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rikkitikkitavi
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Ca(NO3)2 starts to decompose at 500 C , above melting point the decomposition is vigorous acording to Gmelin. There is patents describing a process
for this decomposition, since the CaO formed hardens teh melt and makes heat transfer tricky.
Long before this water is of course given off, and any NH4NO3 is decomposed.
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spudmann-annm1
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I'm new here, can I ask a few questions. First does the glassware need to be from DURAN glass, secondly can you make 95% nitric acid, by putting
70% nitric in a dessicator, or can you destill (or distill, don't know how you say) 70% nitric to 95% nitric acid?
--------------------------------------------------"
READ the thread and educate yourself on the basic principles of chemistry before you post. Check the thread about "The
book on chemistry
[Edited on 12-10-2004 by vulture]
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Theoretic
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"spudmann-annm1"
The username seems a bit dodgy to me. I think if you look carefully, you notice "annm" - yes, ANNM. Seems like another kewl to me...
although I might be wrong.
[Edited on 13-10-2004 by Theoretic]
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Polverone
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Maybe so, but here we do not hunt for <strike>witches</strike> <strike>communists</strike> kewls. Rather we let people speak
until/unless they prove incapable of communicating productively.
PGP Key and corresponding e-mail address
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spudmann-annm1
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Edit my username
Can you please edit my user name to spudmann1, so that the other members won't get nervous, I'm not an anarchist if you mean that, i just
yet don't know how to detillate things, but I am like everyone an expert in a specific field. If you think this post or my membership is
impropriate just exclude my membership.
What is a kewl?
[Edited on 14-10-2004 by spudmann-annm1]
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neutrino
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Your username cannot be edited. You can, however re-register under a different name. You've only made 3 posts, so you wouldn't be loosing a
significant number anyway.
I'm sure that there are those who can define what a 'kewl' is much better than I can, but kewls are usually morons who read the
anarchist or terrorist handbooks or some other crapbook, try stuff out not knowing anything about it, and are, to varying degrees, brain-dead.
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MadHatter
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TROLL
GODDAM ! Is that a troll I'm smelling ?
From opening of NCIS New Orleans - It goes a BOOM ! BOOM ! BOOM ! MUHAHAHAHAHAHAHA !
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Theoretic
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Sorry, meant no offence. 
What TROLL? 
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ADP
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Just did a vacuum distillation of HNO3, pics soon to follow. I'm pretty excited considering it's about 90-95+% HNO3 
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crazyboy
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Someone purely interested in destruction, explosions, mischief or causing harm to living things or property.
| Quote: |
What TROLL?
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I'm not sure if this is a question but if it is here's an answer, a "troll" is a term usually used on totse (generally considered a kewl forum) to
describe a thread or post that is fictitious and is meant to deceive or joke with other members.
Example: I have an intense sexual attraction to fruits especially citrus is this normal?
| Quote: |
Just did a vacuum distillation of HNO3, pics soon to follow. I'm pretty excited considering it's about 90-95+% HNO3
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Can't wait to see the pictures I have been meaning to synth some HNO3 but as of now I don't have a distillation setup and am too poor to afford one.
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ShadowWarrior4444
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| Quote: | Originally posted by crazyboy
Someone purely interested in destruction, explosions, mischief or causing harm to living things or property.
| Quote: |
What TROLL?
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I'm not sure if this is a question but if it is here's an answer, a "troll" is a term usually used on totse (generally considered a kewl forum) to
describe a thread or post that is fictitious and is meant to deceive or joke with other members.
Example: I have an intense sexual attraction to fruits especially citrus is this normal? |
Four years later. *smirk*
I am certainly looking forward to photos of the apparatus used in the vacuum distillation. And perhaps a cursory writeup of the reagents involved.
Also, whether you used a substitute vacuum grease!
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ADP
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HNO3 Vacuum Distillation
Alright guys so after coming home for the summer and rummaging through my chem supply, I decided to synthesize some HNO3. The following "reagents"
were used:
Liquid Lightning (H2SO4 Source)
KNO3 (Nitrate Source)
Because my last scale is broken (new one on the way), I measured out 500mL of liquid lightning and basically added nitrate salt until the solution
was saturated with KHSO4, which makes it hard to stir. I added a small amount of distilled water (50mL or so) to make the solution easier to stir and
so I could add a little more nitrate - the excess H2SO4 will keep it from being distilled over and it will make the solution boil more smoothly.
The following photos are an account of my project:
Here is my distillation setup. It is all 24/40 ground glass. I used an oil bath to maintain temperature at 60dC at all times - my solution boiled
vigorously at this temperature without decomposition.
This is my mixed acid solution for distillation.
After about 25 minutes of distillation...
My final yield - I final run time was about 1hour 10minutes
My vacuum aspirator - this baby does WONDERS
Notes:
There was about 500mL mixed acid at time of distillation.
Temp was held constant at 60dC for 1hr10min.
The distillate stoped coming over when the mixed acid started a runaway "foam" production under vacuum. To prevent this from coming over I
immediately killed the vaccuum. Another attempt was made to boil the solution again but the foam started rising again... I still got a good yield.
I have not measured the volume of the yield yet but think it is about 200mL
Possible improvement: Use NH4NO3 as NH4HSO3 is more soluble in acid.
Purity test:
I plan on (when my new scale arrives) doing a density test on exactly 1cc of the acid to determine purity. I dropped a penny in a small amount of the
acid and it intensely reacted making a cloud of NO2 and totally dissolving the penny - I was impressed...
Any thoughts guys?
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zeppelin69
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Where did you get that aspirator? I have been searching all over and I just can't seem to find anything worth buying, but your's looks pretty decent.
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ADP
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I purchased that one on eBay about 3 years ago, it's does really well for my expectations.
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mr.pyro
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excellent post ADP Ive been looking for something like this with pictures. approx what vaccum do you think your aspirator pulls?
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ADP
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Thanks, glad you like; I believe my aspirator pulls a vacuum down to at least 30mmHg, but it depends how hot or cold the water you run through it is
IIRC. Colder water will produce a slightly stronger vacuum due to the vapor pressure of water. That interests me though... maybe one day this week
I'll see how cold I can get water to boil...
It is very very useful for nitric since decomposition starts at 72dC which is normally much lower than it boils. I can get copious amounts via a
considerably strong boil at 60dC, I remember it boiling at 40dC as well.
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MagicJigPipe
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ADP, in my experience, with density tests, the more liquid you use the better. I suppose because it "evens out" innacuracies. Where if the weight of
the 1cc is off by even .05g, severly affecting accuracy, if the weight of 100cc is off by the same or even more the accuracy won't be as bad. As a
preliminary test you could even use some cheap scale, determine the weight of the bottle and the volume of the liquid, and then... Well, I'm sure you
know.
Try that. At least it will give you some idea until your decent scale arives.
"There must be no barriers to freedom of inquiry ... There is no place for dogma in science. The scientist is free, and must be free to ask any
question, to doubt any assertion, to seek for any evidence, to correct any errors. ... We know that the only way to avoid error is to detect it and
that the only way to detect it is to be free to inquire. And we know that as long as men are free to ask what they must, free to say what they think,
free to think what they will, freedom can never be lost, and science can never regress." -J. Robert Oppenheimer
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Formatik
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I can't get any good density readings with amounts like 1 mL, but I use at least 5 mL. With a graduated cylinder at 5 mL I've been able to get
accurate density readings. Plus if you don't already do it, make sure you are at eye level with the meniscus (bottom) or a density reading will be useless and be off by magnitudes.
[Edited on 20-5-2008 by Schockwave]
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ADP
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Yeah MJP you're right, I ordered a 10mL Mohr pipet so I'll do that for sure, I might do 50mL or something and then divide by 50. I'll do the density
tests this weekend. Today I did another vacuum distillation and got 170mL of nitric. I stored it separate because I used NaNO3 instead of NH4NO3 and
I want to compare results with the density. After that I'll mix the two and get some ACS sulfuric to distill the two to get highest purity HNO3 for
future endeavors...
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mr.pyro
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I tried a vac distillation today and ended up sucking out most of my vapors before they condensed. What did condense however was crystal clear and
dissolved a penny very quickly. I am going to build a fume hood and gas trap and try it again soon. ADP did you notice any leaks around your
ground glass or use any kind of sealant on the joints? Was there much nitric vapor sucked out of the apparatus by the vaccum?
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ADP
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Interesting you mention that problem - texaspete mentioned he had that problem as well, I personally put my receiving flask in an ice bath to prevent
that but I've done without before and had no problems. I don't use any grease for my glass joints, i usually get a couple drops of dH2O and put on
the outside of the joint once the vacuum is running to prevent any air from seeping it - it's usually negligible.
I think the best thing to make sure of is plenty of cold fresh water running through the condenser. I know the inside wall of my condenser 'rains'
vapor and is pretty cool by the time it gets to the receiving end. What does your setup look like?
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mr.pyro
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I have all 19/22 glassware because I bought it as a kit. I hope to upgrade to 24/40 soon however.
My boiling flask is 500 ml and runs through a 200mm west condenser and into a 250ml receiver. I have an old robinair vacuum pump that pulls like 50
torr. I control the vacuum with a T joint and needle valve to let air in and keep it at a relative vacuum of about 20"Hg. I use an inline gauge to
read it. Today I was getting nice rolling boiling with about 20"hg vacuum at around 65-70dC. I shall post pictures tomorrow or the next day as I
have broken the setup down to head home for summer.
Also during the distillation I had constant ice water through the condenser and the receiving flask in an ice bath. I still noticed nitric vapor
condensing in my tubing as well as my tubing connectors being attacked by the acid. However I can do ethanol distillations just fine without any
condensation in the tubing.
[Edited on by mr.pyro]
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mr.pyro
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Here is my setup.
200g of nh4no3 was added to 300ml bullzeye drain cleaner sulfuric acid.
Temp did not rise past 30dC during addition.
here are the photos of my setup.
My valves getting attacked by acid condensing in the tubing.
About 50ml of acid came over after 45 min of distillation under a 20"hg vacuum. Acid mix was kept at 60C. Unfortunately I think my AN might have
been wet or bad and it caused a poor reaction and it seemed to boil much less then other times I have done it. I am going to retry it with kno3 today
that I know works.
I also tried the teflon vacuum grease mentioned in other threads. It worked very well except for on the receiving flask where I had to clean it off
before I could pour out my product.
[Edited on by mr.pyro]
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crazyboy
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Don't fill the boiling flask more the halfway up!
and the thermometer bulb goes where the thermometer adapter meets with the condenser not in the liquid.
Also I would use an aspirator; nitric fumes could ruin your vacuum pump.
http://www.youtube.com/watch?v=3JlIPnyrZMw
^This may help.
EDIT: looks like ADP did it too the thermometer bulb doesn't go in the liquid it goes in the vapor!
[Edited on 26-5-2008 by crazyboy]
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ADP
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| Quote: | Originally posted by crazyboy
looks like ADP did it too the thermometer bulb doesn't go in the liquid it goes in the vapor! |
This is true for most distillations however, I am interested in keeping the temperature of the mix below 70dC therefore I am interested in monitoring
that temperature not the vapor temperature as I would of MOST distillations.
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