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axehandle
Free Radical
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Location: Sweden
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What were you doing your distilling in? When I hear bucket I think plastic... And if it
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A galvanized steel bucket, with 10 layers of aluminum foil strapped to the top, with a lead weight in its middle to make a sloped cone.
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was glass how did you make a hole in it for the trough?
hmm, I just reread some of it and did you make the reaction vessel out of aluminum foil?
If I am not completly confused you made a still out of tinfoil, now thats cool
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Not tinfoil. Al foil and a power drill and some McGyverism, but it worked....
If I had a scanner, I would draw a picture, but imagine that where the drops fall down, there is a V shaped through leading out through the side of
the bucket, slighly sloped. Hardly rocket science, but I was only 15....
[Edited on 2004-6-19 by axehandle]
My PGP key, Fingerprint 5D96 E09E 365D 1867 2DF5 C2FE 4269 9C19 E079 CD35
\"Verbing nouns weirds the language!\"
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vulture
Forum Gatekeeper
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Al is only resistant to HNO3 vapour when it's reasonably pure. That's where the trouble starts with commercial foil, even more because
it's usually based on a PE foil.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Esplosivo
Hazard to Others
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When we are talking about vacuum distillation of nitric acid what should the pressure in the apparatus be? Is 65 mbar sufficient? Thanks
Theory guides, experiment decides.
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Proteios
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65mb give or take 1/10th of an atmosphere.... Yeah.. that aint too bad a vacuum.... i would expect the HNO3 to distill pretty quickly at about 40ish
C.
Certainly with the range of a hairdryer! 
[Edited on 20-6-2004 by Proteios]
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Esplosivo
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Thanks Proteios. I intended to use a water filter pump. I found one better now reducing the pressure of the distillation app to approx. 20 mbar.
Theory guides, experiment decides.
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Marvin
National Hazard
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Water aspirator will depend a lot on the temperature and pressure of the water from the tap. 20mbar is probably very close to the water vapour
pressure.
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Esplosivo
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As seen on catalogue it says it can attain 20mbar with a water pressure of 1bar. There are others which can attain even lower pressures with a water
pressure of 1.4bars - reducing the pressure of the app up to 16 mbar.
Ooo, btw thank you all for the help.
[Edited on 20-6-2004 by Esplosivo]
Theory guides, experiment decides.
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Chemtastic
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Possible Alternate Pathway
Instead of distillation, wouldn't this reaction work?
HCl(aq) + AgNO3(aq) --> AgCl(s) + HNO3(aq)
243g of AgNO3 are soluble in 100g of H2O, but only 0.00019g of AgCl are soluble in the same volume of water.
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Marvin
National Hazard
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If the HCl is a solution in water, and the AgNO3 is a solution in water, you wont get very strong nitric acid at the end.
Recycling the silver is a pain, needed because silver is expensive and silver nitrate is more expensive. Producing silver nitrate uses up nitric acid
and you end up making dilute nitric acid from dilute nitric acid.
Distilling from silver nitrate is a good way to remove trace chloride from nitric acid though.
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demolitions
Banned
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Registered: 1-9-2004
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further concentration
if its not too much trouble, could someone explain to a true chemistry novice how to further concentrate 70% nitric acid to at least 90%? seems like
trinitrotoluene and PETN can be produced with nothing less... and all this distillery talk seems to be in code
it probably kills brain cells
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vulture
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Read the thread mister.
If it's code for you, educate yourself.
Don't be a lazy fuck. I personally detest lazy fucks.
[Edited on 2-9-2004 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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demolitions
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sorry, just looking for a shortcut
maybe if I had the time to write over 1300 posts and sit in my basement with a tinkertoy chem set... your waffling your life away belgian fucker
by the way, i'm sure you have other people to insult seeing as how this is barely the least intelligent question asked on this forum
it probably kills brain cells
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fvcked
Harmless
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Your asking to be spoon fed. And what I say to people asking to be spookfed is "spoon feed your ass!". You are not smart enough to do
ANYTHING other than baking soda and vinegar. Hell I wouldnt trust you with toilette opener. Go bury yourself in a chemistry book, then come back!
(I like to flame)
Oh bubble trumps!
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Magpie
lab constructor
Posts: 5939
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Location: USA
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Mood: Chemistry: the subtle science.
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Is this right: you've got the time to make TNT and PETN but not the time to learn about the distillation of nitric acid?!
Vulture doesn't need anyone to stick up for him - but he is doing more than playing with a chemistry set - he happens to be a chemical
engineering student and that is not a trivial pursuit. I personally don't see how he manages to do that and make over 1300 posts, plus
discipline and dispose carcasses like yours. He must indeed love his work.
The single most important condition for a successful synthesis is good mixing - Nicodem
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The Ed
Harmless
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Yeah dude, seriously. If you didn't notice, Vulture is a mod. Repent as soon as you read this and maybe he'll let you live. He might prefer
seeing you get flamed by all of us than banning you anyway.
One way to further concentrate 70% nitric acid is to mix it with concentrated(i'd say 98%) sulfuric acid, then distill it at 80 degrees C. The
water will stay with the sulfuric acid. That's all the info you'll get from me. But if you want to be able to make PETN and TNT you'll
need to understand enough basic chemistry to break our mysterious code, otherwise you might lose a limb or even your life rather than just your forum
membership.
But... lmfao. "your waffling your life away belgian fucker." Sorry Vulture, I get a kick out of that.
[Edited on 3-9-2004 by The Ed]
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vulture
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Demolitions has been demolished. 
Now back on topic.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Centimeter
Harmless
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Registered: 19-5-2004
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H2SO4 is quite expensive where I live, so its use in HNO3 production is a pain. Thus I shy away from using nitrate salts to produce HNO3 as the
sulfuric acid can't be recycled. Thus I am left with concentrating 68% HNO3. This way I don't even have to use sulfuric acid as no
protonization is neccesary. I was wondering if anybody had a good method of producing HNO3 by bubbling NOx through water. I am prety sure that this
could generate 68% HNO3. Alas, how to produce the NOx gas. Does anybody know of a cheap and easy way of producing the NOx? I know that nitrate salts
can be decomposed through heating, but this seems to involve farely large temperatures. I was thinking that perhaps the reciprocated haber process
would be a good option, however this would invovle some complex equipment. Any thoughts? On another note, I was wondering if I could use HCl as a
substitute for H2SO4 in nitrations/HNO3 production from nitrate. The HCl would easily produce nitronium. One could then use all sorts of chemicals to
take the water out of the reaction; magnessium nitrate comes to mind.
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JohnWW
International Hazard
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As for a possible substitute for H2SO4 in nitrations of aromatics: I think the only definitely viable alternatives would be perchloric acid, HClO4,
and hexafluorophosphoric acid, HPF6. Others which just might work could be periodic acid, perbromic acid, selenic acid, tetrafluoroboric acid, or
phosphoric acid. Permanganic acid and chromic acid, and other high-valent transition-metal acids, would be suitable if they did not decompose, or
oxidize organic compounds, so readily. The reaction conditions may result in oxidation of the Cl- in HCl by nitrate, if HCl is used.
In any case, it has to be a stronger acid than HNO3 and one which resists oxidation, in order for the latter to accept a proton. Because the
electrophile in nitration is the nitronium ion, NO2+, formed by such protonation of HNO3, the only way you could get away without using such a
stronger acid is by using a nitronium salt - which in any case exist only of the strongest acids, i.e. NO2ClO4, NO2PF6, (NO2)2SO4, stronger than
nitric acid.
BTW I have heard somewhere of the tetrafluoroammonium ion, NF4+, having also been produced in combination with the same acid anions, analogous to
NO2+. However, it cannot
be used to produce compounds exactly analogous to nitro-compounds, retaining all 4 fluorines, because pentavalent N cannot have more than 4 covalent
bonds besides an ionic bond with the positive charge on the N. But a compound like N-trifluorophenylammonium perchlorate, [C6H5-NF3]+[ClO4]-, should
be possible, although it does not show up in a Google search.
John W.
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neutrino
International Hazard
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Calcium nitrate, available as a fertilizer, decomposes to CaO, NOx, and O<sub>2</sub> at modest temperatures (~200*C, I think). To
produce nitric acid, the following reactions are utilized:
3NO<sub>2</sub> + H<sub>2</sub>O ->2HNO<sub>3</sub> + NO
NO + 1/2 O<sub>2</sub> -> NO<sub>2</sub>.
[Edited on 12-9-2004 by neutrino]
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Centimeter
Harmless
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I was under the impression that it took somewhere around 500*C to decompose calcium nitrate. This was most likely what I was going to go with, but
500*C uses a lot of energy. I think the most practicle would be to use the haber process. Does anybody have some good plans for such a setup?
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neutrino
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I'm not really sure of the temperature needed. Are you sure you want to use the Haber process to make ammonia? The reason it's used
industirally it because it's cheap and east to do with vast amounts of equiptment (about a small city's worth--the factories are huge), but
on a smaller scale, it would be impossible. Ungodly pressures (~200 atm) would be the main problem. If you want ammonia, there are better ways of
getting it. Get it from the store or decompose some ammonium sulfate fertilizer.
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Centimeter
Harmless
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I guess so, but it just sounds like a realy interesting procedure. Anyhow, I figured out what I am going to do. I have acess to 15.5-0-0 fertilizer. I
am going to convert it all to calcium nitrate by adding Ca(OH)2 and boiling. I am then going to mix a solution of calcium nitrate with iron sulfate
and filter out the subsequent calcium sulfate. This should produce iron (III) nitrate which decomposes at around 100*C. Does anybody know the ratio of
NH4NO3 to Ca(NO3)2 in 15.5-0-0 fertilizer? I wouldn't want to add too much calcium hydroxide now would I.
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JohnWW
International Hazard
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I remember reading somewhere that, before deposits of niter (mostly KNO3 with some NaNO3) were discovered in the rainless north Chilean desert, and
before the Born-Haber process was developed for ammonia along with methods for oxidation to nitrate, nitrates for use in gunpowder were obtained from
urine and animal manure. Of course, it was not very pleasant for the workers.
John W.
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neutrino
International Hazard
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Pure Ca(NO<sub>3</sub> <sub>2</sub> would be 17.1-0-0,
meaning that your fertilizer probably has a bunch of chalk/other binders in it and isn't pure calcium + ammonium nitrate. What I'd do is to
dizzolve the the stuff in a generous amount of water, filter out the insoluble junk, then keep adding Ca(HO)<sub>2</sub> until it stops
dizzolving. Filter and boil down the solution to obtain crystals.
If anyone is interested in nitre beds, there was a thread on EW Here.
[Edited on 13-9-2004 by neutrino]
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MadHatter
International Hazard
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Ratio
Centimeter, if I'm not mistaken, that formula for the double salt appears as:
5[Ca(NO3)2] * NH4NO3 * 10[H2O]
This is for the 15.5-0-0 fertilizer. The stuff I get is always coated with that
pain in the ass wax so I place it in a filter of several paper towels and run
ice water through it until only the wax remains in the filter. Then I treat
the solution according to my needs.
According to both of my CRC manuals, the melting point of Ca(NO3)2,
NOT the hydrated version, is 561 C. Neither manual lists a decomposition
temperature.
The decomposition temperature of the tetrahydrate depends on which
version of the CRC you trust.
Tetrahydrate formula: Ca(NO3)2 * 4[H2O]
The CRC 52nd Edition(1971-1972) says it decomposes at 132 C.
The CRC 81st Edition(2000-2001) says it decomposes at 40 C.
Neither CRC manual says what it decomposes into. It's possible that
it decomposes into the anhydrous version and water vapor but until I
have a more detailed source of information, I can't say for sure.
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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