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Chris The Great
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Some tests today 
My methyl nitrate has now turned yellow, and the small amounts of sodium bicarbonate left after dehydrating it has stuck to the sides and soaked up
all remaining water.
At first, I tried hitting a drop with a hammer, which resulted in nothing, as I can't put much force into a hammer swing or I miss all the time.
But it reassured me that it won't suddenly explode anytime soon.
I then tried (after firing a new detonater design, which worked great and was also used in this test) detonating a mL of methyl nitrate in a thin
metal casing, crimped at the end and taped to the detonater. I made a small cut in the ground with a garden shovel, and dropped it in, and then
closed the gap by stomping (carefully!), in order to keep the roots etc as undisturbed as possible (I tried digging, then packing the dirt over an
explosive once, with the result of the dirt flying up and that was pretty much it). It gave me a half foot crater and according to my brother the
farthest flung piece of grass went up over fifty feet and landed nearly forty feet away. I couldn't see this as I was inside the door of my lab,
as it was raining and I didn't want to get my switch wet. I did find the piece forty feet away however.
Also, the noise was not extreme, nothing to cause the nieghbours to come after me or even look outside.
I am thoroughly impressed.
I'll do it again tommorrow and take some pictures and maybe a video, as I like to document my experiments with a camera, makes them fun to look
back on.
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Chris The Great
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450ml of the same brand drain cleaner was added to a jar in a salt-ice bath (made from crushed ice I chipped out of my freezer, since I ran out of
other ice) and was allowed to cool while I weighed out 300g of ammonium nitrate. The ammonium nitrate was added at first one tablespoon at a time
with heavy stirring (this time with a glass rod, so my stirstick wasn't being dissolved by the nitric acid fumes that come off the mixture). It
turned black, and then an orange colour acid the acid (slowly this time) oxydized the dye. I added the rest much faster since it wasn't fuming too
much and the oxidation was complete. I put a plastic lid on top of the jar to keep the nitric fumes from escaping and let it set for about 15 minutes
to cool down while I measured out some methanol and sat down since my back was sore.
The methanol was added in little squirts from a syringe over 15 minutes. No trouble was had with the temperature and there was no NOx fumes coming
off. The nitration is very tolerant of higher temperatures and rapid addition times. It was stirred for another few minutes after all the methanol
had been added, and then was allowed to sit for 15 minutes or so to finish up.
As can be seen, there is still some dye that colours the mixture a bright orange. Oh well, the coloured acid is much cheaper than the higher quality
clear drain cleaner.
Water was poured in slowly with stirring. The bottom layer was very thick and was a precipitate, most likely ammonium acid sulfate. It dissolved
with a bit of vigorous stirring. The methyl nitrate then slowly floated to the top.
I stuck a length of aquarium tubing to the very bottom, and then sucked a bit on the other end to pull up the liquid (it was about 4 feet of tubing so
there was no danger of me accidently drinking some of the spent nitrating mix). I then let the bottom layer drain out into a 5 gallon bucket half
full of water (it was there in case of runaway, and then to dump the spent acid into after the nitration). It came out fairly quickly, with a fair
amount of pressure. I stopped when the bottom layer was a little more thick then the top layer of methyl nitrate.
More water was poured in, and the methyl nitrate then sunk to the bottom of the jar.
I carefully cleaned the tubing used for the diluted acid, and now used it to drain out the bottom layer of the methly nitrate into a jar. However,
there was too much pressure so I couldn't stop it in time and a fair amount of water also came through. Next time, I'll use pliers to close the tube
and stop the flow.
The top layer was suctioned off carefully using a plastic syringe, leaving behind a large amount of (yellow/orange) methyl nitrate. Some chunks of
anhydrous magnesium sulfate were added to soak up the remaining small amount of water floating on the top, and whatever water is dissolved in the
methyl nitrate. The jar was then closed and some tape wrapped around the lid edges to prevent any methyl nitrate from evaporating out.
Normally, the methyl nitrate would be clear, but it still has dye in it from the acid. Normally I would have washed it, but it is going to be used
within the next two days so I didn't bother. My next batch will be washed, and I suspect it would remove a large amount of the dye from the product
as well.
Finally yield is approximately 130ml, which is a huge improvement over last time. This corresponds to 60% of the theoretical yield.
It burns with a very large, non-luminous gray flame, which looks really cool. It leaves behind some water and the dye, so there is a fair amount of
water dissolved in it. I will probably add some more magnesium sulfate chunks to it to speed up the drying process. The burnt dye hurt my nose when
I sniffed it, probably decomposed to give some toxic products. Shouldn't effect explosive performance too much though.
It is planned on being used in some high power shaped charges
EDIT: I noticed the links to the pics of my first attempt at broken, and I can't edit the original post. So here are the pics with thumbnails on this
thread instead (if I mod wants to edit them back to replace the broken links in my original post, that would be nice )
[Edited on 7-2-2006 by Chris The Great]
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Dream of the iris
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Lol! "Ultra Super Mega Explosive! Don't touch".
Good job. I've been meaning to try this explosive.
BTW, Methanol OTC is sold as "HEET Gas tank Anti-freeze". It's the yellow bottle and it says on the back "Warning contains methanol" :p
\"Woah! Ok, you\'re now shooting your imaginary friend in front of 400 gallons of nitroglycern!\"
-Tyler Durden, Fight Club
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Dream of the iris
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What's the shelf-life of methyl nitrate dynamite?
\"Woah! Ok, you\'re now shooting your imaginary friend in front of 400 gallons of nitroglycern!\"
-Tyler Durden, Fight Club
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Boomer
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One week to one decade, depending on how well it is washed and whether the other stuff is compatible.
Adding 1% chalk helps too. Don't add too strong a base as it DE-creases stability! And the colder the better, every ten degrees C will double the
life, meaning freezer vs. room gets you a 1600% shelf life increase.
PS: The horror stories about frozen NG (no concern here) come from either big amounts of partially frozen stuff, with chunks banging around in the
liquid on transport, or from thawing big amounts without supervision. Does 'Tc' ring a bell? Even for the much more thermally stable PETN, you WILL
get an explosion if you bring a 1m-radius sphere to 88C. Even lower if the packaging is insulating. Small amounts stand that temp for a long time, and
worst case will eventually start to smell .... 
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Chris The Great
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I found that even poorly washed methyl nitrate stores well. However, that was in very small amounts so....
You are more likely to lose it to evaporation than decomposition IMO.
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Zinc
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| Quote: | Originally posted by Madog
i did actualy get NG headaches 2 times, from tasteing it.
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Does it taste good?
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hinz
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I've also made some of it. Later, when I cleaned my glassware, I had the involuntary pleasure to taste some of it as I cleaned my pipettes by sucking
water in it with my mouth. (Sorry I do not have any big pipette nipples)
It tasted spicy sweet, with an burning in the mouth like if you get accidentally acetone or conc. ethanol on your tongue. I didn't get any headaches,
maybe it's because I flushed my mouth with water afterwards, later I used my aspirator to suck the water through it.
I didn't use any given methanol/nitrating acid ratios, I just added as much methanol as the nitrating acid could nitrate.
I used:
400ml 96%H2SO4
250ml 53% HNO3
appr. 150ml more or less absolute methanol, which I destilled once from modell aircraft fuel
In the beginning I used twice Maddog's ratios (22ml H2SO4,14ml 53%HNO3 and 10ml methanol, a bit less than him, it's due my crappy 53% HNO3). I found
out that it's important that all MeOH gets nitrated, only methyl nitrate is insoluble in nitrating acid. If one use to much MeOH, the excess of MeOH
will disolve some methyl nitrate. The disolved MeONO2 is prone to hydrolysis by the nitrating acid. I found this out in the first two more or less
small scale nitrations.
In my third nitration I used appr. 250 ml nitrating acid. I did it in an ice bath and added appr. 20ml MeOH slow enought to keep the temperature
down. As I saw a layer of MeONO2 on the top of the mixture, I decanted the top layer in a graduated cylinder and pipeted the lower layer(nitrating
acid) back into the nitrating baker. I repeated this till no MeONO2 layer formed on top, then I stopped and waited half an hour and took the layer on
top that had formed slowly. It's important that you stop there, because of the hydrolysis. At my first attemps I added to much MeOH so it dissolved
the MeONO2, the solution hydrolysed, forming lots of small bubbles of an undefined gas (maybe CO2) and little NOx.
The power of the first charge (15g), which demolished an old Mac CD-R drive and cutted the herbage in a circle of 20cm was so amazing that I nitrated more (last big scale synthesis) that gave me 130 ml
MeONO2, used with some old stuff to make a charge of 150ml. This charge blew up an old lawn-mower engine with that much power that no parts of it left
at the place, where it detonated.
This was my first nitration and I loved it.
[Edited on 5-7-2006 by hinz]
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Chris The Great
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It really is amazing stuff isn't it?
I fired a film canister a while ago, from a hundred feet away the blast gave a strong thump across mine and the spectators chest, and set off some
guys car alarm a block away (the neighbours actually, since this was a rural area).
Today I set of 45g of 90% methyl nitrate/10% nitrocellulose gell with 30% added aluminum powder
I didn't know about the excess methanol problem, thanks for bringing it up. It might explain why a slight reduction in nitrating acid relative to the
methanol caused a big drop in yield (65% -> 45%) for me...
You will probably end up with methanol dissolved in the methyl nitrate as well as lossing methyl nitrate, giving not only a lower yeild, but an impure
product.
I've done this procedure a few more times, and have gotten it nearly figured out for a completely improvised synthesis...
I get best results with a 10% molar excess of ammonium nitrate realative to methanol, ie 1.1mol AN for every mol methanol. Then, I have 2 moles of
sulfuric acid per mole AN, or 2.2mol H2SO4 per mol methanol. This is using undried AN and sulfuric acid, and I get about 65% yeild.
The reaction only needs very poor cooling. I added all the methanol over 20 minutes using a cold water bath, which was a bucket with cold water in it
with a couple ice packs dropped in. Maybe 10*C or so, not cold at all. The reaction was a little warmer than usual and gave off a lot of fumes, so
an ice bath would be best, but a salt ice bath is not necessary at all and is not worth the trouble mixing it and then disposing off a bunch of wet
caked salt the next day.
I honestly think that this reaction would be impossible to get a runaway, in fact I may try to get one by adding all the methanol to the hot acids
without cooling, on a small scale and outside of course. But I think that the methanol and methyl nitrate will just boil away and prevent a runaway
from occuring even in the absolute worst case scenario.
For washing, I tried making a basic saltwater solution with salt and bicarbonate, didn't work. The stupid bicarbonate doesn't dissolve at all. So
don't bother. You cannot use NaOH, it will destroy your product. However, just saltwater works fine. I use pop bottles to wash it, and about triple
the volume of methyl nitrate in saltwater. I start shaking slowly but the two layers mix quickly, after which I give it a very good shake for a few
minutes. Then I seperate the layers and repeat. I did this two times, but I think three might be better.
Whatever you do, don't wash with a only bicarbonate solution, not only is it useless, it dissolves a large portion of the methyl nitrate!
Whatever the hell makes the orange colour in the drain cleaner does not come in the washing. I might try steam distilling the methyl nitrate (I don't
want to try straight distillation) and see if that helps. Once distilled, I will add salt to the receiver containing the methyl nitrate and water,
which will cause any dissolved methyl nitrate to precipitate. Hopefully that will give a batch of pure (and clear) methyl nitrate.
I mentioned earlier in this post that I suspect some methanol is in the methyl nitrate product, I should point out this will not be removed completely
by washing nor by steam distillation should you choose to do that as well, since the boiling points are almost exactly the same. However, I started
another thread about forming complexes with methanol. Calcium chloride will do so, as well as complex water. If used as a drying agent, not only
will it remove all the water from the methyl nitrate, it will also complex and remove any methanol in the product! See this thread:
http://sciencemadness.org/talk/viewthread.php?tid=6063
I'm thinking for my next batch, I'll make a cheap seperatory funnel from a 2L pop bottle. A plastic tube will go into the bottom (but not the very
bottom, on the side, so it can stand upright) and allow the liquid to flow out, and can be stopped using a pair of pliers to close it off. A small
hole is drilling into the lid.
To operate, the methyl nitrate and diluted spent acid are poured in the top hole with the tube held up high and the lid is screwed on. Then the tube
is crushed with a pair of pliers, and the bottle inverted. You need to close the tube so the mixture can form two layers after being diluted. Some
will squirt out the bottom, but it won't be that bad. Then, open it up and seperate.
It should take a few bucks to make this for this procedure, and beats a $50 seperatory funnel any day. I make a lot of nitric esters so a special
seperatory funnel for them is definateyl worth it.
Sort of off topic, but such a funnel will make this procedure vastly easier for those who don't have access to standard lab equipment.
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hinz
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I've just tried the destillation-nitration method. I borrowed my sister's camera to make some pictures of a synthesis that should give a nice HNO3 to
HE-ratio.
So I set up my destillation apparatus:
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16900...
I heated the mixture of appr. 400ml 53% HNO3 together with appr. 70ml MeOH in a water bath to 65°C. At the beginning no NOx was produced. The mixture
went yellow and began to destill over. I switched the hotplate off, since the water bath temperature was around 70°C and the first vapour bubbles
were forming in the nitration mixture.
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16901...
I took this picture and looked how the first drops condensed inside the liebig, when the mixture began to produce lots of “brown fumes”.
I took the flask immediately out of the water bath, but the NOx production didn’t stop. The production of it was quite scary as you can see in this
picture: (look at the NOx that comes out of the vacuum destillation adapter )
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16901...
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16901...
I grabbed my gas mask and poured some cold water in the pot to stop the NOx generation. After a while this helped to cool down the flask so that the
NOx generation stopped.
Due the heat of the runaway nitration, some more liquid came over. First I poured the stuff into a graduated cylinder and saw those stupid bubbles
again, those which I saw also at the classic H2SO4/HNO3 method. Later I realised that it might be dimethyl ether according to this equation.
CH3-O-NO2 + CH3-OH [CH3+…+…NO3-+...CH3-OH (SN1) ==> H3C-OH+-CH3 + NO3-].==> H3C-O--CH3 + HNO3
This gas was also produced inside of the destillation setup, I know this because some pressure build up at the vacuum destillation adapter (I put my
finger on it and recognised the small pressure, but the gas was not brown). I was able to lead some of it into a test tube and it burned with a
methanol like flame and smelled afterward like some kind of aldehyde (formaldehyde, I suppose). For me this reaction is plausible since:
-MeONO2 is a strong methylation agent (less strong than DMS, but the NO3- group should be a nice leaving group due it’s thermodynamic resonance
stability)
-Dimethyl ether is a gas.
-The gas burns.
-The gas produces a adlehydic smell after burning and doesn’t smell unburnt.
Who is gonna pay me a GC/MS that I can identify this gas for sure
In the end I poured the destillate into a sepeatory funnel and added a saturated, aqueous NaCl solution, but it didn’t form two layers.
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16901...
Does anyone has also some experience with those kind of nitrations and does She/He know what I’ve done wrong? I might add some urea nitrate to get
rid of a bit of NOx but with those amounts I produced, I think the urea nitrate is overstrained and I doen’t have any (but I might produce some with
my own piss ). I might try to destillate the stuff under vacuum, but I think that
the liebig condensor will get some problems to condense liquids that boil below 30°C.
Btw I’m glad that the shit didn’t explode, although I don’t suppose that much MeONO2 formed.
[Edited on 19-7-2006 by hinz]
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nitro-genes
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| Quote: | Originally posted by hinz
In the end I poured the destillate into a sepeatory funnel and added a saturated, aqueous NaCl solution, but it didn’t form two layers.
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Most likely you just collected some methanol and water, no esterification has taken place...
I hope you are aware btw that distillation of methylnitrate, especially without any vacuum, may result in unexpected explosions?
With this setup and destillation temperature it is likely you collect a mixture of methylnitrate, NOx and small amounts of nitric acid all together,
which may sponteanously ignite/detonate.
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hinz
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The only liquid that should come over at 50-70°C is methanol or methyl nitrate, water has a far to low vapour pressure at this temp, for this purpose
I've added a vigreux column. I think it was mostly methanol. Acording to Fedorff IIX p M110, it was first prepared in a small yield by destilling 63%
HNO3 with methanol, not too much different to my reaction conditions. What wonders me why I got that much NOx, if other people prepared it also by
destilling and I don't believe that these people feed their condensors with salt/ice, dry-ice/acetone etc. to destill MeONO2 with a boiling point of
25°C under vacuum. With other methods you can't destill a liquid with bp. of 25°C. The equilibium is also shifted to MeOH/MeONO2, (because it
destills first and water remains). The ratio of 1:3 of MeOH to pure HNO3 should be able to nitrate most of MeOH before it comes over.
Maybe I'm wrong and those people really used vacuum with exotic cooling
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nitro-genes
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Also, wouldn't the use of 53% nitric acid alone make oxidation of the methanol much more favorable? I've no idea how susceptable methanol is to
oxidation though, but at 65 deg...
[Edited on 20-7-2006 by nitro-genes]
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hinz
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After my extremly nice results with the conventional method I came to the conclusion that the destillation method is the biggest crap, at least in the
home lab, because I’m pretty sure, even with conc. nitric that would end up again with lots of brown fumes or I’ll suck half my destillate through
the aspirator if I would use vacuum. Now I used 400ml H2SO4, 400ml fresh destilled fuming nitric acid ( 500ml H2SO4 + 750g KNO3) and a lot of methanol I’ve destilled over CaSO4 to get it completely anhydrous. This
is the yield I’ve got:
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16939...
(not exactly, it would be 20-40ml more if I wouldn’t get a runaway in the end, the last separatory funnel hydrolysed and the mixture boiled out of
it)
One of those numerous fractions I’ve searatd:
http://pic20.picturetrail.com/VOL1206/4241286/11641500/16939...
I’ve only nitrated 50-100ml MeOH at once, this should prevent that too much methanol dissolves into the MeONO2, furthermore it will decrase the mess
at a runaway and the detonation risk due the stirring.
The yield is:
400ml HNO3 x1.5g/cm3 = 600g
600g/m(HNO3/63g/mol)=9.5 mol HNO3
530ml MeONO2 x 1.2 g/cm3 = 636g
636g/m(MeONO2/77g/mol) = 8.25mol MeONO2
This gives a yield of 8.25mol MeONO2 /9.5mol HNO3 =86% product in relation to the used nitric.
This is quite nice, isn’t it?!
Tomorrow I’ll nitrate some cotton and gelatinise the methyl nitrate till it’s nice kneadable and keeps it’s form. Then I’ll put it into a PE
plastic bag to prevent evaporation and knead it over in a 70° bend 0,5mm thick brass sheet. This should give a nice, very improvised linear sharped
charge without any casing, only the liner.I think I’ll lay the blasting cap just on the plastic bag, held by some cardboard strips. After I’ve
detonated it I’ll post my results in the “sharped charges threat”
[Edited on 20-7-2006 by hinz]
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Chris The Great
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You'll need a lot of nitrated cotton. I did a 10% solution and it's still pretty runny stuff. Then again, I could just have made "short"
nitrocellulose which doesn't gell as well... but just keep in mind that the gelatines are very runny compared to nitroglycerin, which is supposably
very thick.
Anyway, sounds like an interesting idea, don't see any reason for it not to work. Good luck!
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gregxy
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Many years ago I made methyl nitrate by distilling methanol with 70% HNO3. I added some urea to the HNO3. This was
supposed to remove any nitrious acid. There were no problems with oxidation. I know that what I got was methyl nitrate since I used to store it under
water. Maybe you need
to add the urea to prevent the oxidation?
I also remember trying to nitrate ethanol and propylene glycol by distilation, but they just oxidize and give brown fumes.
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hinz
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Sorry guys, the sharped charge project wasn't realised, the guncotton didn't really gelatinise my methyl nitrate, so I couldn't knead it on the brass
liner. I first added some chalk to neutralise the excess acid, later I filtered the chalk off aggain (the vapors still colored pH paper, but not as
strong as in the begining) and begann to dissolve NC (appr. 70g). In the beginning the MN got gelatinsed quite well, I found that the MN gets well
gelatinised as long as the NC isn't fully dissolved and the fibres bind the MN between them, so its the best to gel it right before use, but a few
hours later it went syrup-like so I begann to build a case for my sharped charge and coated the brass with epoxy resin so that it won't form any
nitrate together with MN. I wanted to dry it overnight, but in the evening I went bach to my lab and saw that the MN was decomposing together with the
NC, there were only 420ml of the 500ml left. The NC decomposed to a foarmy chuck inside my erlenmayer and nitrous gases were released, maybe I should
have really washed my MN.
So I grabbed a detcap and went together with my erlenmayer outside of the village and detonated it. The erlenmayer had to die the decoposed NC chuck didn't get out of it, so I just sticked the cap at the wall of
the erlenmayer. The crater had an diameter of 30-40cm and was about 25cm deep, I really felt the shockwave going trough me (interresting feeling), I
was arroud 30m away.
[Edited on 24-7-2006 by hinz]
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Chris The Great
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Interesting you got it to decompose... probably dissolved NO2 if it happened that fast. I found my main problems where that the mix isn't thick
enough once fully dissolved, and also that the methyl nitrate loves to evaporate out while I mix it. Not really the best to gell unless you have some
very high viscosity NC.
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Bert
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Hinz, it is more likely that your nitrocellulose was the culprit than your methyl nitrate. It is VERY difficult to properly neutralize home made
nitrocellulose.
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hinz
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Dissolved NO2 might be a reason, my MN was always a bit reddish/brown/yellow, pure MN sould be colourless.
I let my NC stand for one hour in a baker filled with dest. water and then I washed it with ethanol to get it dry faster, I think that the MN was the
culprit of the decomposition because it wasn't pure, but you're right, it's quite difficult to get the acid out of the NC fibres, in water insolube
liquids are easier to wash.
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agent_entropy
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Is there any reason why store bought smokeless powder (double base) couldn't be used for gelatinizing MN? Or might the other ingredients just foul up
the works? IIRC The powder I have (Alliant, Red Dot) is composed of nitrocellulose, nitroglycerin, nitroguanidine, diphenylamine, polystyrene, and
some other ingredients that weren't specifically identified.
Also, just how stable is MN (well neutralized/washed) for storage? Would it maybe be more stable in a solution of methanol?
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Chris The Great
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It's very hard to gell the processed powder AFAIK. It gets pretty hard and takes a long time for solvents to soak in.
I have never had a problem with homemade NC, but I did boil the stuff for many hours...
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agent_entropy
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When you boiled your NC did you use NaHCO3 solution? Because that's what I did, and I think it partially destroyed the nitroesters because it was
pitiful when I burnt it.
Later in the day... no one else has posted since I did so I'll just edit this post.
Anyway, I just made some MN using the method outlined above by Madog (page one) and I washed it once with water, then once with saltwater. This
yielded several ml of perfectly clear, colorless product. Chris, this leads me to believe that perhaps the cloudiness of your MN might be the result
of more than just water diffused (dissolved?) in the mixture. Perhaps something leftover from the drain cleaner or AN instead of or in addition to
water.
I tried putting a drop of the MN on a piece of paper and hitting it with a hammer but it didn't detonate, only deflagrated. So next I tried putting a
few drops on a small piece of fluffy NC, it gelled as expected, and when I hit that with a hammer it sure as heck did detonate (my ears are still
ringing).
So, how stable is methyl nitrate for storage? Is it one of those compounds that just detonates for no reason and without warning? What is the
best/safest way to store it? (if it is indeed storable)
[Edited on 26-7-2006 by agent_entropy]
[Edited on 26-7-2006 by agent_entropy]
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agent_entropy
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I just noticed something, apparently "methyl nitrate"and "nitromethane" are two different things. I've seen the two names used interchangeably in a
couple of places, which is rather confusing.
methyl nitrate > CH3ONO2
nitromethane > CH3NO2
Are we sure that these procedures produces methyl nitrate and not nitromethane? As I understand it, nitromethane is the one used as a racing fuel
additive, and I found an MSDS on it. However, I can't seem to locate a satisfyingly complete MSDS on methyl nitrate. Any help would be appreciated.
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not_important
International Hazard
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yeah, kind of weak
http://physchem.ox.ac.uk/MSDS/ME/methyl_nitrate.html
http://www.chemlaw.co.jp/Result_Eng_M/MethylNitr.htm
methyl nitrate is the ester of nitric acid and methanol, similar in general concept to methyl acetate or whatever.
nitromethane is a nitro-alkane, with the nitrogen directly bonded to the carbon; industrially made by the vapour phase nitration of methane by nitric
acid.
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