megalomania
June 17th, 2003, 08:06 PM
the freshmaker
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posted 05-31-2001 02:30 PM
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Does anyone have more information on nitrosucrose besides this?
Nitrosucrose (Sucrose octonitrate),
C12H1403 (ONO2) s
The nitration of cane sugar , yields sucrose octonitrate, white glistening needles, which melt at 85.5°. If heated slowly, nitrosucrose decomposes at about 135° and if heated rapidly deflagrates at about 170°. The fused and solidified material has a specific gravity of 1.67. It is readily soluble in methyl alcohol, ether, and nitrobenzene, difficultly soluble in ethyl alcohol and benzene, and insoluble in water and in petroleum ether. It reduces Fehling's solution on warming. It is relatively stable when pure. Monasterski reports that it gives a feeble puff under a 20-cm. drop of a 2-kilogram weight, a puff with one of 25 cm., and a detonation with one of 30 cm. He states that samples of 10 grams in the Trauzl test gave average net expansions of 296 cc.
VoD?
If anyone have tried this, please let me know! Thanks
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Mr Cool
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posted 06-01-2001 05:35 PM
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VoD is quite high, probably around 6500 m/s I'd guess. Make it in the same way as you would make MHN (basically, you dissolve 10g of sucrose in 50ml of 99% HNO3 at 0*C, cool to below 0*C, and drip in 55ml of 99% H2SO4, keeping the temp. below 0*C. I got about 10 grams of ONS after lots of purification).
I did this recently, so I have some experience with it, but I don't know about long-term storage or anything.
Can be easily detonated from small amounts of HMTD, by very rapid heating (touching with an orange-hot bit of wire), and by a hammer blow. I bet you could also use the H2SO4/metalNO3 method as well.
If you have any questions I'll try to answer them.
the freshmaker
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posted 06-02-2001 08:40 AM
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High VoD, good sensitivity......sounds great.
I only have around 70% HNO3, would that suffice?
How powerfull is it compared to fx TNT?
Do you think it could be detonated from flashpowder ? (strong heat and a slight shockwave)
How did you purify it, since I have heard it could be unstable if not propobly purified?
thanks alot Mr.Cool
Mr Cool
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posted 06-02-2001 09:55 AM
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I don't know if that 70% HNO3 would work. However, it's very similar chemically to mannitol hexanitrate (except that it's cyclic), so I'm sure the H2SO4/NH4NO3 method would work, like it does for mannitol.
I think it would be more powerful than TNT, by about the same amount as nitrostarch (20-30% more powerful?). Mixing 67% ONS with 33% NH4NO3 makes a mixture with an oxygen balance of roughly zero, that is nearly as sensitive as ONS alone. TNT must have something like 75% NH4NO3 added to make a zero oxygen balance.
Good flash powder will almost certainly detonate it.
I purified it by washing with water, then recrystalising twice from pure methanol with a bit of Na2CO3 added, then twice from pure methanol, and drying at 40*C.
the freshmaker
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posted 06-03-2001 05:56 AM
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It sounds like some really good stuff!
When you mix it with NH4NO3, isn't it also getting more powerfull?
Will ONS/NH4NO3 mix also detonate from a flashcharge?
How dangerous is it to handle it?
(I know ALL explosives are dangerous -in some way or another!)
How sensitive is it compared with Tetryl?
I will make some ONS in my dreams in next week, so if anyone have some tips or warn's please tell me!
Thanks again!
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Mr Cool
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posted 06-03-2001 06:06 AM
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Mixing with NH4NO3 might improve power by using up all of the fuel available, but ONS is more powerful thn NH4NO3.
The mixture will probably detonate from flash, but I've never tried it.
Treat it like a very dangerous primary (that's how I treat all explosives!), this will make sure you don't knock it too hard or anything. I'd recommend not handling it too much, since I don't really know how unpredictable it is. I'd guess it was a lot more sensitive than tetryl, but I haven't compared them.
the freshmaker
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posted 06-03-2001 07:02 AM
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Sucrose octonitrate. ONS
DoV: 6500 m/s (approximately)
spec. volume of gas: ?
Traulz test: 296cm3
impact sensitivity: ? (2kg - 30cm)
friction -- : ?
melting point: ?
Can someone fill in the gabs?
Have anyone else than Mr.cool tried this explosive? what about you PHILOU?
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Mr Cool
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posted 06-03-2001 08:14 AM
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Melting point 85.5*C
Impact sensitivity between 20 and 30cm with 2kg weight, although my hammer weighs about 2kg, and when dropped on a few granules of ONS it detonated from 20cm. It wasn't just a puff like the extract at the top of the thread says. Maybe this is an indication of impurity?
Anthony
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posted 06-03-2001 12:00 PM
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ONS sounds great I'm going to have to give it a go with the H2SO4/NO3 method, what kind of ratios would you need with this method?
the freshmaker
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posted 06-04-2001 05:11 AM
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Anthony please post your results when they are ready. Have you got the ratios? Does anybody have the ratios for H2SO4/NO3 for making ONS?
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Mr Cool
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posted 06-04-2001 01:08 PM
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Just work out how much H2SO4 and XNO3 are needed to make 75 grams of HNO3, and mix these and use them as the HNO3. You might need to add more H2SO4 to dissolve your nitrate (use NH4NO3).
Anthony
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posted 06-04-2001 06:02 PM
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OK, this is something I should really know, so please bear with me as I try to work this out...
RAM of 1 molecule of HNO3 would be 1x1 1x14 3x16 = 63
For one molecule of HNO3 you'd need one molecule of NH4NO3 to supply the NO3 and 0.5 molecules of H2SO4 to supply the H.
So you should need twice as many molecules of NH4NO3 to H2SO4.
RAM of NH4NO3 = 2x14 4x1 3x16 = 80
RAM of H2SO4 = 2x1 1x32 4x16 = 98
80/63 = 1.27
98/63 = 1.55
75gm x 1.55 = 116gm/2 = 58gm H2SO4
75gm x 1.27 = 95gm NH4NO3
So I reckon 95gm NH4NO3 and 58gm H2SO4 to make 75gm HNO3. Was I even close?
the freshmaker
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posted 06-05-2001 05:04 AM
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Nice, Anthony!
One more question: When detonating ONS with flashpowder is it then because of the incredible heat OR the (small) shockwave?
Mr Cool
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posted 06-05-2001 05:36 AM
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I suspect that it's the very rapid rise to a very high temperature, although I haven't actually done it.
Anyone else got any results yet?
Anthony
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posted 06-05-2001 02:16 PM
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If someone can confirm/correct me on the H2SO4/NH4NO3 ratio I'll try it tomorrow.
Mr Cool
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posted 06-05-2001 02:29 PM
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Looks good to me.
Has the font/layout changed, or is it just my computer?
Mr Cool
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posted 06-05-2001 03:57 PM
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It was just my computer
Anthony
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posted 06-06-2001 02:33 PM
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I couldn't do it today as I realised that I didn't have any ice so I'll try it tomorrow.
One question though, does the NH4NO3/H2SO4 mix just replave the 50ml HNO3 in the above procedure? In that you add the sucrose to the NH4NO3/H2SO4 and then drip in 55ml H2SO4?
Mr Cool
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posted 06-06-2001 04:55 PM
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That's right, or drip H2SO4 into a mixture of the sugar and the NH4NO3. But you will need 55 mL of H2SO4, and however much is needed for the NH4NO3/H2SO4.
Who needs ice when you have NH4NO3 and water? You can get down to about -15*C with dry, powdered NH4NO3 and the right amount of water!
the freshmaker
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posted 06-07-2001 05:44 PM
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If some of you guys have made ONS could you please post the exactly method, how much acid, result etc. That would be just perfect!!
Thanx!!
Anthony
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posted 06-07-2001 07:16 PM
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I tried it today, I mixed the NH4NO3 with the H2SO4 in an ice bath, it all dissolved (amazingly) but when it cooled down it became very thick, like a solid mass. I out the reaction vessel in the ice bath in the fridge to assist cooling. Came back a bit later, shit, the ice bath has tipped and water has flooded the reaction vessel - nooo! I managed to tip up the beaker upside and all the water ran out but the NH4NO3/H2SO4 stayed still. I realised I had nothing to loose so proceeded anyway, a stir turned the reactants back into a very thick liquid, I didn't know how much water they'd absorbed but hoped the H2SO4 I was about to add would soak up any excess water. I stirred in the sugar with no noticable reaction. I could be bothered to drip the H2SO4 in so I stirred it in three portions leaving to cool for about 10mins inbetween, temperature stayed below 30*C (oops). I then put it in the fridge and shall look at it tomorrow. The solution was kinda of a yellow colour at the end.
All in all, a pretty botched job
Next time I'll mix the NH4NO3 and sugar dry and then add all the H2SO4 in one go to avoid the super-thick solution.
Mr Cool
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posted 06-08-2001 07:56 AM
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If you're gonna add all the acid in one go, cool it first to stop it getting too hot. Excess heat can cause a shit load of NOx and no product.
PHILOU Zrealone
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posted 06-08-2001 10:04 AM
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I have tried 7 years ago a weird mixture that is called vigorine!
A mix of KNO3/HNO3/Suggar and cellulose!
The mix was evolving red fumes and was like a thick paste; when a portion of it was light, it burned fearcely and flew accross the air!
The problem with this mix is that it needs to be used fast since free HNO3 in a suggar/cellulose matrix is very prompt to self ignite!
On a theorical level it is a good mix (works already with HNO3(70%)!I suspect the final mix with pure HNO3 to contain nitrosuggar,nitrocellulose and some KNO3 to improve the burning and the OB!
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Anthony
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posted 06-08-2001 01:47 PM
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I did wonder whether temps above 0*C would prevent ONS forming, or whether it was just a safety guide.
The result was a thick yellow goo, about the same colour as TNP. As ONS is not soluble I poured the lot into approx 500ml cool water which dissolved the AN prill "shells" (didn't grind the AN enough). I poured this through a paper filter and got didly squat so down the drain with the lot of it!
I didn't expect it to work considering the fuck ups. I think real HNO3 would easier to work with than the NH4NO3/H2SO4 shit.
the freshmaker
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posted 06-10-2001 11:22 AM
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No one have succeded yet? I think I will give it a go with my 70% HNO3. Shouldn't it be possible? If I used the same method as for making MHN how much 70% HNO3 should I be using?
fightclub
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posted 06-10-2001 05:18 PM
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That data above is from T.Davis's book, the references are missing.
Can't forget the data of Will and Lenze as shown in Urbanski for Sacharose nitrate (sucrose octonitrate!):
* Melt.point. 85 deg.C.
* Decomposition point: 135 deg.C.
* Weight loss Stability at 50 deg.C.: 11%
after 3 days --This means that for ex, 10g
after 3 days at this temp. will leave you
with 1.1g.
Also the other data in Urbanski referenced:
Monasterski (1933) examined explosive characterisitics of nitrosugars, and for nitrosucrose gave:
* Heat of explosion: 950 cal/g
* Lead block test: 300 ccm/10g
* Shock-sensitivity: 20 cm (2kg wt.)
Ref.: Monasterski S., Z. ges. Schiess- u. Sprengstoffw. 28, 349 (1933). --The same ref. as in Davis.
I calculated the detonation velocity of nitrosucrose: 7350m/s @ 1.6g/cc. Personally,
I think it is more in between 7000-8000 m/s.
(!)Be careful with sucrose nitrate it is highly unstable in acidic environment and will decompose exothermically in a chain reaction releasing heat energy and possibly exploding. It is absolutley necessary to keep the mixture cool with an ice bath during nitration, even after nitration the solution if left standing (bad idea) will decompose in an uncontrollable violent gas reaction involving nitrogen oxides and lots of heat!
T. Davis should have been(w/ the two refenc.):
Nitrosucrose (Sucrose octonitrate),
C12H1403 (ONO2)
The nitration of cane sugar(.sup. 69, 73), yields sucrose octonitrate, white glistening needles, ----etc.----
.sup.69 Will and Lenze, Ber., 31, 68 (1898).
.sup.73 Hoffman and Hawse, J. Am. Chem. Soc., 41, 235 (1919). Monasterski, Z. ges. Schiess- u. Sprengstoffw. 28, 349 (1933). Wyler, U.S. Pats. 2,081,161 (1938), 2,105,390 (1938), 2,165,435 (1939).
Anthony
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posted 06-10-2001 05:25 PM
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I'm not expert, but if you should still need 75gm of HNO3, which at 70% conc (density 1.41gm/cc) is 75gm/1.41 = 53ml
Mr Cool
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posted 06-11-2001 01:37 PM
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Mine didn't decompose that fast. Maybe it's not fully nitrated?
I don't think it will work well with 70% HNO3. Better to concentrate it, or use H2SO4/NaNO3 etc.
PHILOU Zrealone
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posted 06-12-2001 04:19 AM
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Fightclub:
11% weightloss at 50C in three days will lead to 8.9g from 10g starting material and a weight loss of 1.1g!
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Microtek
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posted 06-12-2001 10:17 AM
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A note on H2SO4/NH4NO3 mixes: It doesn't matter that it becomes solid when cooled; if anything it makes it less prone to runaway nitration as it mixes more slowly.
Just crush up the mix with the thermometer before you start adding the sucrose ( or mannitol or whatever ), and knead the mix during addition instead of stirring.
Mr Cool
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posted 06-12-2001 12:41 PM
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D'oh! Stupid of me. Mine didn't decompose that fast since it wasn't at 50*C!
Also, 11% loss, not 11% remaining, sounds a lot more realistic.
Anyone else made any yet?
the freshmaker
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posted 06-15-2001 04:21 PM
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I'm sorry but my I think my brain is dead... (maybe because of our weedparty last week)
Could someone be so friendly to post a complete recipe for making ONS with the H2SO4/NH4NO3 method, including all acid/nitrate ratios etc.
Thanks alot to everyone who post!!
the freshmaker
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posted 06-17-2001 09:07 AM
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Please!??? BTW is it Octo- or Octanitrate?
Mr Cool
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posted 06-17-2001 09:20 AM
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I've never done it that way, but I'm sure you could just follow the recipe for MHN with H2SO4/NH4NO3, in the MHN thread.
Anthony
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posted 06-17-2001 09:38 AM
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Briefly:
*Mix 95gm NH4NO3and 58gm H2SO4
*cool to *0C
*Add 10g sucrose
*Drip in 55ml H2So4
*Ensure temp stays sub 0*C
*Pour into 200ml water and crushed ice
*filter out ONS
I presume the last two steps will work as ONS is insoluble in water and any solid NH4NO3 will dissolve.
Both the NH4NO3 and sucrose should be dried before use.
Mr Cool
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posted 06-17-2001 09:42 AM
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..and then wash with water, recrystalise from methanol with NaHCO3, then from pure methanol.
the freshmaker
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posted 06-17-2001 10:36 AM
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Thanks guy's!!
Q
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posted 06-19-2001 04:54 PM
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Is it possible to mix all the NH4NO3+H2SO4 at the start to make a nitrating 'mix',cool it and then add the sugar?
Anthony
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posted 06-19-2001 09:31 PM
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I personally don't see why not, as long as the sucrose is added very slowly. Worth checking with MrCool first though
Mr Cool
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posted 06-20-2001 08:22 AM
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...or someone that actually knows what they're talking about! I just dreamed this, remember?!
I can't see any reason why that wouldn't work. Try a small batch, and see what happens.
Q
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posted 06-20-2001 04:15 PM
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I'll do that,but first I need to concentrate my H2SO4.Boiling is the normal way but since Encarta says it solidifies below 10*C could I freeze it to about 5*C and remove whatever liquid remains.I tried this with some old yellow non-fuming H2SO4{frozen to -10*C}except nothing solidified,it must have been contaminated.I can tons of battery acid
{thats about 40%,right}tomorrow.
One more question,would the H2SO4 not dehydrate the sugar into carbon before it had a chance to get nitrated?Just a thought.
frostfire
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posted 06-20-2001 07:01 PM
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whaaa?
H2SO4 solidify at 10 C, are you sure of that? it might be 10 Kelvin
Mr Cool
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posted 06-21-2001 09:27 AM
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It won't be 10*K, maybe 10*F. For all I know it might be 10*C, I've never tried.
The only worry I have about mixing all the nitrating mixture and adding the sucrose to it is that it might get dehydrated, but you might as well try it. It's not as if sugar is a great rarity!
the freshmaker
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posted 06-21-2001 10:41 AM
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How long time does the nitrating-proces of the sucrose need, to get fully nitrated?
[This message has been edited by the freshmaker (edited June 21, 2001).]
10fingers
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posted 06-21-2001 12:01 PM
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Q, pure sulfuric acid freezes at 10 degrees C. If it has water in it the freezing point lowers quite a bit. It wouldn't be much use in car batteries in the winter if it froze.
Q
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posted 06-21-2001 12:11 PM
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OK,I'll boil it down so.
Q
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posted 06-21-2001 05:49 PM
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I decided to try NC with my boiled down battery acid,and I appear to have failed.I boiled it down from 250ml to 90ml by putting it on a cooker ring at full blast.The result was a non-fuming,non-oily liquid.I've worked with conc. H2SO4 before and boiled down battery acid does not seem to the answer.Any pointers on where I'm going wrong would be greatly appreciated.Surely other people have had the same problem and overcome it.Thanks.
fightclub
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posted 06-21-2001 07:45 PM
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Yeah PHILOU Z., that is what I meant sorry for the mix up.
Mr Cool
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posted 06-22-2001 01:31 PM
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When boiling down H2SO4, it should fume strongly (while hot), and if you boil it then it'll certainly be 98%+. It boils at about 327*C IIRC. The cold acid doesn't fume, but it's quite thick, like a thin sugar syrup, and noticably heavier than water. Also, when I boil down drain cleaner, it makes those little "fingers" of liquid on the side of the container, like v. conc. HNO3 or whiskey. This might be an impurity I suppose.
Q
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posted 06-22-2001 02:48 PM
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One more question,for the nitration of glycerine is a high H2SO4 conc. needed because in a recipe given in another thread 4g of AN is added to 6ml of H2SO4.Would this not use up a bit much of the H2SO4 to create HNO3?My boiled down acid was not syrupy.Could I be heating it up to high allow the H2SO4 to evaporate?I didn't think I boiled it all that hard?
Anthony
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posted 06-22-2001 03:06 PM
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Q it shouldn't be a thick syrup, but you should notice it's thicker than water in the way it pours. It should still slosh.
If you did overheat the H2SO4 and boil off some of the H2SO4, it would definitely be at 98% as all the water would have been long gone by that temp. you'd just be reducing the amount of conc H2SO4 you've got.
4gm NH4NO3 to 6ml H2SO4 (that's 11gm) will leave plenty of H2SO4 left to soak up water produced during the nitration. Since tolo much water kills nitrations, having water to start with in low conc H2SO4 is going to reduced yields.
MrCool, surely you don't need to heat the H2SO4 to 300C+? Wouldn't over 100C allow the water to boil off without decomposing any of the H2SO4.
BTW BP of H2SO4 = 290C (Mega's page)
Q
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posted 06-22-2001 04:44 PM
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thanks for the input.
sorry to constantly be asking questions,but,
my h2so4/nh4no3 mixes fume,this is the hno3produced right not NO2 because I added the AN to quikly?
Also will high temps. in the production of NC
help or hinder nitration?Are low temps. purely to prevent runaway nitration or will some of the NC decompose at these high temps?
Thanks.
Q
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posted 06-22-2001 05:35 PM
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OK,I'm havin' serious problems makin' NC.Firstly I dissolved 3.9g NH4NO3 in 20ml of sulphuric acid.The solution goes cloudy and fumes{fumes smell like HNO3}Temp. rises to about 30'C.I then add enough cotton to soak up most of the mixture.No change in temp. is observed.After about 40mins cotton is slightly mushy and yellowed somewhat and smells strongly of HNO3.I then take out the cotton and put it in some water to wash it,but,the acid within the cotton reacts with the water,gets extremly hot and appears to dissolve ih the water[or divide up extremly finely}.On another occasion using the exact same procedure I sqeezed the cotton of most of its acid and put it in a jar with a little water.The cotton again heats up only this time produces lots of NO2 and appears to break down completely.Both proce. used pure and dry AN and 98% lab grade H2SO4.WTF is going on?
John456
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posted 06-23-2001 12:19 AM
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It sounds like when you add your NC to the water it might be getting hot enough to decompose it. Try putting your NC in a bowl of crushed ice after you finish nitrating it. The NC will heat up the ice it touches, melting the rest, but it will remain at a low temperature by the time all the acid is absorbed. Another possibility is that your using synthetic "cotton".
Q
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posted 06-24-2001 09:10 AM
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Well I tried ONS yesterday,following the procedure exept the temp rose to 10*C at one point,but otherwise averaged about 4*C.Anyway on mixing the acid/sugar solution with the water,while stirring,a brown doughlike scum formed on the surface and the rest of the solution was cloudy white.I left it over night to settle and a layer of extremely fine white crystals seemed to collect.I am now filtering them out.This sound normal so far?
Mr Cool
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posted 06-24-2001 09:22 AM
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Fine white precipitate sounds good, but I never got a dough-like brown mess when using HNO3. Sounds like you got patially dehydrated sugar (and perhaps partially nitrated).
I'm sure I read somewhere that H2SO4 boils at 327*C. In fact I KNOW I did, but it could have been a mistake. One of them has to be! And no, you don't need to heat it to it's boiling point to get it concentrated, but it's not necessarily true that heating to 100*C will drive off all the water. 69% HNO3 boils at over 100*C, which is over the bp's of both water and HNO3.
Anthony
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posted 06-24-2001 06:32 PM
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Whichever BP is right they're both much higher than water.
I did wonder whether the boiling point would be higher than 100*C. I think I heated to about 130*C (thermometer only goes to 120) there was a vapour coming off, I presume this could only be water?
Mr Cool
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posted 06-25-2001 04:30 PM
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If it's quite thick then at least some of it is sulphuric acid vapour. Water vapour condenses at a lower temperature, and therefore not just above the liquid like the H2SO4 vapour will.
Q
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posted 06-26-2001 11:22 AM
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So your telling me if I boil it to one third its original volume it will become syrupy because I tried it the last time with no joy and afterwards white crystals appeared to form[slight impurity,I'd say].How -exactly do conc. your acid?
Mr Cool
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posted 06-26-2001 12:44 PM
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Are you using battery acid? Sounds like you have lead sulphate or something if you are, forming crystals. Make sure you get the acid out of a CHARGED battery.
It won't get syrupy, but it's noticably thicker than water. Try putting a drop of it onto some paper - if it's strong, then it'll quickly turn the paper into carbon.
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posted 05-31-2001 02:30 PM
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Does anyone have more information on nitrosucrose besides this?
Nitrosucrose (Sucrose octonitrate),
C12H1403 (ONO2) s
The nitration of cane sugar , yields sucrose octonitrate, white glistening needles, which melt at 85.5°. If heated slowly, nitrosucrose decomposes at about 135° and if heated rapidly deflagrates at about 170°. The fused and solidified material has a specific gravity of 1.67. It is readily soluble in methyl alcohol, ether, and nitrobenzene, difficultly soluble in ethyl alcohol and benzene, and insoluble in water and in petroleum ether. It reduces Fehling's solution on warming. It is relatively stable when pure. Monasterski reports that it gives a feeble puff under a 20-cm. drop of a 2-kilogram weight, a puff with one of 25 cm., and a detonation with one of 30 cm. He states that samples of 10 grams in the Trauzl test gave average net expansions of 296 cc.
VoD?
If anyone have tried this, please let me know! Thanks
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Mr Cool
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posted 06-01-2001 05:35 PM
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VoD is quite high, probably around 6500 m/s I'd guess. Make it in the same way as you would make MHN (basically, you dissolve 10g of sucrose in 50ml of 99% HNO3 at 0*C, cool to below 0*C, and drip in 55ml of 99% H2SO4, keeping the temp. below 0*C. I got about 10 grams of ONS after lots of purification).
I did this recently, so I have some experience with it, but I don't know about long-term storage or anything.
Can be easily detonated from small amounts of HMTD, by very rapid heating (touching with an orange-hot bit of wire), and by a hammer blow. I bet you could also use the H2SO4/metalNO3 method as well.
If you have any questions I'll try to answer them.
the freshmaker
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posted 06-02-2001 08:40 AM
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High VoD, good sensitivity......sounds great.
I only have around 70% HNO3, would that suffice?
How powerfull is it compared to fx TNT?
Do you think it could be detonated from flashpowder ? (strong heat and a slight shockwave)
How did you purify it, since I have heard it could be unstable if not propobly purified?
thanks alot Mr.Cool
Mr Cool
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posted 06-02-2001 09:55 AM
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I don't know if that 70% HNO3 would work. However, it's very similar chemically to mannitol hexanitrate (except that it's cyclic), so I'm sure the H2SO4/NH4NO3 method would work, like it does for mannitol.
I think it would be more powerful than TNT, by about the same amount as nitrostarch (20-30% more powerful?). Mixing 67% ONS with 33% NH4NO3 makes a mixture with an oxygen balance of roughly zero, that is nearly as sensitive as ONS alone. TNT must have something like 75% NH4NO3 added to make a zero oxygen balance.
Good flash powder will almost certainly detonate it.
I purified it by washing with water, then recrystalising twice from pure methanol with a bit of Na2CO3 added, then twice from pure methanol, and drying at 40*C.
the freshmaker
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posted 06-03-2001 05:56 AM
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It sounds like some really good stuff!
When you mix it with NH4NO3, isn't it also getting more powerfull?
Will ONS/NH4NO3 mix also detonate from a flashcharge?
How dangerous is it to handle it?
(I know ALL explosives are dangerous -in some way or another!)
How sensitive is it compared with Tetryl?
I will make some ONS in my dreams in next week, so if anyone have some tips or warn's please tell me!
Thanks again!
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Mr Cool
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posted 06-03-2001 06:06 AM
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Mixing with NH4NO3 might improve power by using up all of the fuel available, but ONS is more powerful thn NH4NO3.
The mixture will probably detonate from flash, but I've never tried it.
Treat it like a very dangerous primary (that's how I treat all explosives!), this will make sure you don't knock it too hard or anything. I'd recommend not handling it too much, since I don't really know how unpredictable it is. I'd guess it was a lot more sensitive than tetryl, but I haven't compared them.
the freshmaker
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posted 06-03-2001 07:02 AM
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Sucrose octonitrate. ONS
DoV: 6500 m/s (approximately)
spec. volume of gas: ?
Traulz test: 296cm3
impact sensitivity: ? (2kg - 30cm)
friction -- : ?
melting point: ?
Can someone fill in the gabs?
Have anyone else than Mr.cool tried this explosive? what about you PHILOU?
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Mr Cool
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posted 06-03-2001 08:14 AM
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Melting point 85.5*C
Impact sensitivity between 20 and 30cm with 2kg weight, although my hammer weighs about 2kg, and when dropped on a few granules of ONS it detonated from 20cm. It wasn't just a puff like the extract at the top of the thread says. Maybe this is an indication of impurity?
Anthony
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posted 06-03-2001 12:00 PM
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ONS sounds great I'm going to have to give it a go with the H2SO4/NO3 method, what kind of ratios would you need with this method?
the freshmaker
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posted 06-04-2001 05:11 AM
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Anthony please post your results when they are ready. Have you got the ratios? Does anybody have the ratios for H2SO4/NO3 for making ONS?
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Mr Cool
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posted 06-04-2001 01:08 PM
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Just work out how much H2SO4 and XNO3 are needed to make 75 grams of HNO3, and mix these and use them as the HNO3. You might need to add more H2SO4 to dissolve your nitrate (use NH4NO3).
Anthony
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posted 06-04-2001 06:02 PM
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OK, this is something I should really know, so please bear with me as I try to work this out...
RAM of 1 molecule of HNO3 would be 1x1 1x14 3x16 = 63
For one molecule of HNO3 you'd need one molecule of NH4NO3 to supply the NO3 and 0.5 molecules of H2SO4 to supply the H.
So you should need twice as many molecules of NH4NO3 to H2SO4.
RAM of NH4NO3 = 2x14 4x1 3x16 = 80
RAM of H2SO4 = 2x1 1x32 4x16 = 98
80/63 = 1.27
98/63 = 1.55
75gm x 1.55 = 116gm/2 = 58gm H2SO4
75gm x 1.27 = 95gm NH4NO3
So I reckon 95gm NH4NO3 and 58gm H2SO4 to make 75gm HNO3. Was I even close?
the freshmaker
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posted 06-05-2001 05:04 AM
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Nice, Anthony!
One more question: When detonating ONS with flashpowder is it then because of the incredible heat OR the (small) shockwave?
Mr Cool
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posted 06-05-2001 05:36 AM
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I suspect that it's the very rapid rise to a very high temperature, although I haven't actually done it.
Anyone else got any results yet?
Anthony
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posted 06-05-2001 02:16 PM
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If someone can confirm/correct me on the H2SO4/NH4NO3 ratio I'll try it tomorrow.
Mr Cool
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posted 06-05-2001 02:29 PM
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Looks good to me.
Has the font/layout changed, or is it just my computer?
Mr Cool
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posted 06-05-2001 03:57 PM
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It was just my computer
Anthony
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posted 06-06-2001 02:33 PM
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I couldn't do it today as I realised that I didn't have any ice so I'll try it tomorrow.
One question though, does the NH4NO3/H2SO4 mix just replave the 50ml HNO3 in the above procedure? In that you add the sucrose to the NH4NO3/H2SO4 and then drip in 55ml H2SO4?
Mr Cool
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posted 06-06-2001 04:55 PM
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That's right, or drip H2SO4 into a mixture of the sugar and the NH4NO3. But you will need 55 mL of H2SO4, and however much is needed for the NH4NO3/H2SO4.
Who needs ice when you have NH4NO3 and water? You can get down to about -15*C with dry, powdered NH4NO3 and the right amount of water!
the freshmaker
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posted 06-07-2001 05:44 PM
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If some of you guys have made ONS could you please post the exactly method, how much acid, result etc. That would be just perfect!!
Thanx!!
Anthony
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posted 06-07-2001 07:16 PM
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I tried it today, I mixed the NH4NO3 with the H2SO4 in an ice bath, it all dissolved (amazingly) but when it cooled down it became very thick, like a solid mass. I out the reaction vessel in the ice bath in the fridge to assist cooling. Came back a bit later, shit, the ice bath has tipped and water has flooded the reaction vessel - nooo! I managed to tip up the beaker upside and all the water ran out but the NH4NO3/H2SO4 stayed still. I realised I had nothing to loose so proceeded anyway, a stir turned the reactants back into a very thick liquid, I didn't know how much water they'd absorbed but hoped the H2SO4 I was about to add would soak up any excess water. I stirred in the sugar with no noticable reaction. I could be bothered to drip the H2SO4 in so I stirred it in three portions leaving to cool for about 10mins inbetween, temperature stayed below 30*C (oops). I then put it in the fridge and shall look at it tomorrow. The solution was kinda of a yellow colour at the end.
All in all, a pretty botched job
Next time I'll mix the NH4NO3 and sugar dry and then add all the H2SO4 in one go to avoid the super-thick solution.
Mr Cool
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posted 06-08-2001 07:56 AM
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If you're gonna add all the acid in one go, cool it first to stop it getting too hot. Excess heat can cause a shit load of NOx and no product.
PHILOU Zrealone
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posted 06-08-2001 10:04 AM
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I have tried 7 years ago a weird mixture that is called vigorine!
A mix of KNO3/HNO3/Suggar and cellulose!
The mix was evolving red fumes and was like a thick paste; when a portion of it was light, it burned fearcely and flew accross the air!
The problem with this mix is that it needs to be used fast since free HNO3 in a suggar/cellulose matrix is very prompt to self ignite!
On a theorical level it is a good mix (works already with HNO3(70%)!I suspect the final mix with pure HNO3 to contain nitrosuggar,nitrocellulose and some KNO3 to improve the burning and the OB!
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Anthony
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posted 06-08-2001 01:47 PM
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I did wonder whether temps above 0*C would prevent ONS forming, or whether it was just a safety guide.
The result was a thick yellow goo, about the same colour as TNP. As ONS is not soluble I poured the lot into approx 500ml cool water which dissolved the AN prill "shells" (didn't grind the AN enough). I poured this through a paper filter and got didly squat so down the drain with the lot of it!
I didn't expect it to work considering the fuck ups. I think real HNO3 would easier to work with than the NH4NO3/H2SO4 shit.
the freshmaker
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posted 06-10-2001 11:22 AM
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No one have succeded yet? I think I will give it a go with my 70% HNO3. Shouldn't it be possible? If I used the same method as for making MHN how much 70% HNO3 should I be using?
fightclub
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posted 06-10-2001 05:18 PM
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That data above is from T.Davis's book, the references are missing.
Can't forget the data of Will and Lenze as shown in Urbanski for Sacharose nitrate (sucrose octonitrate!):
* Melt.point. 85 deg.C.
* Decomposition point: 135 deg.C.
* Weight loss Stability at 50 deg.C.: 11%
after 3 days --This means that for ex, 10g
after 3 days at this temp. will leave you
with 1.1g.
Also the other data in Urbanski referenced:
Monasterski (1933) examined explosive characterisitics of nitrosugars, and for nitrosucrose gave:
* Heat of explosion: 950 cal/g
* Lead block test: 300 ccm/10g
* Shock-sensitivity: 20 cm (2kg wt.)
Ref.: Monasterski S., Z. ges. Schiess- u. Sprengstoffw. 28, 349 (1933). --The same ref. as in Davis.
I calculated the detonation velocity of nitrosucrose: 7350m/s @ 1.6g/cc. Personally,
I think it is more in between 7000-8000 m/s.
(!)Be careful with sucrose nitrate it is highly unstable in acidic environment and will decompose exothermically in a chain reaction releasing heat energy and possibly exploding. It is absolutley necessary to keep the mixture cool with an ice bath during nitration, even after nitration the solution if left standing (bad idea) will decompose in an uncontrollable violent gas reaction involving nitrogen oxides and lots of heat!
T. Davis should have been(w/ the two refenc.):
Nitrosucrose (Sucrose octonitrate),
C12H1403 (ONO2)
The nitration of cane sugar(.sup. 69, 73), yields sucrose octonitrate, white glistening needles, ----etc.----
.sup.69 Will and Lenze, Ber., 31, 68 (1898).
.sup.73 Hoffman and Hawse, J. Am. Chem. Soc., 41, 235 (1919). Monasterski, Z. ges. Schiess- u. Sprengstoffw. 28, 349 (1933). Wyler, U.S. Pats. 2,081,161 (1938), 2,105,390 (1938), 2,165,435 (1939).
Anthony
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posted 06-10-2001 05:25 PM
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I'm not expert, but if you should still need 75gm of HNO3, which at 70% conc (density 1.41gm/cc) is 75gm/1.41 = 53ml
Mr Cool
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posted 06-11-2001 01:37 PM
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Mine didn't decompose that fast. Maybe it's not fully nitrated?
I don't think it will work well with 70% HNO3. Better to concentrate it, or use H2SO4/NaNO3 etc.
PHILOU Zrealone
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posted 06-12-2001 04:19 AM
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Fightclub:
11% weightloss at 50C in three days will lead to 8.9g from 10g starting material and a weight loss of 1.1g!
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Microtek
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posted 06-12-2001 10:17 AM
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A note on H2SO4/NH4NO3 mixes: It doesn't matter that it becomes solid when cooled; if anything it makes it less prone to runaway nitration as it mixes more slowly.
Just crush up the mix with the thermometer before you start adding the sucrose ( or mannitol or whatever ), and knead the mix during addition instead of stirring.
Mr Cool
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posted 06-12-2001 12:41 PM
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D'oh! Stupid of me. Mine didn't decompose that fast since it wasn't at 50*C!
Also, 11% loss, not 11% remaining, sounds a lot more realistic.
Anyone else made any yet?
the freshmaker
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posted 06-15-2001 04:21 PM
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I'm sorry but my I think my brain is dead... (maybe because of our weedparty last week)
Could someone be so friendly to post a complete recipe for making ONS with the H2SO4/NH4NO3 method, including all acid/nitrate ratios etc.
Thanks alot to everyone who post!!
the freshmaker
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posted 06-17-2001 09:07 AM
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Please!??? BTW is it Octo- or Octanitrate?
Mr Cool
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posted 06-17-2001 09:20 AM
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I've never done it that way, but I'm sure you could just follow the recipe for MHN with H2SO4/NH4NO3, in the MHN thread.
Anthony
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posted 06-17-2001 09:38 AM
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Briefly:
*Mix 95gm NH4NO3and 58gm H2SO4
*cool to *0C
*Add 10g sucrose
*Drip in 55ml H2So4
*Ensure temp stays sub 0*C
*Pour into 200ml water and crushed ice
*filter out ONS
I presume the last two steps will work as ONS is insoluble in water and any solid NH4NO3 will dissolve.
Both the NH4NO3 and sucrose should be dried before use.
Mr Cool
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posted 06-17-2001 09:42 AM
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..and then wash with water, recrystalise from methanol with NaHCO3, then from pure methanol.
the freshmaker
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posted 06-17-2001 10:36 AM
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Thanks guy's!!
Q
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posted 06-19-2001 04:54 PM
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Is it possible to mix all the NH4NO3+H2SO4 at the start to make a nitrating 'mix',cool it and then add the sugar?
Anthony
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posted 06-19-2001 09:31 PM
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I personally don't see why not, as long as the sucrose is added very slowly. Worth checking with MrCool first though
Mr Cool
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posted 06-20-2001 08:22 AM
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...or someone that actually knows what they're talking about! I just dreamed this, remember?!
I can't see any reason why that wouldn't work. Try a small batch, and see what happens.
Q
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posted 06-20-2001 04:15 PM
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I'll do that,but first I need to concentrate my H2SO4.Boiling is the normal way but since Encarta says it solidifies below 10*C could I freeze it to about 5*C and remove whatever liquid remains.I tried this with some old yellow non-fuming H2SO4{frozen to -10*C}except nothing solidified,it must have been contaminated.I can tons of battery acid
{thats about 40%,right}tomorrow.
One more question,would the H2SO4 not dehydrate the sugar into carbon before it had a chance to get nitrated?Just a thought.
frostfire
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posted 06-20-2001 07:01 PM
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whaaa?
H2SO4 solidify at 10 C, are you sure of that? it might be 10 Kelvin
Mr Cool
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posted 06-21-2001 09:27 AM
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It won't be 10*K, maybe 10*F. For all I know it might be 10*C, I've never tried.
The only worry I have about mixing all the nitrating mixture and adding the sucrose to it is that it might get dehydrated, but you might as well try it. It's not as if sugar is a great rarity!
the freshmaker
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posted 06-21-2001 10:41 AM
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How long time does the nitrating-proces of the sucrose need, to get fully nitrated?
[This message has been edited by the freshmaker (edited June 21, 2001).]
10fingers
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posted 06-21-2001 12:01 PM
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Q, pure sulfuric acid freezes at 10 degrees C. If it has water in it the freezing point lowers quite a bit. It wouldn't be much use in car batteries in the winter if it froze.
Q
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posted 06-21-2001 12:11 PM
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OK,I'll boil it down so.
Q
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posted 06-21-2001 05:49 PM
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I decided to try NC with my boiled down battery acid,and I appear to have failed.I boiled it down from 250ml to 90ml by putting it on a cooker ring at full blast.The result was a non-fuming,non-oily liquid.I've worked with conc. H2SO4 before and boiled down battery acid does not seem to the answer.Any pointers on where I'm going wrong would be greatly appreciated.Surely other people have had the same problem and overcome it.Thanks.
fightclub
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posted 06-21-2001 07:45 PM
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Yeah PHILOU Z., that is what I meant sorry for the mix up.
Mr Cool
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posted 06-22-2001 01:31 PM
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When boiling down H2SO4, it should fume strongly (while hot), and if you boil it then it'll certainly be 98%+. It boils at about 327*C IIRC. The cold acid doesn't fume, but it's quite thick, like a thin sugar syrup, and noticably heavier than water. Also, when I boil down drain cleaner, it makes those little "fingers" of liquid on the side of the container, like v. conc. HNO3 or whiskey. This might be an impurity I suppose.
Q
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posted 06-22-2001 02:48 PM
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One more question,for the nitration of glycerine is a high H2SO4 conc. needed because in a recipe given in another thread 4g of AN is added to 6ml of H2SO4.Would this not use up a bit much of the H2SO4 to create HNO3?My boiled down acid was not syrupy.Could I be heating it up to high allow the H2SO4 to evaporate?I didn't think I boiled it all that hard?
Anthony
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posted 06-22-2001 03:06 PM
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Q it shouldn't be a thick syrup, but you should notice it's thicker than water in the way it pours. It should still slosh.
If you did overheat the H2SO4 and boil off some of the H2SO4, it would definitely be at 98% as all the water would have been long gone by that temp. you'd just be reducing the amount of conc H2SO4 you've got.
4gm NH4NO3 to 6ml H2SO4 (that's 11gm) will leave plenty of H2SO4 left to soak up water produced during the nitration. Since tolo much water kills nitrations, having water to start with in low conc H2SO4 is going to reduced yields.
MrCool, surely you don't need to heat the H2SO4 to 300C+? Wouldn't over 100C allow the water to boil off without decomposing any of the H2SO4.
BTW BP of H2SO4 = 290C (Mega's page)
Q
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posted 06-22-2001 04:44 PM
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thanks for the input.
sorry to constantly be asking questions,but,
my h2so4/nh4no3 mixes fume,this is the hno3produced right not NO2 because I added the AN to quikly?
Also will high temps. in the production of NC
help or hinder nitration?Are low temps. purely to prevent runaway nitration or will some of the NC decompose at these high temps?
Thanks.
Q
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posted 06-22-2001 05:35 PM
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OK,I'm havin' serious problems makin' NC.Firstly I dissolved 3.9g NH4NO3 in 20ml of sulphuric acid.The solution goes cloudy and fumes{fumes smell like HNO3}Temp. rises to about 30'C.I then add enough cotton to soak up most of the mixture.No change in temp. is observed.After about 40mins cotton is slightly mushy and yellowed somewhat and smells strongly of HNO3.I then take out the cotton and put it in some water to wash it,but,the acid within the cotton reacts with the water,gets extremly hot and appears to dissolve ih the water[or divide up extremly finely}.On another occasion using the exact same procedure I sqeezed the cotton of most of its acid and put it in a jar with a little water.The cotton again heats up only this time produces lots of NO2 and appears to break down completely.Both proce. used pure and dry AN and 98% lab grade H2SO4.WTF is going on?
John456
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posted 06-23-2001 12:19 AM
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It sounds like when you add your NC to the water it might be getting hot enough to decompose it. Try putting your NC in a bowl of crushed ice after you finish nitrating it. The NC will heat up the ice it touches, melting the rest, but it will remain at a low temperature by the time all the acid is absorbed. Another possibility is that your using synthetic "cotton".
Q
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posted 06-24-2001 09:10 AM
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Well I tried ONS yesterday,following the procedure exept the temp rose to 10*C at one point,but otherwise averaged about 4*C.Anyway on mixing the acid/sugar solution with the water,while stirring,a brown doughlike scum formed on the surface and the rest of the solution was cloudy white.I left it over night to settle and a layer of extremely fine white crystals seemed to collect.I am now filtering them out.This sound normal so far?
Mr Cool
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posted 06-24-2001 09:22 AM
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Fine white precipitate sounds good, but I never got a dough-like brown mess when using HNO3. Sounds like you got patially dehydrated sugar (and perhaps partially nitrated).
I'm sure I read somewhere that H2SO4 boils at 327*C. In fact I KNOW I did, but it could have been a mistake. One of them has to be! And no, you don't need to heat it to it's boiling point to get it concentrated, but it's not necessarily true that heating to 100*C will drive off all the water. 69% HNO3 boils at over 100*C, which is over the bp's of both water and HNO3.
Anthony
Moderator
Posts: 2306
From: England
Registered: SEP 2000
posted 06-24-2001 06:32 PM
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Whichever BP is right they're both much higher than water.
I did wonder whether the boiling point would be higher than 100*C. I think I heated to about 130*C (thermometer only goes to 120) there was a vapour coming off, I presume this could only be water?
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-25-2001 04:30 PM
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If it's quite thick then at least some of it is sulphuric acid vapour. Water vapour condenses at a lower temperature, and therefore not just above the liquid like the H2SO4 vapour will.
Q
New Member
Posts: 19
From: ireland
Registered: JUN 2001
posted 06-26-2001 11:22 AM
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So your telling me if I boil it to one third its original volume it will become syrupy because I tried it the last time with no joy and afterwards white crystals appeared to form[slight impurity,I'd say].How -exactly do conc. your acid?
Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted 06-26-2001 12:44 PM
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Are you using battery acid? Sounds like you have lead sulphate or something if you are, forming crystals. Make sure you get the acid out of a CHARGED battery.
It won't get syrupy, but it's noticably thicker than water. Try putting a drop of it onto some paper - if it's strong, then it'll quickly turn the paper into carbon.