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Fantasma4500
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Unreasonably fast nitration product of cellulose
im talking with some guy who doesnt care if people watch what he makes, he doesnt have no background what so ever in chemistry, most likely will get
confused if you yell HCl loud enough at him 
anyhow, he got hold of the nessecarities for making NC, as a person close to him knows how to handle this can help him with it, no worries about that.
to the point although, he send me videos of the results, and seemingly by this ratio
H2SO4 100 mL
KNO3 70g
he got some insanely fast NC, i suspect this of being hexanitrate, as it selfconfines, and makes a small poof
i got plenty of videos to back this up
______________________
http://www.youtube.com/watch?v=DsClF2j2n34
http://www.youtube.com/watch?v=5gAHAxvU7O4
http://www.youtube.com/watch?v=delfSJMf9xU
http://www.youtube.com/watch?v=zKeDIjsVuRQ
______________________
the video he followed to make this, i talked to him, he got the same results in his videos, but after asking him he openly said that he double
nitrated it, i know however the guy who owns the videos i linked above didnt double nitrate it, not only because he told me during the whole process
what he was doing and it was also his first nitration
it was let nitrate first 1 hour in water that had been standing in icecold water, thereafter for a total of 14.5 hours nitration it was washed with
water and baking soda, of what i understand
this isnt beginners luck, neither is this a definition, i attempted to repeat this but got the usual results, seemingly tri nitrated NC, nothing
special
i cant figure out what that could make any difference, and im now recrystallizing my KNO3 as theres seemingly AntiCakingAgent in it, but this wouldnt
make a that massive difference, anyhow.
any inputs around this would be appreciated, especially suggestions on what to check up on that could be missed, as in differences about nitrations,
because theres major difference
i neutralized the last parts of acid left in the lumps with NH4OH, very weak solution, then water again, also i let it nitrate from approx 19:00 to
13:00 next day
again, seemingly hexanitrate, without 99% HNO3!!
i dont recall hearing about hexanitrate ever without 99% HNO3
edit: forgot a word
[Edited on 3-8-2013 by Antiswat]
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Dany
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from the video, i think this is ordinary nitrocellulose but a very pure form of it. deflagration speed of energetic material is influenced by many
factors (e.g., particle size, morphology, physical state...). Impure NC leave residue, it is clear in the video that the NC is pure so the
deflagration is fast with no residue left . Don't think that if you nitrated the NC many time you will get a pure glucose hexanitrate, because acid
hydrolyses of sugar polymers (cellulose, chitin) generated lots of organic byproducts. in my opinion this is a pure form of NC not glucose
hexanitrate.
Dany
[Edited on 3-8-2013 by Dany]
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papaya
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Antiswat, I've heard that treating cellulose with NaOH solution (maybe boiling, don't know) before nitration helps a bit. Also what if NC is soaked in
KNO3 and dried, will this be faster?
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Bot0nist
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Cellulose doped with a nitrate salt will not burn faster at all!. I suspect either additional nitrations, higher temp, or longer durations in the salt
acid mix. Any of these or a combination will result in much more completely nitrated cellulose. Hexanitrate is incorrect here, IIRC. The trinitrate
is the fully nitrated product... me and Rosco and others debated it in one of the lengthy, pre-existing cellulose nitrate threads.
[Edited on 3-8-2013 by Bot0nist]
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papaya
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Hexanirate is correct in regards to "two monomeric units" of cellulose, while trinitrate is to single "di-glucose" unit, this all stems from
definitions rather than different structures (if I remember correctly there was even dodeca- one once used, sorry don't remember source).
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Dany
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It is interesting to calculate theoretically the density of the two possible anomer (alpha and beta) of glucose hexanitrate. although the alpha
diasterioisomer should be the major one after nitration of glucose (because of anomeric effect) some beta anomer will be formed during the nitration.
I don't expect a large crystal density difference between the two anomers but it is interesting to see what diasterioisomer is the denset.
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malford
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I recently made a thread on the various forms of NC. This conversation obviously should have been had there.
Some of my samples of NC made a cracking sound after igniting them, not a whooshing sound.
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Fantasma4500
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hmh.. yes malford, im sure bfesser will be more than glad to merge the threads haha
i realised that using larger quantities of my new yield i get this same somewhat selfconfining, but im still doubtful that its of same quality as the
guys stuff is, i will however try taking some trinitrate and add to KNO3 H2SO4 mixture
anyhow i mean to have seen an old document, where they described 1 - 10 nitrate (mono to deca) from hepta to deca was used in gunpowder industry, so
im pretty clear that they measured that it was deca and not hexa, and neither tri
they found as much as 10 different qualities..
the thing with NaOH sounds pretty interesting tho, and makes abit of sense to me.. i might try that, but chemcamtv have a video on trinitrate
(supposedly) re-nitrated with HNO3 and H2SO4
i also once had ONE little damn drop of 99% HNO3, in which i nitrated some trinitrate with and got a much better burn rate..
so there most definately is more than just decent nitrocellulose, magicians use a very high quality NC also, which burns away very quickly
but what comes to my mind is that there must be something making a massive difference, because my stuff doesnt burn as fast as his does..
ill have another go with 99.9 KNO3, recrystallized
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papaya
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I wonder if you deliberately introduce into your nitrating mix small amounts of "impurities" like heavy metal ions, Fe3+, Cu2+, etc and some of it
will get stuck into NC in micro quantities, will it show any catalytic effect ? I feel the secret may lay in impure chemicals.
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Bot0nist
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Burn rate is a poor way to determine quality, as many variables can effect this, like dryness, consistancy, partical size/surface area. The best way
to tell if you have a fully nitrated cellulose is impact testing. A small peice of fully nitrated cellulose (~14% N, IIRC), nutralized and dried,
wrapped tightly in foil, will detonate consistantly when struck by a steel hammer on a steel anvil. A lesser product will rarely respond, if at all.
Unrelated, but this is also the best way to determine if TNP is acually mostely TNP, and not a large portion of it is DNP and other
oxidation/nitration products. TNPs impact sensitivity is much higher than DNP. This holds true for fully nitrated vs. lesser nitrated cellulose as
well...
[Edited on 4-8-2013 by Bot0nist]
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Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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caterpillar
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Cellulose hexanitrare is a nonsense. Highly nitrated NC burns fast- one can put a piece of it onto his arm and ignite. There will be no pain- it
disappears in an instant. And look at the rest- there should be no carbon (carbon means NC with low percentage of nitrogen).
Women are more perilous sometimes, than any hi explosive.
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plante1999
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Just a random note. I remember saying an old extract from an explosive book saying how 0.5g !!!! of nitroso guanidine could be detonated on one upper
hand making no flash and only scratching the surface of the skin. Those old time chemist where really manly! Detonate stuff on hand ha ha!
I never asked for this.
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caterpillar
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Most likely, it was not a detonation but deflagration only. Some people want to feel a shock wave- they have a fun, exploding stuffs, standing near
them (as for me, shock wave is not as dangerous as splinters). BTW, one of my friends told me about his experience in Afghanistan. An ordinary hand
grenade doesn't kill. If one wants to kill himself, he has to use "limonka"- a lemon- shaped grenade with thick steel body. The other story which I
heard was about an first-class private German. He has a habit to explode German hand grenade (it has a long wooden handle) in his own hand. He was on
leave and it was a way to win something from young officers- they did not believe that such triick is possible.
Women are more perilous sometimes, than any hi explosive.
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Fantasma4500
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well bot0nist, if i start hammering inside my neighbours will realise its me.. (:
i have however packed decent quality (trinitrate) in 4 layers of al foil, very very tightly, then when i held a flame to it, it detonated, throwing
off a trick shred of al foil in one direction, blasting a hole through the 4 layers of al foil
i do believe you can test the quality on deflagration, but yes as papaya also mentions, it might even be about catalysts???
it COULD actually be quite interesting to check up on it.. but im sceptical, as the Fe2O3 would come as FeSO4 or Fe(NO3)2 and then need heating to go
into Fe2O3..
same for CuO etc.
so i find it pretty unlikely actually
about 0.5g on the hand im also pretty sure it wasnt a detonation.. usually a detonation knocks a hole in a metal plate.. dont know how many times you
want to repeat that on your own flesh, lol
anyhow a grenade CAN kill.. trust me.. we can make a bet.. if you swallow a live grenade im quite sure it wouldnt be the fragments alone killing you,
but i suppose the old german grenades must of been made somewhat like a claymore and yet a grenade.. perhaps he was just playing with the chances??
cant imagine he wouldnt get the handle shot through .. well everything??
but be sure a grenade thats not pineapple shaped can surely kill, otherwise they wouldnt be considered dangerous, right?
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Fantasma4500
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also another thing.. there must be someone with head in the business very very sure on the grades.. here they talk in percentages of nitrogen..
Type Nitrogen content
Grade A, Typ I 12.60 + 0.10 %
Grade A, Typ II 12.60 + 0.15 %
Grade B 13.35 % min.
Grade C, Typ I 13.15 + 0.05 %
Grade C, Typ II 13.25 + 0.05 %
Grade D 12.20 + 0.10 %
Grade E 12.00 + 0.10 %
http://nitrocellulose.synthesia.eu/eng/energetic-nitrocellul...
ive seen these infamous percentages mentioned alot of times before, but wouldnt you need the full chemical formula to be able to calculate on the % by
weight nitrogen? i havent found it for hexanitrate, infact i dont recall reading the chemical formula for any specific xnitrate NC
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Dany
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A simple elemental analysis of the NC will let you now the percentage of each element. Molecular weight can be calculated from experimental data. for
example, Mw of polymer can be calculated by measuring their viscosity and compare it to a known reference (reference which Mw
is known accurately).
Dany.
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Dany
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for Antiswat,
Cellulose hexanitrate is completely false. A glycosidic unit of cellulose has 3 free hydroxyl group at position 2,3,6. On the other hand, position 1
and 4 ar attached to another glycosidic unit to form a glycosidic bond which is an acetal (AND NOT AN ETHER!). of course the configuration at position
1 and 4 in cellulose (or chitin) is beta, this mean that the bond formed with the next glycosidic unit is equatorial. again, position 2,3,6 are
available for nitration or other reaction (e.g., acetylation). you can talk about glucose hexanitrate or other diasterioisomeric form (galactose,
mannose...), because all hydroxyl unit are free for reaction so complete nitration will yield the hexanitrate product.
Dany.
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caterpillar
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Quote: Originally posted by Antiswat  |
anyhow a grenade CAN kill.. trust me.. we can make a bet.. if you swallow a live grenade im quite sure it wouldnt be the fragments alone killing you,
but i suppose the old german grenades must of been made somewhat like a claymore and yet a grenade.. perhaps he was just playing with the chances??
cant imagine he wouldnt get the handle shot through .. well everything??
but be sure a grenade thats not pineapple shaped can surely kill, otherwise they wouldnt be considered dangerous, right? |
As I remeber, an ordinary grenade contents 90 gr of TNT. I was not killed, when my charge (200 gr approximately- well, not as powerful as TNT- AN+
dinitronaphtalene) went off, when I was standing near it (1 meter, surely less than two).
Women are more perilous sometimes, than any hi explosive.
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Bot0nist
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Shrapnel...
Lets get this back on topic please... No weapons disscusion.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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Fantasma4500
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you sound like youre right dany, im not anywhere near that knowledge on organics, so i will take it as being trinitrate as the best
but still very surely there is better NC than tri nitrate, or well by burn speed.. how come?
my goal with NC is to get the fastest burn speed of all.. if you made NC you will know that you cant have NC laying around freely for long time before
you have burnt it all off in your hands
apart from that, the elemental calculation / measuring is something ive always wondered about, and as ive always expected it does sound complicated,
thanks for the input, now i can finally sleep ^^
always expected it to be a rough 200g tho, taking ''gr'' as not being grains but rather GRammes, but yes as bot0nist says lets get back to.. well no
weapon talk again..
anyhow i would expect 90g of HE to give pretty well ringing ears no matter how you cover your ears..??
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Dany
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For Antiswat,
theoretically when all the hydroxyl in cellulose are nitrated you have 14.1%N, however in industry nitrocellulose is synthesized having 13.5%N. if you
could fully nitrated cellulose to reach 14.1%N and then purify the resulting compound you should be able to get very fast burnig NC. Impure NC, often
leave residue. these impurities, act as a flame cooling agent when NC burn, so impure NC will burn relatively slow with a dim flame, and don't forget
that other physical properties affect deflagration not only a single factor. as for determination of nitrogen content, ion chromatography can also be
used (Anal. Chim. Acta. 2011, 2, 196-203).
Dany
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killswitch
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Dissolve the nitrocellulose in acetone or methyl ethyl ketone and allow it to partially evaporate. Using tweezers, pluck the thin sheet of white
matter off of the surface of the liquid. Please note that it will likely be extremely delicate, exhibit excessive static cling, and can float across a
room just from the air current produced by someone walking through at a brisk pace.
My very first nitration of cellulose, using drain cleaner sulfuric acid, singly-recrystallized and not-quite-dry instant cold pack ammonium nitrate,
and a cotton ball from the drug store, neutralized with Arm-and-Hammer, produced a yellow cotton ball that simply became very gooey and sticky upon
addition of acetone. Decanting the acetone and evaporating it produced a small quantity of nitrocellulose that functioned just as well as the sample
in the video.
Alas, the rest of the cotton ball was mostly a bust. It did burn slightly faster than a normal cotton ball, but not by much.
So, in essence, reprecipitation from acetone or other solvent is key to purity.
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Bot0nist
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That will seperate any non-nitrated cellulosem but will not seperate only fully nitrated product, because even partially nitrated cellulose is soluble
in acetone. It is a good way to remove any big clumps or fibers of cotton that were not nitrated though. I store most of my cellulose nitrate as a
dilute laquer in acetone, actually. Thats how I use it though, to paint on things like e-matches or homeade fuses and such. The laquer can also be
poured onto a peice of foil very thinely, and dried. The resulting sheet can be powdered up quite finely by hand. This is a good way to achieve a good
density if detonation of the product is the goal.
The choice of substrate definatly matters as well. Look into micro-crystalline cellulouse. a very fine and consistant substrate will make make
complete and fast nitration much easier I would imagine. I have never obtianed any myself, but have read about it on this board. Let me search and see
if I can find the post I read that in...
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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caterpillar
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if you want to get NC with the highest amount of nitrogen, use phosphorous acid instead of sulfur one (actually, it means mixture of HNO3 and P2O5-
read famous book, written by Ledgard)
Women are more perilous sometimes, than any hi explosive.
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Fantasma4500
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well thanks, Dany..
i did read a new thread, if you have seen it in energetics you might recall it if you come around this thread again, as in being the one where a new
user describes nitration of 1.5kg cotton with 8kg H2SO4 and 5kg HNO3
he describes that the finished NC is BOILED in NaHCO3 solution to remove ABSOLUTELY ALL acid traces
this might also affect burn speed
edit: i was one time able to increase burn speed of what seemed as being really good NC with dumping 1 drop of VERY VERY precious 99% HNO3 on it and
forgetting about it, thats the best way to run long time chemical syntheses and what not
[Edited on 28-8-2013 by Antiswat]
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