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Author: Subject: Sucralose Nitrate
Madog
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[*] posted on 13-4-2003 at 16:50
Sucralose Nitrate


for a while ive been wondering about nitrateing Sucralose, aka splenda, its a non-calorie sweetner. its just sucrose with 4 Cls subsituteing for 4 of the OHs.

i took 3 packets of splenda, they each contain a gram of sucralose. i added them to 15ml of nitric acid and they disolved easily, then i put it in an ice bath and slowly added 30ml of sulfuric acid with stirring. it turned cloudy and there were chunks of product forming. after the addition i let it sit for a little while and then crashed it into some water and let it sit on my coffee machine hot plate while it settled. it was pretty liquidy on the bottom but i was able to get it all out and stuff. it looksl ike i have a good yield but its not weighed.

some of it actualy looked yellow, and some was green, but now sience they mixed when i fished it out its white, strange. this must have to do with the other things in the splenda.

it is alot more gooey than sucrose nitrate, its sticky. i burnt some and i could smell the chlorine. it burns more inconsistantly than sucrose nitrate because it cnat be over tetranitrate. this is also why its so gooey

the point of this was to make an explosive that released a toxic gas on decomposition, im going to set it off later.

does anyone else have any ideas like this? just anything strange or new to nitrate?




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Madog
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[*] posted on 14-4-2003 at 12:57


i just set some of the sucralose nitrate off with a hammer, its pretty sensitive but not as sensitive as PETN, close though



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a123x
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[*] posted on 16-4-2003 at 15:59


That's pretty cool. I might tr making some sucralose nitrate when I get the chance. Sounds like it has a pretty nice sensitivity, sensitive enough to initiate with a hammer but is still safe to handle and also easy to make. This is a bit off topic but how sensitive is normal sucrose nirate?
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Madog
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[*] posted on 16-4-2003 at 18:35


well, the whole reason i made it was for the hell of it and because it releases chlorine which is cool. it is actualy a mixture of nitrates of some other things that are in the sweetner too.

sucrose nitrate is pretty sensitive, more so than PETN.

for something to use i would just make sucrose nitrate. but sucralose nitrate is cool. sucrose nitrate is alot easier to work with cause its not so damn gooey!(at least if you make it so its not under nitrated)

they are both really neat explosives




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[*] posted on 24-4-2003 at 07:54


Is sucrose nitrate soluble in acetone? I ask because my only source of reasonably pure nitric is to make it with sulfuric acid and calcium nitrate with calcium sulfate being insoluble. I don't want to have to bother with filtering the calcium sulfate out but rather I'd prefer to just add the sucrose, then add the H2SO4 slowly in small amounts at a time in accordance with the only procedure I could find for sucrose nitrate. The problem would be that CaSO4 will endup remaining in the product. I figure if sucrose nitrate is soluble in acetone I could dissolve it in acetone then filter out the CaSO4. Also, is the slow addingof the H2SO4 necessary in the production of sucrose nitrate or could it be done more along the lines of cellulose nitrate synths in which the H2SO4 and HNO3 are mixed before the cellulose is added?
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Madog
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[*] posted on 24-4-2003 at 08:10


you dont have any KNO3 NaNO3?

it is soluble in acetone, and not in water.




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[*] posted on 24-4-2003 at 09:39


I have NH4NO3, from that I can produce other nitrates. The reason I would use Ca(NO3)2 is because CaSO4 is insoluble so that the reaction between Ca(NO3)2 and H2SO4 would end up not having any metal cations in it. Pretty much it just produces a purer HNO3.
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[*] posted on 24-4-2003 at 10:01


You should just use NH4NO3 + H2SO4 then. The AN dissolves nicely in sulfuric acid, though it tends to solidify at about 0 C. You can get around this by using excess sulfuric.
Then just use the solution directly as your nitration acid and drown in ice and water when the reaction is complete; the only insoluble is your product.
This procedure works when synthesizing all nitric esters that I can think of from EGDN and NG over nitromannitol and other nitrated sugars to PETN.
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Madog
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[*] posted on 24-4-2003 at 10:05


sucrose carbonises on contact with H2SO4, ever seen one of those little kiddy science shows where the dude throws some H2SO4 in a beaker of sugar and it makes a colum of ash?

does manitol carbonise as easy?

get it really cold, the reason why the sucrose/sucralose is disolved in the HNO3 first and H2SO4 is added carefuly is cause of the carbonation




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[*] posted on 24-4-2003 at 11:03


Yesterday I didn't boil my 2NH4NO3 + Ca(NO3)2 solution long enough since it still smells quite strongly of ammonia so I'm jut going to go ahead and try using H2SO4 + NH4NO3 to nitrate some sucrose.
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[*] posted on 24-4-2003 at 23:08
success


Well I think I've succeeded in making sucrose nitrate. I added NH4NO3 to H2SO4 let it dissolve which took an annoyingly long time since the NH4NO3 wasn't very finely powdered. Then I added the sugar which was not reduced to carbon. At this point it was like a rather thik syrup. Then a little at a time I added more H2SO4. Still a pretty thick syrup. I stirred it for a while until I started noticing some chunks forming in the mixture. I allowed about 10 minutes from the start of them forming to when I ended the nitration by pouring the mix into ice water. The white and rather moldable did not dissolve in the water. I added some sodium bicarbonate to the solution to neutralize it a bit then poured it into a filter and as I type this it is filtering. I don't see what these white chunks could be other than sucrose nitrate. Well I have to go remove the product from the filter and completely neutralize it.
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[*] posted on 25-4-2003 at 08:54


Only semisuccessful. It was really quite moist so I decided to dry it on an ashtray on a small hotplate for keeping coffee mugs warm. This turned out tobe a bad idea because it got too hot and seems to have decomposed some of my product. The rest I allowed to cool down a bit and then I scraped it off into a little ball an lit it. It deflagrated decently, not as well as fluffy cellulose trinitrate but I think as well as NC thats been dissolved in acetone and rehardened into a solid piece. I also took a small amount and tried detonating it with a hammer, with no success. I think my mistakes were that I used stoichiometrical ratios of nitrate to sucrose when I really should have used excess nitrate. Also the weather hasn't been very good so I can't concentrate my drain cleaner so the H2SO4 is most likely only aound 93%. The weather seems decent today though so I might be able to do that today and then make a more succesful batch tonight.
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[*] posted on 25-4-2003 at 09:09


how much did you use? you know, sucrose nitrate can be as high as a octaanitrate



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[*] posted on 25-4-2003 at 09:41


I used 12g of NH4NO3 to 5.9g of sucrose. This puts the ratio of NH4NO3 to sucrose at just over 8moles NH4NO3 to 1mole sucrose. I imagen that a large part of the problem is really just that my sulfuric acid really wasn't as concentrated as it really should have been.
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[*] posted on 25-4-2003 at 10:21


Remember that the sticky product will retain a LOT of acid after neutralization, so you should dissolve it in acetone and add some bicarbonate to the acetone solution. Then pour into water to precipitate. It might not crystallize very fast, but leave the ( water ) soln overnight and it should collect at the bottom.
The liquid might still be very opague, but I think this is mostly oxidation products and other impurities.
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[*] posted on 25-4-2003 at 18:31


ok, hm, good idea microtek, heat the water to melt it after it precipitates and get it under control(i sugest)



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[*] posted on 25-4-2003 at 19:25


Interested too is the sweet nitration of
melampyrit

hexanitroxymelampyrit
O2NO-CH2-(CHONO2)4-ONO2

or the experimental way to the Peroxide of the tetranitrate,
the dicyclonitroxy isomer and the tricyclonitroxy isomer --->

dicyclotetranitroxymelampyritperoxide
>O-CH2-(CHONO2)4-O-O-CH2-(CHONO2)4-O->

and

tricyclotetranitroxymelampyritperoxide
>O-CH2-(CHONO2)4-O-O-CH2-(CHONO2)4-O-(CHONO2)4-O->


:)




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[*] posted on 25-4-2003 at 22:49


Error correction of the copy mistakes to my last post !!!

hexanitroxymelampyrit
O2NO-CH2-(CHONO2)4-CH2-ONO2

dicyclotetranitroxymelampyritperoxide
>O-CH2-(CHONO2)4-CH2-O-O-CH2-(CHONO2)4-CH2-O->

tricyclotetranitroxymelampyritperoxide
>O-CH2-(CHONO2)4-CH2-O-O-CH2-(CHONO2)4-CH2-O-O-CH2-(CHONO2)4-CH2-O->




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Madog
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[*] posted on 9-5-2003 at 17:52


i looked in the bottle of sucralose nitrate, the substance is fuill of bubbles

then i opened it and took a little sniff, the Cl was enough to make me jerk back. it decomposes

may just be from acid tho




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[*] posted on 14-5-2003 at 06:40


al23x, you used 12 grams of NH<sub>4</sub>NO<sub>3</sub> and 5.9 grams of normal sugar, but how many grams/ml's of H<sub>2</sub>SO<sub>4</sub> did you use? You make a statement that you put as much H<sub>2</sub>SO<sub>4</sub> in to make it a little less sticky.
This sounds like a fun explosive to make as a test, but has anyone ever tried it in a bigger scale? Like a detonation of >100 grams?
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Madog
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[*] posted on 14-5-2003 at 10:44


i would, but the yields suck so bad, it would be awsome sience its high density, sensitive, and damn powerful(if its highly nitrated)



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smile.gif posted on 4-6-2003 at 03:46


Krypton:
melampyrit = sorbitol or manitol or else?
Never eard of that polyol.

Sorbitol is HOCH2-(-CHOH-)4-CH2OH
Manitol is the same but stereochemisty is different.
You can have:
8 different stereoisomers!

Inositol is also interesting being cyclohexanhexol it could lead to a cyclic hexanitrate ester (-CHONO2-)6

Normal suggar is aldohexose
HOCH2-CHOH-CHOH-CHOH-CHOH-CH=O
C6H12O6
Complete reaction with HNO3 will lead to
O2NOCH2(-CHONO2-)4CO2H plus oxydation compounds.
Because of the acid moity the pentaester is unstable and hard to stabilise...reason why production has been stoped just after war where it was used in gunpowder in place of NG (because there was a lack of glycerol).

It is much better to reduce the suggar first in a way to get sorbitol and then to make it react to get the hexaester... no -CO2H, thus neutral.
:cool:
:cool:
:cool:




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[*] posted on 4-6-2003 at 13:45


Hey maddog, do you suppose that a flash powder salute in the 3-5g range might be enough to detonate sucrose nitrate in quantities of like 10g+. I was just thinking about this because I think it would be pretty decent and safe as booster for ANFO or just as a charge by itself rather than having to use a sensitive organic peroxide.
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wink.gif posted on 4-6-2003 at 23:53


Melampyrit is only a special form or stereoisomer of hexanehexol for the microbiology. :mad::P:mad:
The mp, density and PH is a bit different
to the others.




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smile.gif posted on 6-6-2003 at 09:56


I have at home:
*80% bw sorbitol solution
*4 kg pentaeritritol
*mesoinositol
*Polyvinylic alcohol

I can't wait to try nitration of those, but I need to redistill some 98% HNO3 ... and now my mother is too often at home.
:(:(:(

About flash to detonate solid polynitric ester...yes but you would need confinement.
Better use CuO/Al explosive and ultraheat generating thermite (4600°C at 2km/s should give enough kick to detonate anything).
:cool::o:cool::o:cool::P:P:P




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