megalomania
June 8th, 2003, 01:02 PM
TylerDurden
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posted 04-24-2001 11:24 AM
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I needed a method to get NM out of race fuel mixtures (methanol with nitromethane). I know that you can distill the mixture under reduced pressure. Another method is to add smokeless powder to gel the NM (with the nitrocellulose).
But I found a new and very simple method: just add a lot of water to the race fuel mixture. The water dissolves in the methanol and NM sinks to the bottom because it no longer can dissolve in the methanol. The only disadvantage is that water also dissolves a little in NM (to about 2.5%). So this NM should be "dried" before it can be used in ANNM explosives. Maybe this can be done simply by filtering the "wet" NM through a little dry AN. Or maybe just a little AN can be added.
Do you guys have any comments on this method? Or any suggestions for improvements?
And I thought of another method: just letting the race fuel evaporate overnight at room temperature. Because methanol will evaporate faster than NM. It would be "distilling" at room temperature, but what kind of mixture would result? Will it lead to a mixture with high(er) NM content? (Tim Lewis let's his distilled NM stand overnight to let the remaining methanol evaporate which results in a 80-90% mixture. That's where I got the idea from). Is it possible?
[This message has been edited by TylerDurden (edited April 24, 2001).]
Anthony
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posted 04-24-2001 02:51 PM
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I tried vacuum distilling model fuel (20% NM, 20% castor oil, 60% methanol) the other day.
I basically follwed the instructions in KIPE2, it claims to heat the retort to 50*C, I couldn't get an noticeable amount of vapour being produced untill the temperature was raised to 65*C. The process was very slow and I only colletced a few ml of purified fuel, although my collection vessel may not have been cold enough.
I left the purified fuel to stand over night, nearly all of it evaporated (room temp was about 15*C), what was left would not burn. An oily residue was also in the evaporating dish - probably castor oil.
Tyler, your method sounds very easy, but won't the castor oil also settle out to the bottom? Maybe if the NM and castor oil formed noticable layers then the NM could be sucked off with a pipette. Could NM be dried by placing in a dessicator with H2SO4 or NaOH?
Leaving the fuel to evaporate would probably leave a mixture of NM and castor oil an you'd probably loose some of the NM to evaporation.
pete
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posted 04-24-2001 02:56 PM
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I have tried to do this myself, never worked. It should do but it didn't, the problem that i experienced was that i couldn't separate the nitromethane from the water as the oils in the nitromethane stained the water a green colour which i could not get rid of. I also added NaCl to the water before i mixed it with the fuel, as this reduces nitormethane solvation. I know that the nitromethane had separated out as if you but a rod in the mixture it came out covered in nitromethane.
Anthony
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posted 04-24-2001 03:34 PM
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If you knew the nitromethane was seperating at the bottom of the solution, couldn't you just drain it off from a tap at the bottom of the vessel?
fightclub
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posted 04-25-2001 02:00 AM
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Tyler Durden is a great man.
PHILOU Zrealone
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posted 04-25-2001 05:22 AM
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THus your problem is only to separate NM from methanol and castor oil!
1)With an exces of water, you would take methanol away because NM is not very soluble in water ( especially if there is some acid; just add a little H2SO4 or whatever acidic), shake and decantate ; you collect the NM and the castor oil. Yes you loose a little NM but not that much.
2)With evaporation at room temp, you loose both NM and methanol since both are very volatile! Maybe you increase a little the % of NM but you loose much more NM than in the first process....but you stil have castor oil!
3)By distillation is one of the best ways; just add water to the mix like 0.5Vol/1Vol mix and distill at ambiant temp whit a cooling flask!
-First the methanol will come out because it has a boiling point of 65-67C...that's what those guys making a distillation has obtained...it burns but it is not NM!!!!So disgard everything passing under 80C(or keep if you want methanol to make methanol nitrate or as a solvant).
-Then comes water and NM between 95C and 110C
Since NM is not soluble in water, in the cooling flask you should see a turbidity and a decantation; one of the layer is water (upper) and the other is NM (pure).
-In the bottom of your distillating flask will remain castor oil with very little NM and water since it has a much higher boiling point...it will burn before distilling so stop when you get white fumes inside the distilling flask!
Under reduced pressure the same order of outcome for the products, same procedure but temperatures are lower...I don't know them since it depends on the pressure!
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TylerDurden
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posted 04-25-2001 07:27 AM
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I didn't think about the castor oil because the race fuel I used didn't contain castor oil (or at least it wasn't mentioned on the label). But it would indeed settle down with the NM (or does the castor oil float on top of the water layer like some other oils? in that case castor oil is no problem at all). But if it settles down dissolved in/with NM that would only be a problem if the race fuel contains a lot of it. But I thought that when castor oil is used it would be in the range of 1-2%. 20% seems to me a very high percentage but if so it would render the very simple method useless. Because the result would be a NM/castor oil mixture (50/50).
By the way, I would not recommend adding acid to the water because it will sensitize the NM (making it unstable). The use of NaCl or acid is also not necessary because it would reduce the amount of methanol that will dissolve as well.
And drying the resulting NM (which you get by just decanting the water off or letting the NM drip out of the bottom of the container) with AN seems to me the most handy. You need AN anyway so why use other chemicals.
TylerDurden
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posted 04-25-2001 08:15 AM
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I was wrong about the castor oil content. It is indeed used in 10-20% range. So this method would only be usefull if the amount of NM exceeds the amount of castor oil a lot. For example a mixture of 10% castor oil, 50% NM and 40% methanol. This would result in a mixture with about 20% oil. Maybe this can be used for ANNM explosives. But I'm not sure.
PHILOU Zrealone
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posted 04-25-2001 09:25 AM
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My guess is that castor oil is almost fully soluble in NM (or the contrary!) that means that no way to separate them by droping in water!Only distillation can help!
NM sensitised by acids??? I have never seen this in any book I have on nitrocompounds!
What I know is that the solubility comes from a partial decomposition into nitronate...nitronic acid is soluble slightly in water and its solubility decreases when there is a trace of acid in the media!
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Anthony
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posted 04-25-2001 03:36 PM
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I poured some of the NM fuel I had into water. It immediately turned cloudy white and a thick layer of yellow castor oil went stright to the top. I've left it so hopefull the NM will settle out at the bottom.
Thanks philou, I will try again soon. I had presumed that you needed to distill the NM under vacuum or it would decompose from the heat. I was using a pretty strong vacuum (for re-gassing fridges). I will do it without the vacuum next time so that I can tell when the different fractions are coming off by reading the temp. I'll also make a condensor instead of using a cooled flask.
PHILOU Zrealone
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posted 04-26-2001 07:15 AM
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Yes there is no need of vacuum for the distillation of NM; no risks of explosion! You don't even need a glass rod distillator; a simple wooden (i guess its is that in french we say "liege" a kind of agglomerated wooden foam that is used to close wine bottles)stop rod will do the thing since NM is non reactive substance (not acidic like HNO3) towards wood. The thermometer must be placed near (in front of) the top of the cooler/condenser pipe so it gives the temp of the gas that is condensing there!
Don't put the thermometer in the mother liquor since that has a higher temp (overheated castor oil/water mix)!!!
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Anthony
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posted 04-26-2001 04:43 PM
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In English it is "cork"
I just tried again with a cork bung with a glass tube through it and then some PVC hose leading to a cooled flask (I found the vapour condensed in the tube as soon as it left the retort so no need for a condensor). I had the thermometer in the heating water bath for the retort, I know it's not very accurate but it was all I could do. I had the methanol coming off nicely but didn't have time to get it all out.
I got some rubber bungs for wine making which fit my thermometer with a short piece of pvc hose over the thermometer to make it fit tightly in the bung. I managed to make a small (approx 3mm) parallel to the original hole for the glass tubing (I only have small diameter stuff at the moment). So now I can have a thermometer in there to read the vapour temperature. Only trouble is that the bung is far too big to fit into the bottles I use for a retort. So I'll punch a hole in a metal jar lid and use the jar as a retort.
This stuff sure is hard when you don't have proper lab supplies!
The NM fuel in water: it is still cloudy white (caused by the methanol) and I cannot see any kind of seperation that would be the nitromethane. So I think it's not going to work.
TylerDurden
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posted 04-27-2001 04:56 AM
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Philou, I didn't say you could separate NM from castor oil with this method. I said you can separate NM from the methanol by adding water to the race fuel (about as much as the amount of fuel, and not by pouring the fuel in a lot of water). The mixture will turn cloudy white and letting it stand 10 minutes results in a layer of NM at the bottom.
Now, if castor oil is present it will most likely settle down with (dissolved in) the NM (or maybe float on top). And if the amount of castor oil is low you get a mixture of NM/castor oil that can be used (after drying) for explosives.
By the way you can separate the NM from the castor oil by adding pingpong balls (celluloid) this will gel the NM (adding PPB's directly to the race fuel will not work becuase celluloid dissolves in methanol. If you want to gel NM out of race fuel you need guncotton/smokeless powder).
And NM is sensitized by acids! NM is sensitized by almost anything! alkalies, acids, oxidizing agents, reducing agents, and lots more.
And the advantage of this method is that it's EASY. You only need water. Of course destillation yields a better, purer product without the castor oil but you need glassware , heating source, thermometer, and time. If you have it I would recommend distilling race fuel. And remember that castor oil is probably just as good as fuel oil for producing ANFO, so a bit of castor oil in NM will probably have no negative effect when used to make the ANNM explosive.
[This message has been edited by TylerDurden (edited April 27, 2001).]
[This message has been edited by TylerDurden (edited April 27, 2001).]
TylerDurden
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posted 05-08-2001 06:44 AM
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Anthony, I think the yellow layer at the top is NM with castor oil. Since no layer is formed at the bottom and NM dissolves castor oil. So the mixture of NM/castor oil in this case is lighter than water/methanol and therefor floats on top.
The race fuel I used resulted in the NM settling down (probably with some castor oil), but I think it depends on the ratio of NM/castor oil wether it settles down or floats on top. It's impossible that NM stays dissolved in the methanol/water mixture.
So you ended up with a 50/50 mixture of NM/castor oil. This is probably not very usefull but you can get NM out if the mixture with celluloid. And if you use race fuels with less castor oil the resulting mixture contains mostly NM and can directly be used in ANNM explosives.
Anthony
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posted 05-08-2001 02:25 PM
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Maybe it does float with castor oil dissolved in it, I don't know. I've got the seperation by distillation sorted now some I'm not really worrying about it. An easy way to tell what fraction is coming off is to drop a drop of the distilate into water, if it's methanol it'll form a little white cloud. If it's NM it'll sink to the bottom in a little ball.
TylerDurden
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posted 05-09-2001 06:30 AM
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Yes, distillation is by far the best method (if you got the glassware and thermometer and stuff). But I was just wondering about an easier way to extract NM, so...
By the way, if you distil race fuel you will end up with a NM/methanol mixture (80-90%)(depending on the quality of your distillation equipment: with bad equipment it's impossible to separate the two and you'll end up with a mixture with a lot of methanol) because the boiling points of methanol and NM are too close together. And methanol has some serious disadvantages: it's poisonous and atracts water from the air quite quickly (a drop of race fuel spilled will turn cloudy white within a short time because of the water that is absorbed from the air!).
But if you would distil the NM/castor oil mixture that you get after adding water to race fuel, you would get PURE NM without methanol and without castor oil! (and the distillation is much easier and can be done with some improvised equipment since you just have to evaporate the NM and somehow cool it and collect it).
So my method proves to be handy after all: it will give you a route to pure NM without methanol (or a usefull NM/castor oil mixture if you don't want to distill).
"one can make all kinds of explosives using a few simple household items"
[This message has been edited by TylerDurden (edited May 09, 2001).]
[This message has been edited by TylerDurden (edited May 09, 2001).]
Anthony
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posted 05-09-2001 03:48 PM
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I agree with what you're saying but I'd hardly say it's difficult or impossible to seperate NM from methanol with improvised equipment! Methanol B.P = 65*C NM = 101*C that's a fair amount of difference. I usually discard the first NM drawn off as it could contain the last dregs of methanol.
If you add race fuel to water and draw off the NM/castor oil layer and try to distil it, you're going to have water in your "pure" NM.
TylerDurden
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posted 05-10-2001 05:15 AM
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Yes, you're right, the NM would contain water (max. 2.5%). But it's easy to dry, with some AN. And then you have 99% NM.
Besides, your resulting NM/methanol mixture will probably also contain water since the methanol atracts it from the air (before or during the distillation or when in the receiving flask with NM, or afterwards). Maybe that's why it should be done under reduced pressure? And stored airtight.
Even if you dry it, you would have a hydroscopic NM/methanol mixture of max 90%.
TylerDurden
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posted 05-14-2001 11:46 AM
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Any comments on that? Getting water in the NM/methanol mixture would be a problem I think.
Anthony
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posted 05-14-2001 02:17 PM
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OK, I'll try both methods and compare the results.
TylerDurden
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posted 05-15-2001 06:03 AM
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OK, thanks. Let me know.
TylerDurden
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posted 05-24-2001 07:10 AM
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Don't want to rush you, but are there any results already?
Anthony
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posted 05-24-2001 03:02 PM
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Ah yes, my conclusion: Bollocks to the both of them I'm going to just buy some pure NM.
You're right, seperating NM from methanol is difficult having to work at low temperatures to stop them both coming off takes forever.
Seperating the castor oil collected from pouring the fuel into water seemed to work, except the "NM" extracted didn't smell right, dissolved in water and was flame retardant!
TylerDurden
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posted 05-25-2001 06:16 AM
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I can accept that my idea doesn't work. Sometimes a perfectly good idea turns out to be bullshit. But what I don't understand is WHY it doesn't work. And I can't stand that. So does anyone have an explanation for this result??
Maybe the NM is still dissolved in the methanol/water mixture (and makes it turn cloudy white)? But this seems unlikely. It would prefer the castor oil wouldn't it? And it can't stay all in the water/methanol can it?
And if the resulting "NM" is not nitromethane (and it clearly isn't) what the fuck is it then? And how can it dissolve in water when it is distilled from the layer that is separated by the water?!
This makes me crazy. So please help me.
Teck
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posted 05-27-2001 02:57 AM
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why not just buy the NM its $30 for a gallon at http://www.worldwideracingfuels.com/products/fuel.htm
ezekiel
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posted 05-27-2001 06:50 AM
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Nitromethane boils at 101'C, and is soluable in water.
Methanol boils at 64.6'C, and is miscible in water.
Thus bisolvent extraction with water won't work, or at least won't work very well at all.
Much better is distilation. You don't even need one of those expensiv vacuum pumps. The difference in Bps is so great that it should be piss easy.
Admittedly I have never done it, and certain parts of the fuel may piss around with the boiling points.
Step by step guide:
Boil of methanol at 65'C
Distill off nitromethane at 102'C, discarding residue.
Dry the distillate with calcium chloride to remove any water picked up.
Filter... you now have hopefully pure-ish, 0% water Nitromethane.
Remember to use a closed flame, or oil bath or double boiler for heating as both NM and Methanol are flammable.
Anthony
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posted 05-27-2001 10:18 AM
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Ezekiel, if you heat to 65*C you get left with nothing but the castor oil.
ezekiel
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posted 05-27-2001 05:29 PM
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I don't know what to say: nitromethane boils at 101'C.
Is this s general consensus opinion or just anthony's experience?
Anthony
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posted 05-27-2001 07:58 PM
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I don't claim to know what I'm doing, I'm learning as I go along. I don't see why NM shouldn't vaporise and condense at 65*C, afterall, BP of water is 100*C and it evaporates at room temperature.
TylerDurden
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posted 05-28-2001 06:02 AM
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Nitromethane isn't soluable in water! The solubility in water is about 10%. It is of course completely miscible with methanol. And about 2.5 % of water will dissolve in NM.
And water and methanol are also completely miscible. So far the facts.
Now what the effects are of adding water to race fuel I'm not quite sure anymore (I assumed that nitromethane was totally insoluble in water). The amount of water is probably important just like the percentage of NM in the race fuel.
If to 100 ml of race fuel (20%NM, 20% castor oil, 60 methanol) 100 ml of water is added what happens? Maybe the NM stays dissolved partly in the methanol partly in the water and only the castor oil separates. Who knows?
Maybe using another solvent is helpful?
By the way, you should distil under reduced pressure because otherwise the methanol attracts water from the air.
The resulting NM/methanol (80-90% NM) mixture you get after distillation has the same problem. (Distillation won't lead to 100% pure NM!)
[This message has been edited by TylerDurden (edited May 28, 2001).]
CodeMason
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posted 05-28-2001 06:13 AM
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To get the water out of a mix of NM and water, try chilling it to 0ºC. NM can remain liquid at temperatures as low as -25ºC, so the water will become ice but not the NM. All you'd have to do then is filter out the ice.
gcic
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posted 05-28-2001 08:36 AM
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Isn`t it a danger to cool the nitromethane to 0°? Cooling down nitroglycerine is also dangerous, so I could imagine, that NM probably behaves in the same manner(?)
PHILOU Zrealone
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posted 05-28-2001 11:00 AM
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No because nitromethane is a nitrocompound while nitroglycerine is a nitrate ester...and thus is much more sensitive and high detonating explosive!
Nitroglycerine is actually propantriol trinitrate ester!
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gcic
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posted 05-28-2001 12:50 PM
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Yes, I know what nitroglycerine is. Philou, could you tell me, please, what is exactly responsible for the increasing sensitivity of very cold NG? I mean, what chemical background does that have?
10fingers
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posted 05-28-2001 01:26 PM
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Actually, nitroglycerine is less sensitive when cold.
Mr Cool
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posted 05-28-2001 02:25 PM
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I think it's just friction between crystals of frozen NG. Also, crystaline explosives are always more sensitive than amorphous forms (look at crystaline TNT and quickly cooled cast TNT).
gcic
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posted 05-28-2001 05:22 PM
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ah yes, thx. That sounds like a reasonable explanation. Do you know, at which temperature nitroglycerin starts freezing?
My book says +10°C, but I can`t imagine this.
Well, let`s better close this topic. It has nothing to do with the original discussion anymore.
PHILOU Zrealone
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posted 05-29-2001 11:08 AM
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Actually it is irregularities in the cristals that generates such a sensitivity (innerstresses)! Also since when frozen the density is higher for most of the substances (water is an exception yes; ice of other products goes to the bottom of the fluid!), then the VOD is as high as 8000m/s!
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Mr Cool
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posted 05-29-2001 11:21 AM
Oh yes, stresses. Like when big crystals of lead azide form if you don't add dextrin or whatever, and they spontaneously detonate. And when AP sublimes and re-crystalises, forming vey sensitive crystals.
PHILOU Zrealone
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posted 05-30-2001 05:15 AM
Precisely!
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posted 04-24-2001 11:24 AM
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I needed a method to get NM out of race fuel mixtures (methanol with nitromethane). I know that you can distill the mixture under reduced pressure. Another method is to add smokeless powder to gel the NM (with the nitrocellulose).
But I found a new and very simple method: just add a lot of water to the race fuel mixture. The water dissolves in the methanol and NM sinks to the bottom because it no longer can dissolve in the methanol. The only disadvantage is that water also dissolves a little in NM (to about 2.5%). So this NM should be "dried" before it can be used in ANNM explosives. Maybe this can be done simply by filtering the "wet" NM through a little dry AN. Or maybe just a little AN can be added.
Do you guys have any comments on this method? Or any suggestions for improvements?
And I thought of another method: just letting the race fuel evaporate overnight at room temperature. Because methanol will evaporate faster than NM. It would be "distilling" at room temperature, but what kind of mixture would result? Will it lead to a mixture with high(er) NM content? (Tim Lewis let's his distilled NM stand overnight to let the remaining methanol evaporate which results in a 80-90% mixture. That's where I got the idea from). Is it possible?
[This message has been edited by TylerDurden (edited April 24, 2001).]
Anthony
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posted 04-24-2001 02:51 PM
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I tried vacuum distilling model fuel (20% NM, 20% castor oil, 60% methanol) the other day.
I basically follwed the instructions in KIPE2, it claims to heat the retort to 50*C, I couldn't get an noticeable amount of vapour being produced untill the temperature was raised to 65*C. The process was very slow and I only colletced a few ml of purified fuel, although my collection vessel may not have been cold enough.
I left the purified fuel to stand over night, nearly all of it evaporated (room temp was about 15*C), what was left would not burn. An oily residue was also in the evaporating dish - probably castor oil.
Tyler, your method sounds very easy, but won't the castor oil also settle out to the bottom? Maybe if the NM and castor oil formed noticable layers then the NM could be sucked off with a pipette. Could NM be dried by placing in a dessicator with H2SO4 or NaOH?
Leaving the fuel to evaporate would probably leave a mixture of NM and castor oil an you'd probably loose some of the NM to evaporation.
pete
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posted 04-24-2001 02:56 PM
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I have tried to do this myself, never worked. It should do but it didn't, the problem that i experienced was that i couldn't separate the nitromethane from the water as the oils in the nitromethane stained the water a green colour which i could not get rid of. I also added NaCl to the water before i mixed it with the fuel, as this reduces nitormethane solvation. I know that the nitromethane had separated out as if you but a rod in the mixture it came out covered in nitromethane.
Anthony
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posted 04-24-2001 03:34 PM
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If you knew the nitromethane was seperating at the bottom of the solution, couldn't you just drain it off from a tap at the bottom of the vessel?
fightclub
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posted 04-25-2001 02:00 AM
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Tyler Durden is a great man.
PHILOU Zrealone
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posted 04-25-2001 05:22 AM
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THus your problem is only to separate NM from methanol and castor oil!
1)With an exces of water, you would take methanol away because NM is not very soluble in water ( especially if there is some acid; just add a little H2SO4 or whatever acidic), shake and decantate ; you collect the NM and the castor oil. Yes you loose a little NM but not that much.
2)With evaporation at room temp, you loose both NM and methanol since both are very volatile! Maybe you increase a little the % of NM but you loose much more NM than in the first process....but you stil have castor oil!
3)By distillation is one of the best ways; just add water to the mix like 0.5Vol/1Vol mix and distill at ambiant temp whit a cooling flask!
-First the methanol will come out because it has a boiling point of 65-67C...that's what those guys making a distillation has obtained...it burns but it is not NM!!!!So disgard everything passing under 80C(or keep if you want methanol to make methanol nitrate or as a solvant).
-Then comes water and NM between 95C and 110C
Since NM is not soluble in water, in the cooling flask you should see a turbidity and a decantation; one of the layer is water (upper) and the other is NM (pure).
-In the bottom of your distillating flask will remain castor oil with very little NM and water since it has a much higher boiling point...it will burn before distilling so stop when you get white fumes inside the distilling flask!
Under reduced pressure the same order of outcome for the products, same procedure but temperatures are lower...I don't know them since it depends on the pressure!
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TylerDurden
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posted 04-25-2001 07:27 AM
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I didn't think about the castor oil because the race fuel I used didn't contain castor oil (or at least it wasn't mentioned on the label). But it would indeed settle down with the NM (or does the castor oil float on top of the water layer like some other oils? in that case castor oil is no problem at all). But if it settles down dissolved in/with NM that would only be a problem if the race fuel contains a lot of it. But I thought that when castor oil is used it would be in the range of 1-2%. 20% seems to me a very high percentage but if so it would render the very simple method useless. Because the result would be a NM/castor oil mixture (50/50).
By the way, I would not recommend adding acid to the water because it will sensitize the NM (making it unstable). The use of NaCl or acid is also not necessary because it would reduce the amount of methanol that will dissolve as well.
And drying the resulting NM (which you get by just decanting the water off or letting the NM drip out of the bottom of the container) with AN seems to me the most handy. You need AN anyway so why use other chemicals.
TylerDurden
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posted 04-25-2001 08:15 AM
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I was wrong about the castor oil content. It is indeed used in 10-20% range. So this method would only be usefull if the amount of NM exceeds the amount of castor oil a lot. For example a mixture of 10% castor oil, 50% NM and 40% methanol. This would result in a mixture with about 20% oil. Maybe this can be used for ANNM explosives. But I'm not sure.
PHILOU Zrealone
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posted 04-25-2001 09:25 AM
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My guess is that castor oil is almost fully soluble in NM (or the contrary!) that means that no way to separate them by droping in water!Only distillation can help!
NM sensitised by acids??? I have never seen this in any book I have on nitrocompounds!
What I know is that the solubility comes from a partial decomposition into nitronate...nitronic acid is soluble slightly in water and its solubility decreases when there is a trace of acid in the media!
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Anthony
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posted 04-25-2001 03:36 PM
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I poured some of the NM fuel I had into water. It immediately turned cloudy white and a thick layer of yellow castor oil went stright to the top. I've left it so hopefull the NM will settle out at the bottom.
Thanks philou, I will try again soon. I had presumed that you needed to distill the NM under vacuum or it would decompose from the heat. I was using a pretty strong vacuum (for re-gassing fridges). I will do it without the vacuum next time so that I can tell when the different fractions are coming off by reading the temp. I'll also make a condensor instead of using a cooled flask.
PHILOU Zrealone
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posted 04-26-2001 07:15 AM
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Yes there is no need of vacuum for the distillation of NM; no risks of explosion! You don't even need a glass rod distillator; a simple wooden (i guess its is that in french we say "liege" a kind of agglomerated wooden foam that is used to close wine bottles)stop rod will do the thing since NM is non reactive substance (not acidic like HNO3) towards wood. The thermometer must be placed near (in front of) the top of the cooler/condenser pipe so it gives the temp of the gas that is condensing there!
Don't put the thermometer in the mother liquor since that has a higher temp (overheated castor oil/water mix)!!!
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Anthony
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posted 04-26-2001 04:43 PM
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In English it is "cork"
I just tried again with a cork bung with a glass tube through it and then some PVC hose leading to a cooled flask (I found the vapour condensed in the tube as soon as it left the retort so no need for a condensor). I had the thermometer in the heating water bath for the retort, I know it's not very accurate but it was all I could do. I had the methanol coming off nicely but didn't have time to get it all out.
I got some rubber bungs for wine making which fit my thermometer with a short piece of pvc hose over the thermometer to make it fit tightly in the bung. I managed to make a small (approx 3mm) parallel to the original hole for the glass tubing (I only have small diameter stuff at the moment). So now I can have a thermometer in there to read the vapour temperature. Only trouble is that the bung is far too big to fit into the bottles I use for a retort. So I'll punch a hole in a metal jar lid and use the jar as a retort.
This stuff sure is hard when you don't have proper lab supplies!
The NM fuel in water: it is still cloudy white (caused by the methanol) and I cannot see any kind of seperation that would be the nitromethane. So I think it's not going to work.
TylerDurden
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posted 04-27-2001 04:56 AM
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Philou, I didn't say you could separate NM from castor oil with this method. I said you can separate NM from the methanol by adding water to the race fuel (about as much as the amount of fuel, and not by pouring the fuel in a lot of water). The mixture will turn cloudy white and letting it stand 10 minutes results in a layer of NM at the bottom.
Now, if castor oil is present it will most likely settle down with (dissolved in) the NM (or maybe float on top). And if the amount of castor oil is low you get a mixture of NM/castor oil that can be used (after drying) for explosives.
By the way you can separate the NM from the castor oil by adding pingpong balls (celluloid) this will gel the NM (adding PPB's directly to the race fuel will not work becuase celluloid dissolves in methanol. If you want to gel NM out of race fuel you need guncotton/smokeless powder).
And NM is sensitized by acids! NM is sensitized by almost anything! alkalies, acids, oxidizing agents, reducing agents, and lots more.
And the advantage of this method is that it's EASY. You only need water. Of course destillation yields a better, purer product without the castor oil but you need glassware , heating source, thermometer, and time. If you have it I would recommend distilling race fuel. And remember that castor oil is probably just as good as fuel oil for producing ANFO, so a bit of castor oil in NM will probably have no negative effect when used to make the ANNM explosive.
[This message has been edited by TylerDurden (edited April 27, 2001).]
[This message has been edited by TylerDurden (edited April 27, 2001).]
TylerDurden
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posted 05-08-2001 06:44 AM
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Anthony, I think the yellow layer at the top is NM with castor oil. Since no layer is formed at the bottom and NM dissolves castor oil. So the mixture of NM/castor oil in this case is lighter than water/methanol and therefor floats on top.
The race fuel I used resulted in the NM settling down (probably with some castor oil), but I think it depends on the ratio of NM/castor oil wether it settles down or floats on top. It's impossible that NM stays dissolved in the methanol/water mixture.
So you ended up with a 50/50 mixture of NM/castor oil. This is probably not very usefull but you can get NM out if the mixture with celluloid. And if you use race fuels with less castor oil the resulting mixture contains mostly NM and can directly be used in ANNM explosives.
Anthony
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posted 05-08-2001 02:25 PM
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Maybe it does float with castor oil dissolved in it, I don't know. I've got the seperation by distillation sorted now some I'm not really worrying about it. An easy way to tell what fraction is coming off is to drop a drop of the distilate into water, if it's methanol it'll form a little white cloud. If it's NM it'll sink to the bottom in a little ball.
TylerDurden
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posted 05-09-2001 06:30 AM
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Yes, distillation is by far the best method (if you got the glassware and thermometer and stuff). But I was just wondering about an easier way to extract NM, so...
By the way, if you distil race fuel you will end up with a NM/methanol mixture (80-90%)(depending on the quality of your distillation equipment: with bad equipment it's impossible to separate the two and you'll end up with a mixture with a lot of methanol) because the boiling points of methanol and NM are too close together. And methanol has some serious disadvantages: it's poisonous and atracts water from the air quite quickly (a drop of race fuel spilled will turn cloudy white within a short time because of the water that is absorbed from the air!).
But if you would distil the NM/castor oil mixture that you get after adding water to race fuel, you would get PURE NM without methanol and without castor oil! (and the distillation is much easier and can be done with some improvised equipment since you just have to evaporate the NM and somehow cool it and collect it).
So my method proves to be handy after all: it will give you a route to pure NM without methanol (or a usefull NM/castor oil mixture if you don't want to distill).
"one can make all kinds of explosives using a few simple household items"
[This message has been edited by TylerDurden (edited May 09, 2001).]
[This message has been edited by TylerDurden (edited May 09, 2001).]
Anthony
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posted 05-09-2001 03:48 PM
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I agree with what you're saying but I'd hardly say it's difficult or impossible to seperate NM from methanol with improvised equipment! Methanol B.P = 65*C NM = 101*C that's a fair amount of difference. I usually discard the first NM drawn off as it could contain the last dregs of methanol.
If you add race fuel to water and draw off the NM/castor oil layer and try to distil it, you're going to have water in your "pure" NM.
TylerDurden
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posted 05-10-2001 05:15 AM
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Yes, you're right, the NM would contain water (max. 2.5%). But it's easy to dry, with some AN. And then you have 99% NM.
Besides, your resulting NM/methanol mixture will probably also contain water since the methanol atracts it from the air (before or during the distillation or when in the receiving flask with NM, or afterwards). Maybe that's why it should be done under reduced pressure? And stored airtight.
Even if you dry it, you would have a hydroscopic NM/methanol mixture of max 90%.
TylerDurden
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posted 05-14-2001 11:46 AM
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Any comments on that? Getting water in the NM/methanol mixture would be a problem I think.
Anthony
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posted 05-14-2001 02:17 PM
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OK, I'll try both methods and compare the results.
TylerDurden
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posted 05-15-2001 06:03 AM
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OK, thanks. Let me know.
TylerDurden
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posted 05-24-2001 07:10 AM
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Don't want to rush you, but are there any results already?
Anthony
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posted 05-24-2001 03:02 PM
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Ah yes, my conclusion: Bollocks to the both of them I'm going to just buy some pure NM.
You're right, seperating NM from methanol is difficult having to work at low temperatures to stop them both coming off takes forever.
Seperating the castor oil collected from pouring the fuel into water seemed to work, except the "NM" extracted didn't smell right, dissolved in water and was flame retardant!
TylerDurden
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posted 05-25-2001 06:16 AM
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I can accept that my idea doesn't work. Sometimes a perfectly good idea turns out to be bullshit. But what I don't understand is WHY it doesn't work. And I can't stand that. So does anyone have an explanation for this result??
Maybe the NM is still dissolved in the methanol/water mixture (and makes it turn cloudy white)? But this seems unlikely. It would prefer the castor oil wouldn't it? And it can't stay all in the water/methanol can it?
And if the resulting "NM" is not nitromethane (and it clearly isn't) what the fuck is it then? And how can it dissolve in water when it is distilled from the layer that is separated by the water?!
This makes me crazy. So please help me.
Teck
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posted 05-27-2001 02:57 AM
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why not just buy the NM its $30 for a gallon at http://www.worldwideracingfuels.com/products/fuel.htm
ezekiel
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posted 05-27-2001 06:50 AM
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Nitromethane boils at 101'C, and is soluable in water.
Methanol boils at 64.6'C, and is miscible in water.
Thus bisolvent extraction with water won't work, or at least won't work very well at all.
Much better is distilation. You don't even need one of those expensiv vacuum pumps. The difference in Bps is so great that it should be piss easy.
Admittedly I have never done it, and certain parts of the fuel may piss around with the boiling points.
Step by step guide:
Boil of methanol at 65'C
Distill off nitromethane at 102'C, discarding residue.
Dry the distillate with calcium chloride to remove any water picked up.
Filter... you now have hopefully pure-ish, 0% water Nitromethane.
Remember to use a closed flame, or oil bath or double boiler for heating as both NM and Methanol are flammable.
Anthony
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posted 05-27-2001 10:18 AM
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Ezekiel, if you heat to 65*C you get left with nothing but the castor oil.
ezekiel
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posted 05-27-2001 05:29 PM
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I don't know what to say: nitromethane boils at 101'C.
Is this s general consensus opinion or just anthony's experience?
Anthony
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posted 05-27-2001 07:58 PM
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I don't claim to know what I'm doing, I'm learning as I go along. I don't see why NM shouldn't vaporise and condense at 65*C, afterall, BP of water is 100*C and it evaporates at room temperature.
TylerDurden
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posted 05-28-2001 06:02 AM
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Nitromethane isn't soluable in water! The solubility in water is about 10%. It is of course completely miscible with methanol. And about 2.5 % of water will dissolve in NM.
And water and methanol are also completely miscible. So far the facts.
Now what the effects are of adding water to race fuel I'm not quite sure anymore (I assumed that nitromethane was totally insoluble in water). The amount of water is probably important just like the percentage of NM in the race fuel.
If to 100 ml of race fuel (20%NM, 20% castor oil, 60 methanol) 100 ml of water is added what happens? Maybe the NM stays dissolved partly in the methanol partly in the water and only the castor oil separates. Who knows?
Maybe using another solvent is helpful?
By the way, you should distil under reduced pressure because otherwise the methanol attracts water from the air.
The resulting NM/methanol (80-90% NM) mixture you get after distillation has the same problem. (Distillation won't lead to 100% pure NM!)
[This message has been edited by TylerDurden (edited May 28, 2001).]
CodeMason
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posted 05-28-2001 06:13 AM
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To get the water out of a mix of NM and water, try chilling it to 0ºC. NM can remain liquid at temperatures as low as -25ºC, so the water will become ice but not the NM. All you'd have to do then is filter out the ice.
gcic
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posted 05-28-2001 08:36 AM
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Isn`t it a danger to cool the nitromethane to 0°? Cooling down nitroglycerine is also dangerous, so I could imagine, that NM probably behaves in the same manner(?)
PHILOU Zrealone
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posted 05-28-2001 11:00 AM
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No because nitromethane is a nitrocompound while nitroglycerine is a nitrate ester...and thus is much more sensitive and high detonating explosive!
Nitroglycerine is actually propantriol trinitrate ester!
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gcic
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posted 05-28-2001 12:50 PM
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Yes, I know what nitroglycerine is. Philou, could you tell me, please, what is exactly responsible for the increasing sensitivity of very cold NG? I mean, what chemical background does that have?
10fingers
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posted 05-28-2001 01:26 PM
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Actually, nitroglycerine is less sensitive when cold.
Mr Cool
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posted 05-28-2001 02:25 PM
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I think it's just friction between crystals of frozen NG. Also, crystaline explosives are always more sensitive than amorphous forms (look at crystaline TNT and quickly cooled cast TNT).
gcic
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posted 05-28-2001 05:22 PM
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ah yes, thx. That sounds like a reasonable explanation. Do you know, at which temperature nitroglycerin starts freezing?
My book says +10°C, but I can`t imagine this.
Well, let`s better close this topic. It has nothing to do with the original discussion anymore.
PHILOU Zrealone
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posted 05-29-2001 11:08 AM
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Actually it is irregularities in the cristals that generates such a sensitivity (innerstresses)! Also since when frozen the density is higher for most of the substances (water is an exception yes; ice of other products goes to the bottom of the fluid!), then the VOD is as high as 8000m/s!
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Mr Cool
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posted 05-29-2001 11:21 AM
Oh yes, stresses. Like when big crystals of lead azide form if you don't add dextrin or whatever, and they spontaneously detonate. And when AP sublimes and re-crystalises, forming vey sensitive crystals.
PHILOU Zrealone
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posted 05-30-2001 05:15 AM
Precisely!