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Haggis
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Deusexmachine- my reccomendation is that you bend the glass tubing. That way there is a less chance for the XNO3/H2SO4 to bubble while boiling and
splash in the receiving vessel. To do this, hold your glass tubing over an alcohol lamp. Hold the tube firmly on each side of the flame, protecting
your fingers with two handtowels. Hold the area to be bent over the flame and keep a firm but gentle pressure on the tube while heating. When the
glass softens, it will start to bend. Take it slightly off the flame and continue with the 90 degree bend. Then let the tubing cool naturally
(without dropping into cool water). Do the other side with the same method, taking care that they are perfectly level to eachother.
[Edited on 26-2-2003 by Haggis]
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PHILOU Zrealone
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I thought Al(NO3)3 is an explosive, easy hydrolysed salt?
If you can use Ru(NO3)2, then use Au(NO3)3 it's cheaper ;-)!Believe me, I have worked with Ruthenium chlorides!
 
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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PHILOU Zrealone
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As a parenthese: relative freeable oxygen by weight available to burn a fuel
HNO3 (63,5% bw)
LiNO3 (58%)
NaNO3 (47%)
KNO3 (39,56%)
Be(NO3)2 (60,1%)
Mg(NO3)2 (53,94%)
Ca(NO3)2 (48,75%)
Sr(NO3)2 (37,8%)
Ba(NO3)2 (30,6%)
Ti(NO3)4 (54%)
Cr(NO3)3 (50,4%)
Mn(NO3)4 (52,8%)
Mn(NO3)3 (49,8%)
Fe(NO3)3 (49,6%)
Al(NO3)3 (56,34%)
Or put by oxygen efficience:
HNO3 (63,5% bw)
Be(NO3)2 (60,1%)
LiNO3 (58%)
Al(NO3)3 (56,34%)
Ti(NO3)4 (54%)
Mg(NO3)2 (53,94%)
Mn(NO3)4 (52,8%)
Cr(NO3)3 (50,4%)
Mn(NO3)3 (49,8%)
Fe(NO3)3 (49,6%)
Ca(NO3)2 (48,75%)
NaNO3 (47%)
KNO3 (39,56%)
Sr(NO3)2 (37,8%)
Ba(NO3)2 (30,6%)
Al(NO3)3 is amongst the bests!
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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osamafon
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how fast is al picrate
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PHILOU Zrealone
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All picrates must have about the same VOD at an identical density (if it was what you asked?); the major difference are density and sensitivity!
PH Z (PHILOU Zrealone)
"Physic is all what never works; Chemistry is all what stinks and explodes!"-"Life that deadly disease, sexually transmitted."(W.Allen)
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Skean Dhu
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ok, i tried to make some HNO3 today, but the still didn't work.
i had a glass beverage bottle with about 50-70ml of H2SO4+KNO3 in a hot oil bath, and then for the tubing i had 3ft of Al tubing with a PB jar full
of ice saltwater (about 4" away from the bend)to condense the fumes. the tubing was bent at 50degrees, put through the bottle cap(it was a
resealable type) and then coated in many layers of teflon tape.
the still stood up to the heat and fumes fine however nothing but the occasional puff of NOx came out the end (which was about 4-6' lower than
the bottle)
is the tubing too long, at too steep of an incline or what,
aldo how do you post a picture(ie; paintbrush) i want to give a general schematic of what my still looks like
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Mendeleev
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Darkfire, I agree that brainfever's method is the best but why do you use such small quantity beakers? I use 20 L stainless steel stockpots and
get 2-4 L of nitric acid after several days distilling at 65 degrees Celsius, density 1.5 g/mL. Your way would give you about 100-150 mL that's
not even enough for a kilogram of nitroglycerin.
[Edited on 25-12-2003 by Mendeleev]
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hodges
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Another Idea
I was just thinking about this thread and have another idea for getting HNO3. I have not tried it, so don't know if it would work.
I seem to recall that HNO3 reacts with copper to form various oxides of nitrogen. Why not create a solution of HNO3 by adding H2SO4 to a nitrate.
Even though there will now be a sulfate salt in that solution, I would expect the HNO3 to still react with copper. So drop in some copper. Bubble
the NO2 produced into another flask with water, and you have HNO3.
Maybe I'm all screwed up, so don't take my word on this. But it seems like it would work.
Hodges
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Mendeleev
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The Copper process would be redundant. XNO3 + H2SO4 gives you XHSO4 + HNO3, so all you have left to do is distill, and no copper step. Plus the NO2
+ H2O would give you a lot of water in you HNO3 I think due to equilibrium issues, low concentration. Distilling from XNitrate gives you 90% to 100%
concentration depending on the sophistication of your methods. Industrially nitric acid is made by reacting NO2 with H2O and the concentration
achieved is about %50. The NO2 is gotten from the NO + O2 reaction, and the NO is gotten from the NH3 + O2 reaction.
[Edited on 7-1-2004 by Mendeleev]
[Edited on 7-1-2004 by Mendeleev]
[Edited on 7-1-2004 by Mendeleev]
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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axehandle
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Anyone know if 50% nitric acid concentration is the maximum obtainable by bubbling NO2 through water, or if it's just for economical reasons
(time) the industrial yield is only 50%?
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Mendeleev
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You can probably get higher concentrations using NO2 + H2O, but the reason they don't in the industry is that they recycle everything. The
process is three step.
4 NH3 + 5 O2 ---> 4 NO + 6 H2O
2 NO + O2 ---> 2 NO2
3NO2 +1 H2O ---> 2HNO3 + 1 NO
As you can see there is originally more water formed in the first reaction, and less water than NO2 used in the third reaction thus more is left over
which is why the concentration is only 50% by mass. They just heat up the tank after the second step is finished so that the water is a gas and
reacts with the NO2 gas more. This most likely requires a catalyst. I was actually wondering, since in the industry it is unlikely that they use
glass for 100,000 liter vats of nitric acid, what materials are there besides glass which are both heat resistanct and nitric acid resistant, and have
enough structural integrity to hold 100,000 liters?
[Edited on 7-2-2004 by Mendeleev]
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rikkitikkitavi
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stainless steel ...
above 95 % aluminium..
/rickard
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Mendeleev
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Are you sure stainless steel stands up to nitric acid? Aluminum is the least acid resistant metal I know, and what about sulfuric, can stainless
steel stand up to sulfuric acid? After all they distill the nitric acid using sulfuric to get high purity.
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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axehandle
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I recently researched suitable materials for nitric, so here is from the top of my head:
Aluminum forms a protective oxide layer on contact with nitric acid (which is a very strongly oxidizing acid), and is indeed a suitable replacement
for glass tubing if you're going to distill nitric acid and are building a condenser.
If the acid is hot though, it WILL eventually eat through.
Modern stainless steel can supposedly withstand nitric acid up to 70%, if memory serves me right.
Oh, and PVC also is resistant to nitric acid (any concentration) as long as it's not hot.
About stainless and sulfuric I'm not sure. I would construct the tank out of teflon or pvc coated stainless as they are both resistant.
This link may be of use, it's a chart of the resistances against a multitude of acids w.r.t. various plastics/polymers.
http://ptcl.chem.ox.ac.uk/MSDS/glovesbychemical.html
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Mendeleev
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Interesting, yet when nitric acid is distilled it is hot. Perhaps the insides of the tank have a glass coating? I was also wondering about titanium.
Trogdor was a man. A dragon man. Or maybe just a dragon. . .
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axehandle
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Porcelain enamel has had a great comeback in industry as protective coating. As I understand it, it can, using modern techniques, be applied to almost
any metal substrate.
I'm wondering if huge reactor vessels nowadays consist of cheap, mild steel with an also cheap porcelain enamel coating? It would make both
technological and economical sense... hmmmmm.
My PGP key, Fingerprint 5D96 E09E 365D 1867 2DF5 C2FE 4269 9C19 E079 CD35
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rikkitikkitavi
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PVC is NOT resistant to concentrated nitric acid. It is resitant to cold conc sulfuric acid < 40 C, and hydrocloric acid.
Stainless steel is not resistant to sulfuric or hydrocloric acid .
axehandle, sometimes they make reaction vessels like that. A few caveats though:
i plants, worker tend to use force and various tools in contact with the eqipment
(for example banging a sledge hammer at a silo ,when the product is stuck in the bottom, banging it broken that is...)
second, it is sometimes difficult to match the
temperature expansion of both materials.
But there is a few areas , fex in the pharmacutical industry where the clean surfaces of enameld steel is used.
The extra cost for enamelling often doesnt justify the use of a cheaper steel. Also consider the fact that corrosive chemicals has a tendency to be
found outside the equipment, mostly where they do most harm... (Murphys Law as applied to a chemical engineers everyday headache)
/rickard
[Edited on 9-2-2004 by rikkitikkitavi]
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axehandle
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Then pray tell why Oxford University would list PVC as nitric acid resistant. When coming to think of it, I've seen it listed as resistant in
several other places.
Can you cite a reputable source saying otherwise?
And, btw, and this is not meant as a flame, but I researched porcelain enamel for another pet project of mine that you don't want to know about
--- the modern porcelain enamels have a very high tolerance to impulse as well as tensile stress; basically, anything that doesn't deform the
substrate won't deform or crack the enamel.
[Edited on 2004-2-12 by axehandle]
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Mumbles
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Does it specifically say concentrated Nitric Acid though? The way I understand is it is resistant to nitric acid at normal temps. At elevated
it doesn't stand a chance. Just because it is resistant to it doesn't mean it can hold it. It might hold up for a week or so, but it will
be eaten away eventually.
http://hillbrothers.com/msds/nitric.htm Look at section X
I did see a lot more saying it was resistant to, than not though.
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axehandle
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Yes, it does. Actually is say "resistant" both for <30% >70% and "concentrated".
But I agree that PVC wouldn't stand a a snowball's chance in hell at elevated temperatures...
The chart I'm referring to is for gloves for emergency spill sanitation. PVC might not stand up to long time exposure, like e.g. storing
andydrous nitric in a PVC canister....
The info in your link doesn't say if PE-HD is resistant. I would like it to be once my first batch of nitric is ready, since I really HATE glass.
Glass breaks, plastics don't.
[Edited on 2004-2-13 by axehandle]
[Edited on 2004-2-13 by axehandle]
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