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madscientist
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[*] posted on 20-5-2002 at 19:30
Nitrated sugars


I prepared a small amount of nitrated sucrose recently. The procedure that I followed was:

1) Place 250mL beaker in ice/salt bath.
2) Pour 20mL of concentrated nitric acid into beaker.
3) Slowly add 40mL of concentrated sulfuric acid, making sure the temperature of the contents of the beaker does not rise about 20 degrees Celcius.
4) Wait for temperature to fall to 10 degrees Celcius.
5) Slowly add 14g of C12H22O11 (sucrose) to the mixed acids, making sure the temperature does not rise about 20 degrees Celcius.
6) Stir gently for several minutes. The sucrose will slowly form a gelatinous mass, usually attaching to the stirring rod.
7) I then left it in the ice bath to nitrate overnight.
Filter out the mixture from the beaker, running water through the contents of the filter to reduce the acidity.
9) Take the filtered nitrated sucrose and place it in another beaker. Add several grams of NaHCO3 (baking soda). Add around 40ml of water. Stir and poke the nitrated sucrose until the mixture is no longer bubbling.
10) Pour off the remaining water. Rinse the nitrated sucrose until it is neutral.
11) Let water evaporate off.

I believe runaway nitration temperature is about 40 degrees Celcius, due to a disaster that occurred two days ago when I was distracted by a parental figure for a short while, immediately after I had removed the beaker from the ice bath for a few moments to raise the temperature... I then forgot about that. When I went back outside to check on it later, I found a black mass in the beaker, acid splattered everywhere, and my good mercury thermometer had been broken and ejected from the beaker. By the way, I was able to salvage the mercury, which remained in the mixed acid so all I had to do was rinse out the beaker until the pH was about 7, pour off the water, and dump the mercury into a tiny glass container.




I weep at the sight of flaming acetic anhydride.
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[*] posted on 20-5-2002 at 19:32


Nitrated sucrose is very annoying to dry; it takes days to get the water content down to a reasonable level. It is not sensitive enough to be a primary explosive (does not explode when heated by flame) but it does burn far faster than nitrostarch. When burned, it releases the faint odor of nitrogen oxides. It burns fairly quickly, and leaves little to no residue. Soon I will carry out sensitivity tests.



I weep at the sight of flaming acetic anhydride.
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PHILOU Zrealone
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[*] posted on 20-5-2002 at 19:37


Madscientist forgot also to say what was the concentration of the acids...concentrated means everything and nothing in chemistry!

Anyway:
Assuming that you meant over 90% HNO3 and 98% H2SO4;
Suggar is C6H12O6
CH2OH-CHOH-CHOH-CHOH-CHOH-CH=O or an aldohexose.
Reaction with HNO3 leads to oxydation product of the aldehyd part into gluconic acid and other inerchain oxydation products.
Reduction of the aldehyd part leads to an hexaalcool = sorbitol or manitol....
When conc HNO3 is used in the cold, you get a moderate yield of pentanitric ester; excess HNO3 is needed and this causes a lot of oxydative degradation --> risks of runaway since oxydation is always exothermic.
Conc H2SO4 dehydrates suggar into C black and also lower the yield if ever used to increase HNO3 power and absorbs water.
The best way to go good yields is thus cold and excess 100% HNO3 and very little 98% H2SO4!

From Rudolph-Meyer's Explosives, 4th edition:
During the first WW, cane sugar was processed to get nitrosuggar or (pentanitrogluconic acid).
In its pure form, it is too unstable to be used in practice; a liquid explosive called "nitrohydren" was prepared by conitration of cane sugar solutions in glycerol and processed into gunpowders.However those mixtures were much more difficult to stabilise than NG alone and are no longer of interest.

Power must be right in the middle of Nitroglycerin (propanetriol trinitrate)/Hexanitromanite (manitol hexanitrate/ hexanehexol hexanitrate):
*VOD between 7600 and 8200m/s
*lead block test between 520 and 510 ccm/10g
*impact sensitivity between 0,2Nm and 0,8Nm
might be lower than 0,2 since they mention it to be hard to stabilise unless they mean storage lifetime stabilisation!

If nitrate ester are below the critical mass, they simply burn! Hammer impact test on 1mg sample is the way to feel its power or wrap a little of it in Al foil prior to heating, keep a safe distance, goggles, gloves and labcoat!

PH Z
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[*] posted on 10-7-2002 at 09:04


there are many other sugars you can nitrate, like Sorbitol and Mannitol.
i have expirience with SorbitolHexanitrate, very good explosive with a quiet good brisance(for a nitrated sugar). When i have acces to mannitol i will try to make Mannitolhexanitrate, wich should be very good like i've heard.





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[*] posted on 13-7-2002 at 16:21
??


Would it be usable as a primer to a larger explosive?

Raistlin




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PHILOU Zrealone
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[*] posted on 8-9-2002 at 11:59


Yes of course! If fully nitrated it is equivalent to solid/frozen NG and a little less than HNM (so better than PETN but more sensitive too).The only problem is to know if it is well nitrated or not...you can have a mix of 5 mononitrates esters+ 10 dinitrate esters+ 10 trinitrate ester + 5 tetranitrate esters and 1 pentanitrate ester...owing to the high probability of uncomplete nitration in non water free excess HNO3; the resulting product might be hard to cristallise (owing to the mix of various molecules), hygroscopic (due to free OH unnitrated).
This not counting with the inner oxydation possible products of OH groups (cetons, aldehydes, carboacids).

For infomationnal purpose, and for the ones that like the things to be clear and correct on the chemical level (like me :P)
Suggars are defined to be aldo and ceto pentose/hexoses; sorbitol and manitol even if they are sweeteners derived from the reduction of some suggars can be called suggars; they are polyols!
Sorbitol and mannitol are hexols and doesn't contain any aldehydic group (aldose) nor cetonic group (cetose)!

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[*] posted on 8-9-2002 at 12:01


By "can be called suggars" I meant CAN'T BE CALLED SUGGARS...
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[*] posted on 22-9-2002 at 08:28


Has someone tried nitro-fructose and what are it's properties as aposed to nitro-mannite
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Lynard
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smile.gif posted on 12-10-2002 at 04:12
powerful primary explosive


Can somebody tell me, if it possible convert
trideuteroacetonitrile (C2D3N)
into a powerful liquid-explosive ?




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Nick F
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mad.gif posted on 12-10-2002 at 04:20
What the fuck?


That has nothing to do with nitrated sugars!
And, why would anyone be SO stupid as to use the deuterated compund instead of normal acetonitrile?
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[*] posted on 6-11-2002 at 08:45
Nitrated sugars


It`s always a idiom !



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[*] posted on 6-2-2003 at 11:00


Has somebody tried nitrated fructose??
if not I will tryb and make it as soon as I get some new H2SO4 and post the results.
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bonemachine
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[*] posted on 9-2-2003 at 13:28
no sulfuric?


Is it possible for a sugar to be nitrated without the presence of sulfuric acid? The only reason i wonder is because the sulfuric dehydrates sugar every time i try to nitrate it.
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[*] posted on 9-2-2003 at 14:09


I while a go I made some mannitol hexanitrate and tried to make it detonate with some flash powder,
It failed.
I heard that mannitol hexanitrate could be detonated with flash, and that it was a primary is this true?
Or can it only be detonated with a detonator
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[*] posted on 9-2-2003 at 14:56


Well, if you have a kilo, it might me. But if you have a small quantity (a few grams) you'll only burn it. And the flash powder is supposed to be confined in a tube, so the tube rupture will produce the shock. It's like a hammerblow, but a VERY powerfull one.
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thumbdown.gif posted on 9-2-2003 at 22:08
Sucrose nitrate failure


I too had tried to prepear some sucrose nitrate. I added 30ml of H2SO4 into a 250ml beaker then added 25ml of HNO3, set it into a ice bath then slowly added 10 grams of sucrose not letting the temperature go above 20*C.Then I let it react for a hour.I took it out of the ice bath, brought it inside and went to the local ace hardware . After 2 hours I return home along with some NaBr, Ca(OCl)2, KNO3, NaNO3 ,H2SO4, and teflon tape. When I got home my house had a strong smell of HNO3. Then when I went to chech my experiment the thermoneter was at 80*C. And there was a carbon mass in there. And the liquid was also baclk. My mixture had dehydrated. And my whole house smells like strong HNO3. I opened up all the windows, then my parents arrived home they was pissed off at me. I am in trouble right now with my parents.



TNT
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[*] posted on 10-2-2003 at 05:43


Trinitrotoluene, hopefully that will teach you not to leave a nitration alone for TWO HOURS!!

Bonemachine, you ned to dissolve the sugar in cold HNO3 first, and then slowly drip in H2SO4. This will avoid dehydration.
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[*] posted on 10-2-2003 at 19:23
halogens


For what purpose is NaBr sold? I've been wanting to expirement a bit with the non-gaseous halogens like bromine and iodine, mainly to see how well stuff burns in them but its not exactly easy to find elemental halogens but I figure it isn't too difficult to generate chlorine which could be used to replace the Br- or I- in a salt, outdoors an in small amounts of course as not to suffer from the chlorine. For that matter, are there any common iodides that can be found in any usable amounts(2% iodine out of an ounce in tincture of iodine is a bit costly). I've searched online and pretty much the only one I could find is KI for protection against raiation.
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[*] posted on 11-2-2003 at 20:50


NaBr is sold as a pool cleaner or balences, needless to say it is at pool stores, home depot, and target among others.

Bromine is toxic and corrosive, as is iodine and all other halogens so dont think beacause they are not gasses there safe, for producing any halogen most likey all you will need to do is use MnO2 and an acid and heat the halogen bearing material. For iodine use an acidified h2o2 soultion and it will ppt.

CTR




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[*] posted on 19-3-2003 at 06:56


CD3-CN would be denser,but hell expensive vs CH3-CN!

You can make a binary explosive of it that has the power and sensitivity of NG simply by mixing it with HNO3(100%), N2O4(l) or C(NO2)4!
Using CD3-CN will only increase a bit the power (by 1 to 5%) owing to a better density but it is not worth the price!

Also CD3-CN is unstable!
CD3-CN + H2O (air) --> CD2H-CN + CDH2-CN + CH3-CN + HDO + D2O

A much better thing to test would be:
Heavy metal salts of polynitrogluconic acid...for sure sensitive primaries; also the cyclohexanhexol (inositol I think) (-CHOH-)6

All suggars should display relatively comparable properties except some of them are a little more stressed and will display slightly different densities, impact sensitivities, heat sens or VOD!




PH Z (PHILOU Zrealone)

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[*] posted on 7-10-2003 at 11:30


i nitrated some sugar today using NH4NO3 and H2SO4 since i don't have HNO3 available, the yeld was poor but not too bad, i nitrated 20 grams of sugar and now i have around the same amount on nitrosucrose in a sticky form.
I am trying to dry it, even is not easy at all since is damn sticky and impossible to handle.
I wonder, is that possible to nitrate oil products? like nitrate the tablets used for light starting? and is that possible to nitrate paraffin?
Thanks




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[*] posted on 7-10-2003 at 18:21


Fire starting tablet are generaly hexamine, there is already a lot of info on this, for parafine i dont know...



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[*] posted on 7-10-2003 at 20:07


not over here, here they are petrouleum products, nver seen hexamine..
Beside that the yeld of nitrosugar is extremely poor, i used equimolar amount of NH4NO3 and H2SO4, 40 ad 44g, 20 grams of sugar in order to operate in large excess nitration mix, the nitration was performed by dissolving sugar in the nitration mix at low temp, then add conc H2SO4 while stirring, kept the temperature around 0°C for one hour, then the sludge was dumped in large excess water, and the sugar nitrate was floating on top, was collected and neutralized with NaHCO3 molding with hand to make it penetrate. Then was left over a piece of plastic wrap where it almost melted like a gum under the sun becaming extremely sticky.
A burn test was performed and was rather fine, burns fiercerly but slower than NC making lotsa of smoke. Now is drying out, i guess for taking it out from the plastic wrap i'll have to freeze it...


[Edited on 8/10/2003 by Nevermore]




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[*] posted on 10-11-2003 at 16:21
Nitrofructose


I got some pure fructose for some tests about nitrating it, looks like nobody tried to nitrate it until now, i hope the presence of the pseudo ring won't led to excessive sensitivity or instability of products and that it will be easy to nitrate as mannitol.
[Edited on 11/11/2003 by Nevermore]
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[Edited on 15/11/2003 by Nevermore]




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[*] posted on 15-11-2003 at 05:55
synth result


Today i performed a test synth of nitrofructose, 40 grams powdered and dried NH4NO3 were mixed with 30ml H2SO4 96%, the mixture was cooled till it reached 8°C in a large water-ice bath, then 6grams of pure human grade fructose were added in little parts while vigorously stirring; temp raised to 10°C where it remained for all the nitration time, before all the fructose was added it was noticed that chuncks started to appear in the mix. After 5 minutes the mix was full of large chuncks of a yellow hard solid, rubber like consistance (definitely not chewingum like nitrosucrose). The nitration was let continue for 10 minutes while stirring then it was watered down in a far large excess water, the yellow solid collected at the bottom in two large chuncks, after the acid were decanted off and new water was added a change was noted in the solid, it started to turn white and to powder down.
In a cople of minutes, and with the help of the stirring rod all the chuncks were broken in small pieces that turned to be white small cristals. I suppose the fructose agglomerated so only the outside layer could be fully nitrated, the lower nitrate were soluble and gummy consistence and eventually dissolved in water.
Neutralization was performed, the synth yelded abour 3 times (still wet) the volume of fructose used in tiny white cristals, completely insoluble, very similar to AP cristals.
They are drying at now over a porcelain surface for successive testing.




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