my nitrating solution carefully I have never noticed any large amount of HNO3 mist. The mixture fumes slightly orange as the NH4NO3 is added, and then more so when it is agitated. Working with cool acid and really dry NH<sub.4NO3 seams to reduce the amount of fumes that I observe. The only time I had serious problems with the fumes was when I dumped 31g of AN into 55ml of warm sulfuric all at once. This did produce a very large cloud of fumes.

I just happen to find the distillation of boiling acids more unappealing than the creation of an 'improvised' nitrating solution. To each there own, I suppose.

Also, wouldn't the distillation of nitric acid we were discussing require adding nitrate salts to sulfuric?

[Edited on 17-3-2011 by Bot0nist]