static_firefly
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Registered: 9-2-2004
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Strange oil
Hello
Reciently i was attempting a HDN nitration with HCl 30%, Hexamine fuel tablets, and KNO3. The KNO3 and HCl was added and cooled in a freezer until
about 0-3degrees C. Then a saturated soultion of Hex was added to the mix, approxamitly doubleing the volume. Sorry for not haveing weights, i didnt
take any. A precipitate formed and quickly disolved into the soultion, as it does when not filterted fast enough. The mix was warm when the hex
soultion was added. I attempted to precipitate the HDN out by adding approx 1/1 ratio of metho (96%ethanol) and stired. The mix went a slight milky
colour which i am belive was probably the HDN. This was stired and left to sit for 10min. When i observed it again there was a small amount of oil
floating on top. It smells terriable, kinda like alcohol but different and much more intense. It seems to give me a slight head ache when i got near
it (with in a meter or so). When i try and stir the oil into the solution it doesnt seem to sink. I stir as fast as i can and it doesnt seem to sink
down into the mix. Its flammable like metho, but its not metho (im sure because theres a lot less oil then there is metho in the mix). I soaked a
little into some tissue paper and slamed it with a hammer, but it doesnt seem to be sensitive to impact (judgeing if it were a primary exposive). I
then soaked a little in some tissue paper and wrapped that in alfoil and put that in a fire (doing that to AP will cause it to detonate). The oil
didnt seem to detonate so i dont think its a primary explosive.
my question is, what is this oil? its smells very bad and gives me a slight head ache, so it might be a nitrate of some sort (like ng head aches). I
duno what this is but i dont want to invesigate it too much if its extreamly deadly.
I can probably get a photo. All the chemicals seem quite pure.
Thanks
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JDP
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Well if I had to guess what you got I'd say either ethylinechloride(does that even exist?) or ethylnitrate(which I dought because of the weak
conc. of the HNO3 formed). I think in future experiments when the hex. is added and it heats up, you should cool it down to as cold as possible, that
should precipitate out the HDN. Then filter it and then wash it with the alcohol.
[Edited on 9-2-2004 by JDP]
~JDP
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chemoleo
Biochemicus Energeticus
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For one thing, I would purify the hexamine first. Dissolve it, as it is, in water and see if you get any solid/liquid residues that do not dissolve.
Get rid of that by filtration.
Then, for formation of the nitrate salt, use COLD temperatures (<5 deg C), and add your acid slowly to prevent heating up. I wouldn't use HCl,
use dilute H2SO4. HNO3 and HCl together surely forms additional products which could be very reactive.
Also, prepare your acid separately and then only add it to your hexamine solution.
Anyway, this belongs into the Energetic Materials section.
[Edited on 9-2-2004 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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