Nitric Acid by Kno3

[endotherm]

Can someone post a good procedure for synthesizing Nitric Acid using Potassium Nitrate as the nitrate source?

<small>[ June 05, 2002, 05:26 PM: Message edited by: endotherm ]</small>

[photonic]

PYRO500 wrote a very good, detailed pdf on this procedure.

It basically just says to mix 32G H2SO4(98% or >) and 68G of KNO3 then vacuum distill at about 90C. If your HNO3 isn't pure enough, just add some H2SO4 and distill again. THe pdf is/was available on the ftp( which I no longer have access to :( ) but it has been down for a while. If you want it, i'll put up a server and let you d/l it.

[mongo blongo]

I don't think those weights are right. From the equation for this reaction you should end up with 101g of KNO3 and 98g H2SO4.So for the amount of KNO3 above (68g) you need 65g of H2SO4.Remember that the H2SO4 molecule only gives one H atom to the HNO3 molecule.
If you vacuum distill it you should heat it at a much lower temp than 90C. The whole point of using a vacuum is that it will boil at a lower temp so that there is less formation of NOx. I can't remember the right temp but it's something like 60C.

[Nitro]

Best Temperature is between 83- 85 C.With this Temp. there is not so much NOx in your nitric acid.Here is an very good german side with Destilling apparatures/methodes.
<a href="http://www.chemikalienlexikon.de/cheminfo/1248-lex.htm" target="_blank">http://www.chemikalienlexikon.de/cheminfo/1248-lex.htm</a>

"Was der Affe für den Menschen ist der Mensch für den Übermenschen"

[Celtick]

I uploaded a <a href="http://us.f1.yahoofs.com/users/241add87/bc/E%26W/Synthese+Rood+Rokend+Salpeterzuur.pdf?bcLb9_8ALEL9 KFsz" target="_blank">PDF</a> with the Fuming Nitric Acid synthesis converted from <a href="http://www.pyrolabs.cjb.net/" target="_blank">Pyrolabs</a> witch appears to be offline for a while now.
(It’s a Dutch article)

[megalomania]

I had a wonderful source with pictures, equations, and whatnot, but I will be damned if I can find it. There isn't much to it really, but it does help to have exact information to be specific. I do however have some related safety information that I think is relevant to this. Here is a reprint of a discussion about distilling with sulfuric acid and a nitrate:

A retort is not strictly necessary. The best thing to use is a pyrex
distillation rig with ground glass joints. The main thing is that you
cannot use rubber, as the hot nitric acid vapor will eat it.

I have made nitric acid using a pyrex boiling flask with a teflon stopper as the reaction vessel, and a 6' piece of .25" i.d. teflon tubing run into a separate flask sitting in an ice water bath as the condensor. I made the stopper by turning a piece of teflon rod down on a lathe. It might be possible to use rubber by wrapping it thoroughly in teflon plumbing tape to protect it, but I have not tried this. You will have to heat the mixture. You MUST use an oil bath for this. The oil bath eliminates hot spots, and reduces the tendency to "bump". Vegetable oil is ok, and it's cheap. Mineral oil is better. Don't try motor oil, it stinks like hell when you heat it. I tried this once using an electric hot plate without an oil bath, and had a liter of boiling hot sulfuric acid/sodium nitrate slurry shoot out of the flask in a single solid stream, right in front of my face, spray all over the ceiling, and drip down on my head. I was lucky not to be blinded or killed. You must also be able to control the heat precisely. I use a variac. If you don't have acess to a fume hood, you can do this in front of a window with a fan. The vapors are intensly poisonous, and some of the oxides of nitrogen which are formed will not be stopped by the condensor.

When I did this reaction using concentrated sulfuric acid obtained by
boiling down battery acid and sodium nitrate from the local feed and
seed, I did not observe any undue heating when the components were
initially mixed. It might behave differently with KNO3, though I
would tend to doubt it. The nitrate was in form of "prills", little
balls slightly smaller than BB's. The prills did not begin to dissolve
until after the mixture had been boiling for a good five minutes. A
more finely divided nitrate might behave differently. It took a fair
amount of time after the boiling started for the acid to start coming
over, which tells me that you have to drive the reaction pretty hard
in order to get the nitric acid form in the first place. The first thing you get is a bunch of dark brown vapor, but it turns clear once the acid starts distilling over. For the benefit of those who may have missed the beginning of this thread, I want to stress again the importance of using an oil bath to heat the distilling flask. This stuff tends to bump violently, to the extent that it can shatter the flask or spray the the boiling acid/nitrate slurry all over the room. The temperature needs to be brought up slowly, over the period of an hour, because there is a substantial lag between the the temperature that the oil reaches and the temperature in the flask. You don't want to overheat it, and it's a good idea not to fill the distilling flask more than one third full as the goo tends to foam up a lot. This really is a dangerous procedure, but with good equipment and a great deal of caution it can be performed sucessfully. I would also recommend only doing small batches, especially at first.

[photonic]

Hey, I would like to set up a distillation apparatus for making HNO3 from KNO3/H2S04. I don't want to pay for glassware so I was searching for teflon tubing. I couldn't find a local supplier of it but I did find one that will sell me 50ft of some flexible plastic tubing called "Nalgene." They say it is very chemically resitant and will handle temperatures up to 550F. Do you think this would be suitable for distilling nitric acid?

EDIT: Further searching revealed that Nalgene is PTFE which is the chemical name for Teflon. So, I'm assuming this ought to work?

<small>[ June 08, 2002, 02:56 AM: Message edited by: photonic ]</small>

[Flake2m]

Nalgene would handle the Nitric acid without any problems. The only substances that PTFE are not chemically resisant to are very hot flourine and very hot sodium.
Glassware is expensive, and where I live (Australia) if you by anything other than beaker and/or test tubes, the pigs will think you are setting up a drug lab.

Has anyone tried my method of making nitric acid by decomposing xNO3 and then bubbling the NO2 gas though water?

[vulture]

I once tried making a little bit of HNO3 with H2SO4 and NH4NO3 in a testtube. Although it was not finely divided, I had to abandon my lab because of the insane formation of HNO3 vapor. The sulfuric was &gt;90%.

[Demolition]

Flake2m - Have you found a source of Nalgene (Teflon) tubing in Australia?I've looked around and so far cant find anything. :(

Also is Aluminum tubing HNO3 resistant?IIRC there was a topic a little while back on making HNO3 and I *think* a member stated that Aluminum tubing was HNO3 resistant however im not to sure.

[Demolition]

I found it,my search button wasnt working before. :o

Originally posted by Microtek.
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">Did you know that aluminium is compatible with nitric acid ?
My destillation setup is made with Al tubing and foil and the only effect on the Al is that it forms a thin oxide layer ( and on most tubing this has already occurred).</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Originally posted by 10fingers.
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica">Aluminum is impervious to nitric acid at lower temperatures. I once tried to make a distillation condenser out of aluminum but the warm nitric acid vapors started to react with it.</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Both quotes came from the topic 'HNO3 by desiccation' September 18 2001.
I guess my memory isnt as bad as what I thought it was. :)

[Mick]

what aboout nylon and HNO3?
like nylon fuel hose?

maybe its a dumb question, but its easy to get...so it might pay off..

or PVC pipe (or ABS pipe)

i honestly don't have a clue about HNO3, cause i've never made it before(no KN03 :( )

[photonic]

I'm pretty sure that the nitric would eat 'both' of those. Also, i guess it's possible that it would react with the pvc and give unwanted effects, but I have no chemistry background.

[rikkitikkitavi]

only plastics surviving contact with 68+ % HNO3 is teflone types.

there is something called PVDF (polyvinyledifluoride, similar to PVC, polyvinylechloride) that is partially resistant, but only shortterm,

Nylon, PVC e t c are all goners.

Stainless steel (316) is resistant to HNO3 at up to ~90% , Al is resistant to 100 %, but it has to be pure Al, not Dural or alloys with copper, zinc e t c since these metalls causes electrochemical corrosion.
The high oxidation potential of HNO3 increases the passivation process where the surface gets covered with a thin layer of
Al2O3 or Cr2O3(stainless)

But neither cant be used in the reaction vessel , where H2SO4 is present. This causes the metal to corrode very fast.

/rickard

[vulture]

When vacuum distilling, does the material of the hose which concects the vacuum outlet with the vacuum aspirator have to be HNO3 resistant or do only NOx escape that way?

And can I use the water stream which comes out of the condenser to run the vacuum aspirator or will the pressure be too low using a Liebich cooler?

[mongo blongo]

I have found that Polypropylene resists HNO3 very well. I use polypropylene bottles to store my HNO3.

[vulture]

Seems like PTFE is the only plastic that is 100% nitric acid resistant :( Shame because it's rather expensive for tubing.
Even PP degrades after some time in contact with 100% HNO3.

[VX]

Glass tubing is OK though, and can be found at some hobby shops. It's usually soda glass too so it can be softened with heat and bent into the desired shape. :)

[megalomania]

I find the pressure drop (of the vacuum) to be unnaceptable when I use my aspirator for both vacuum and coolent water for a condenser. Once the water backflowed into my flask :mad: Since I have mine set up for a garden hose connection, you can get a Y adapter for the hose. You can then get a plastic or metal hose thread to tubing bung adapter for the condenser. Alternately you can get various pipe thread fittings to do this, the same adapters can be found for the standard faucet (kitchen type) thread if you wish to use that. Then there are all the connection adapters to go from garden, to pipe, to faucet threads. I usually spend an hour at a time looking at all the goodies at Home Depot.

<small>[ June 19, 2002, 09:28 PM: Message edited by: megalomania ]</small>

[PYRO500]

I managed to build a water aspirator recirculating station out of a spa turbing pump some pvc and a water aspirator I got from
sigma-aldrich it works fairly well I use PE tubing (for water transport to refridgerators and other low flow jobs it seems at least NO2 and heat resistant not like vinyl tubing witch I used to use to connect the small tubing to my vacuum adapter and soon turned to yellow stickey goo. I get around 20 torr with my setup until the water temp rises witch I can prevent by adding a hose into the tank (10 gallons) and letting the cleanout plug loose to let a little water bleed out but it'sdifficult to get a good balance of water addition so I normally just let it run at room temp.

[vulture]

Okay, I distilled some nitric today, but the stuff has a funky green color and smokes like hell, even at 10C! <img border="0" title="" alt="[Eek!]" src="eek.gif" /> What has happened here? It was made by drain opener H2SO4 &gt;95% and NH4NO3.

I managed to connect the vacuum aspirator to the condenser flow and it still pulled a reasonable vacuum, when I accidently ripped out the tubing I heard a very loud fwwwooooossh and the boiling flask shot off the setup.

[kingspaz]

think the green colour is caused by HNO2 contamination.

[vulture]

Hmm, could be. Is that a sign it's highly concentrated or the contrary?

Oh, btw, I just found out that my 1l of 70% HNO3 from Fisher scientific is stored in a brown HDPE (High Density PolyEthylene)bottle.

I recommend everyone who plans on vacuum distilling to buy an aspirator with anti-kickback valve. Then you can simply turn down the water pressure when you have got the desired vac and no water gets into your setup.

<small>[ July 05, 2002, 05:46 PM: Message edited by: vulture ]</small>

[kingspaz]

HNO2 is an impurity and a sign of decomposition.

[PYRO500]

I had green HNO3 once it was one of my first vacuum distilations. it could be that beacuse my vac. was not high enough I had a small amout of NOx gasses in the flask, it also could have been I heated the acid too strongly. As far as Water aspirators go keep a long length of tubing between the aspirator and your setup. that will avoid most of the water siphoning problems that occur when the water pressure is reduced. I happen to have a PE water aspirator that has a kickback valve but when it wasw hoooked to my water supply the thing would allow water to be sucked into my flask when the water was on regardless of the fact that it was supposed to stop that. I found that it works ok to stop an abrupt change in pressure but for small changes such as your well running low on pressure the valve may not firmly seat and will leak waer into your system. I now use a 15 foot length of PE tubing run along the roof of my lab to not only extend the distance from the pump but also it works wonders at making reverse flow evident ad stoppable before it does damage. I'd recomend a pfte stopcock easily accessable near the end of the vacuum line to avoid accidents just remember that if you shut of the path of exiting gasses and you are heating a liquid and creating a much less dense gas that you are going to have the presssure increase untill catastrophe when the ground glass joints force each other apart possibly damaging your glassware.

[Flake2m]

the green colour is an impurity from the distillation process. I think it is N2O3. If you HNO3 starts turning yellow add a small amount of urea, it will remove the HNO2 from the acid.

[vulture]

Well, after a day in cold water (10C) the green color changed to very faint yellow.

[shrek]

Well my synth went a little better... but only to an extent. I made a page explaining what I did at:

<a href="http://www.ogreswamp.net/explosives/nitric1.html" target="_blank">http://www.ogreswamp.net/explosives/nitric1.html</a>

[DBSP]

Sounds like the anarchist cookboook or some other crap. And I really hate meassuring things that recuire weighting by volume.

[nbk2000]

Well I'm certainly impressed.

Someone actually tried the BB method and took pictures of it. And it does work, if you're careful (and the gods are smiling on you :D ) so the bottles don't crack.

Next time, try using teflon tape instead of cloth. Al;so, poke a small hole throgh the tape with a large sewing needle so there's a pressure relief so the gases don't blow out the tape.

Next, have a continuous flow of cold water running over the collection bottle, rather than occasionally cooling it. The (probable) reason your bottle cracked was because it got hot from the gases, and when you poured cold water over, it stressed the glass and broke it.

Finally, you may want to have the acid/nitrate bottle sitting in a slightly largere soup can filled with DRY sand. I can just see the hot nitric paste splattering on you when the bottle shatters.

[kingspaz]

i'm quite surprised it worked! its good when people actually write up their stuff and have pictures and things.
another point to note though, when heating the H2SO4 bottle try and do it very slowly to minimise the risk of a fracture.
trust me i've spilt concentrated 120*C H2SO4 on a burning stove before. made an instant cloud of H2SO4!

[shrek]

Thanks for the tips for next time. For teflon the pipe tape should work right? It is not very wide, but I'll just wrap it around a lot of times. I'll give it another go, hopefully later this week but first I got to go buy some more of that Pina colada concentrate for the bottles, have a little more time setting up, and wait till the parents aren't home. (They don't mind low explosives and stuff like ANNM or ANFO, they just hate me synthesizing things.)

shrek

[nbk2000]

Teflon is teflon. As long as it's wrapped tightly and thickly, it'll work fine. I used it for holding together flask and condenser for refluxing when the clips holding the equipment together litterally dissolved!

[Richy]

when concentrating the nitric, how much sulphuric should one add? also, what temperature for concentrating, and whats the concentration of the H2SO4 in car battery acid?

<small>[ October 13, 2002, 01:35 AM: Message edited by: Richy ]</small>

[vulture]

The amount of sulfuric depends on the amount of water in your HNO₃. Calculate the MASS of water that's in it by measuring density, concentration or pH (quite unreliable unless you got an electronical pH meter). Then calculate how many moles of water that are.
If you know that 98% H₂SO₄ binds water like this:
H₂SO₄.H₂O
then you should be able to calculate the stoichiometric amount of H₂SO₄ needed.
That is, if your H₂SO₄ is 98%.

The distilling temperature shouldn't exceed 60C. That means vacuum, because nitric boils at 80C at 1 atm.

Car battery acid usually is 37%. It takes quite some time to boil that down. Get drain opener acid.

<small>[ October 13, 2002, 06:07 AM: Message edited by: vulture ]</small>

[rikkitikkitavi]

in addition to vultures post:

the water-binding properties of the sulfuric acid decreases rapidly below 75-80 % so the calculation for how much sulfuric acid is needed has to take this in account , otherwise some water will also distill off with the nitric acid and dilute it.

/rickard

[Marvin]

The nitric acid is bound to sulphuric in a very similar way to water, which is why you need a higher temperature to liberate it. You can use both acidic hydrogens on sulphuric acid, but this requires a higher temperature. Industrially, when this was done industrially, it was prefered to leave quite a high percentage of bisulphate as product rather than go all the way to sulphate becuase the molten bisulphate/sulphate mixture could be poured out of the still.

A tip from somewhere, and I forget where, is to only heat the glass in contact with the liquid, which results in less decomposition. As an interesting (In my opinion) and apropriate (also in my opinion) sidenote, during the war when germany only had a weak nitric acid process, in the time before they built a concentrating plant, they reacted the weak nitric acid with sodium carbonate and evaporated, and then distilled this with conc sulphuric to generate the acid to make explosives.

[PhRaZMAkInEtIcS]

Actually my chem books say that the boiling point is 86 C.And i also remember reading in some chemistry book that Fe(ferrum sp?) also forms an oxyde layer(passivates -don't know if that's the word in english ,sorry)when exposed to concentrated nitric acid ,but it dissolves in unconcentrated HNO3.

Isn't aluminium supposed to be totaly nitrique acid resistant even at high temperatures(it should form a oxyde layer to protect it.)

I think some metals are deliberately processed with concentrated HNO3 to increase there corosion resistance.

May someone answer the folowing question becouse i am not so good in chemistry:

I have this equation about producing HNO2:
NO2 +H20=HNO2+HNO3
And this one about producing HNO3
NO2+H2O -&gt;HNO3+NO
........&lt;-
when bubling NO2 throught water which of the above equations would take place?

[knowledgehungry]

Correct me if i'm wrong. Pure aluminum is resistant to HNO₃ but aluminum often already has a layer of aluminum oxide on it which reacts with the nitric.

<small>[ October 26, 2002, 09:41 AM: Message edited by: knowledgehungry ]</small>

[CyclonitePyro]

I think you got it backwards. My understanding it that the nitric acid will oxidize the aluminum into aluminum oxide, so if the aluminum already has been oxidized by air, then the nitric acid can't do any further damage.

<small>[ October 27, 2002, 01:54 AM: Message edited by: CyclonitePyro ]</small>

[PhRaZMAkInEtIcS]

Boiling metals in HCl,treatating them with atomic hydrogen or when used as a catode.These are some of the metods used for removing the oxyde layer.Also i think you can scrape it off.But really where are going to get pure aluminium tubing.I think glass is the cheapest

[vulture]

The aluminium needs to be atleast 99.8% pure to resist nitric acid, because other impurities will cause an electrochemical minicell to form and the corrosion process will continue by itself then.

[kingspaz]

and also to be resistent the nitric has to be above 90% (guesstimate) concentration. at lower concentration the acid is much more ionised and will react with the Al.

[NoltaiR]

I have tried the IM style on more than one occasion back in the day. I have found that the cracking of glass is not necessarily because of the instaneous change of temp from the water, but rather it depends on the type of glass used. Try to get a glass that is fairly heat resistant and not too large. The IM handbook suggests coke bottles which work rather well. Of coarse you can't make more than 25-50mL at a time because the depression is not much. If you are using larger bottles keep an eye on the thickness of the bottle, thicker glass will shatter from heat easier (that is why lab glassware is thin). Also do not keep a continuous flame, you need to regulate it. An easy way to do this is to get one of those thin 'thermometers' made for aquariums. You can stick it on the inside of the neck of the bottle to be heated. Also I only used a 'pan of fire' (also suggested by the IMH) in a few labs before abandoning the idea; I decided it was easier to take a oxygen/acetylene torch (for welding) and turned it on a gentle steady flame--basically I just cut of the oxygen although that meant I had to put up with all the smoke that un-oxidized acetylene puts off.

I never used cloth (although that is the suggested idea), but rather I made an improvised tape made by taking a lentgth of duct tape an placing a metal strip (cut from a sheet of aluminum foil) down the center, so that only about 1/4" of duct tape is in the open on either side of the aluminum strip.

You seem to have yours balanced well enough (from what I can see) but I know that a big problem that I always faced was that if the lips of each bottle was not perfectly flush, then once the pressure built up the gas always blew (and then the lab is pretty much ruined unless you fill like trying to retape the bottles while the HNO3 gas is fuming out. Another idea (though I have never tried this) would be to put wieghts against the foot of each bottle so that there is less chance of the bottles separating.

As far as puncturing to release the gas, I have never done this but it may make your labs have a much higher chance of being successful. But I would not suggest just leaving a punctured hole open, rather just cover it up with another small peice of tape that you can occasionally remove and replace (for maybe a couple seconds) throughout the lab.

And lastly the cooling is a very important part (obviously) especially since the heated chamber is so close to the cooling chamber. If you are planning on using running water, make sure you have a place for the water to run-off. This may sound stupid but I can't tell you how many times the water would run collect into a puddle and makes the hole lab quite messy (which is especially true to the 'real' improvised chemist who is working outside on the ground). But the best way I have found to cool off the second bottle is to build a wooden (or similar) box that has a hole cut in the side of it just wide enough for the cooling bottle to set in. The box is partially filled with ice, then the bottle inserted, and then filled the rest of the way with ice. Once your HNO3 is fuming well inside the bottles, gently pour water into the box to make it cool even quicker.

When the lab is done, separate and close off the bottles as fast as possible (this is just basic lab safety so you don't have any unnecessary HNO3 fumes floating around). And as far as storage goes, I just like to keep it in the freezer.. that way it didn't fume when I opened the bottle.

The product always had some impurities (you can see specks floating around near the top and settling on the bottom of the HNO3). I tried to redistill it in a couple labs but decided it was far to time consuming for my uses (I have only used my improvised HNO3 for making nitrocellulose in the past, and it worked well enough).

[NoltaiR]

You will have to cut and paste the pics on this page.. and sorry about the bad quality, this whole lab was done in a bit of a hurry.

Well it has been about 5 months since I have done this lab so I decided I would have a go at it today.

Materials (that I used):
*80mL KNO3 (finely powdered)
*40mL 94% drain cleaner H2SO4
*2 Snapple bottles
*2 cloths
*duct tape
*gallon bucket
*vice
*2 100mL graduated cylinders (I know this is supposed to be an improvised lab, but using good measurements is always a key)
*oxygen/acetylene torch (oxygen turned off)
*ice
*water

Here are my materials
<a href="http://www.geocities.com/noltair/start.jpg" target="_blank">www.geocities.com/noltair/start.jpg</a>

Procedure:
A hole is cut into the gallon bucket for one of the Snapple bottles to fit into. The bottle is inserted and ice is poured around it. The reason I chose to use Snapple bottles was because of the thinness of the glass (makes it much less likely to crack from temp change.. the problem is that when using a bottle as large in diameter as this, water and ice isn't really cold enough to do the job.. this is my first mistake).

The KNO3 and H2SO4 is poured into the other bottle.. fuming will start almost immediately. Mix the two well with a stirring rod or similar (this is my second mistake.. in my haste to complete this lab before my mom got home I forgot to mix the two.. this doesn't necessarily ruin the lab, but it makes the time required to distill much longer). The second bottle is placed in the vice.. I would have used a ringstand but my last one was taken from me about 3 months ago during my parents last lab raid.

The two bottles are lined up as close as possible and a cloth is wrapped around the lips of the bottles. Duct tape to follow. The cloth is best used because extra pressure created in the bottles will be allowed to slowly slip through the cloth, but not enough to have much of a loss.

Here is the setup:
<a href="http://www.geocities.com/noltair/setup.jpg" target="_blank">www.geocities.com/noltair/setup.jpg</a>

Here is the Snapple bottle in the bucket of ice.
<a href="http://www.geocities.com/noltair/cool.jpg" target="_blank">www.geocities.com/noltair/cool.jpg</a>

The torch is lit and the burning begins.
<a href="http://www.geocities.com/noltair/burn.jpg" target="_blank">www.geocities.com/noltair/burn.jpg</a>

Soon the heating bottle is filled with gas.
<a href="http://www.geocities.com/noltair/gas.jpg" target="_blank">www.geocities.com/noltair/gas.jpg</a>

This went on for about 20 minutes when my mom called and said that she was almost home. I had made only about a few mL (5mL at most) because I just couldn't keep the cooling bottle cold enough to condense the gas. The bottles were separated and disposed of. If I would have had more HNO3 I would have saved it, but because 5mL just isn't enough to save I decided to see if it was possible to pour the HNO3 into another bottle (this is an obvious 'no no' because the liquid was just barely cold enough to keep from being a gas as it was). As soon as the bottle was turned upside down, the liquid turned into a fumes as soon as it contacted air, and that was the end of that.

Reasons for error:
*A busen burner or other form of continuous flame should have been used (I used to have bunsen burner that I simply plugged the hose to the end of the acetylene torch for fuel)... the actylene torch just didn't cut it because I could not hold it there long enough... especially while the smoke was blowing all around me.

*A smaller bottle (with the same thickness of glass) should have been used and/or a colder form of coolent should have been used (such as dry ice).

*The two chemicals should have been stirred before heating.

<small>[ November 04, 2002, 06:46 PM: Message edited by: NoltaiR ]</small>

[knowledgehungry]

Ammonia nitrate(in water) will work nicely to cool the bottle down.
Speaking of Ammonia nitrate yesterday i decided to be curious and heated a mixture of AN and sulfuric. I heated it in a test tube with a rubber stopper. Dark orange fumes came out and attacked the rubber was that nitric acid? Thanks.

[Anthony]

It was NO2 - Nitrogen Dioxide

[kingspaz]

chemistry lesson:
H2SO4 + NH4NO3 ---&gt; HNO3 + NH4HSO4
4HNO3 ---&gt; 4NO2 + 2H2O + O2
NO2 is toxic shit so don't breathe it!

<small>[ November 06, 2002, 06:25 PM: Message edited by: kingspaz ]</small>