Sciencemadness Discussion Board

nitroglycerin

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Ral123 - 11-2-2012 at 08:59

If that is workable then I can store like 300ml egdn at an apartment no danger(except cops) what so ever. Is pure NG so sensitive that we can rely on it? Like if I throw glass vessel with 50ml?

quicksilver - 11-2-2012 at 13:22

When you make a mistake...... it's too late to say you're sorry.

Injury1.jpg - 70kB


300ml is a LOT OF WEIGHT! It's enough to create a blast wave that will drive objects into you. Close enough; and you're dead, no 2nd chances. Liquid explosives have a different set of rules and that's why they are not used in industry. The liquid is generally poured into an absorbent, etc.

What's more, YOU don't have to make the mistake. A loved one, a child,a friend, anyone mishandles over half a pound of EDGN or NG and the price paid is much too steep.
Do the math: even though EDGN is more viscous than NG, it's still over a gram per ml. One ounce is how many grams? Two ounces of TNT is what was used in the old Mk II "Pineapple" grenade. And TNT is less bisant and slower than EDGN.


EDIT:
Please don't take chances.



[Edited on 12-2-2012 by quicksilver]

caterpillar - 11-2-2012 at 15:07

This nice image reminded me my own experience. Blood, draining from my leg, slowly converted to something like red wax. I made (tryed, more precisely) NG twice. At the first time I got 5-8 ml of NG and dissolved some gun cotton in it, making blasting gelatine. At the second time temperature went up. I ran away and was waiting for explosion, that did not occured. I think, NG preparation is too simple and therefore not very interesting (to say nothing about properties of aforementioned compaund). HMX for example is much more challenging.

Ral123 - 12-2-2012 at 01:36

What's that thing into his leg? It looks too small for the hole it made? If I'm not going too much off topic, what can make egdn detonate. I'm currently ready to bet all my possessions and my life vs a dollar that a drop of egdn wouldn't detonate when falls to the ground. What are the risks of a 100ml pet bottle with well washed egdn? Btw I'm interested in your opinion, but I never keep any explosive in house. Make small quantity, do my stuff with it, if I regain interest, make more.

quicksilver - 12-2-2012 at 08:08

Well, friction and static are some of the real hidden devils. The problems start when any liquid nitric ester gets into threads of a container. There HAVE been means to reduce the risk. Teflon plumber's tape wrapped in the direction of close and the use of saran-wrap over the top to make sure none leaks becasue then you don't have to crank down tightly the threaded top. The use of a "cork" has never been a good idea becasue it stays in place through friction. albeit much less than grinding an amount with sandy shoes on a hard floor. There's very little you can do for static other than attempt to ground yourself at any point you may come in contact with the free material. An automobile can build up a substantial static charge - people forget that because it's insulated by the tires from the earth, but it can. Any transportation of a free, sensitive explosive with a car or truck should always have individuals check 1st if they have a static charge.

I used to work at a copper mine and we had collections of grisly photos. I still have them. Management would encourage that, almost. I think that's a piece of conduit driven into a worker's leg. I have some that I honestly can't look at for too long but I think it's in bad taste to just go OT and get into"Gore-pornography" simply to make a point. And in this case the format of the explosive is very problematic. The liquid nitric ester would almost always shoot faster than an absorbent. So why do companies use absorbents? In fact Dynamite and it's relatives are virtually no longer made for common usage. I think there may be one or two companies left that produce what would be considered dynamite today..... That's significant! It demands an explanation. And that is that water-gels and det-sheet (or plastique) can accomplish the same bisancy with far greater safety. It's very similar to firearms safety: you wouldn't sleep with your finger on a trigger because of the POTENTIAL of a discharge occurring.


edit:

Collections of photos (back in 1993!) got into the hundreds of megabytes. And that is a ridiculous amount of still photos of explosive-related mutilations. That fact alone suggests that the interest in energetics MUST be tempered with a great deal of common sense. The fact that the Child Protection Act was in response to hundreds of eyes and fingers and hands and genitals being ripped off suggests that this is something to take as seriously as any other agenda that has a similar potential. The CPSA's issues with fireworks alone didn't occur in a vacuum. Every time an incident occurs, it's another nail in the coffin of exploring energetic chemistry.

[Edited on 12-2-2012 by quicksilver]

Fusionfire - 12-2-2012 at 12:16

And of course NG is a HE. A bit of glass driven by HE can kill you and the shockwave can burst the alveoli in your lungs or rip flesh off your bones.

But let's talk about something more benign first so that one gets a healthy respect for HE. Do a Google image search for "firecracker injury". If that is what a low explosive with a deflagration velocity of 300-400m/s can do to the human body, imagine one with a VOD of 7km/s. It isn't like in the movies where you get thrown around by an explosion; you get torn apart by it!

When I make or manipulate HE it is always with polycarb goggles and a full face visor, in small quantities, on a tidy desk and I always try to put something between my hands and the test tube/beakers/etc., e.g. tongs + electrician's gloves.

caterpillar - 12-2-2012 at 15:21

Some NG stories. One of my friends made it and more than once. In a forest. Nice spring and enough snow to cool reaction vessel (basin, covered with paraffin). He thinks, that legends overestimate ability of NG to spontaneously explode. But, he never stored NG. The simplest experiment was how it burns. 1.5 liter was ignited in a hole. Hissing sound, growing column of flame and tremendous explosion. In my city (it was many years ago) one man, who's bride leaved him and was going to marry to another man visited this ceremony with a bottle, fulfield with light yellow liquid. Probably, he nocked a wall with it- sew needles was found on the other side of the street.

freedompyro - 12-2-2012 at 18:25

If your storing NG just add 20% acetone to desensitize. For most things you need it for it's going to need acetone added anyway. NG doesn't exactly dissolve NC easily.

caterpillar - 12-2-2012 at 22:03

Of course I did! I added some acetone to NG and only after it I was able to get blasting gelatine. But, I have to admit, I was unable to blow it up. I made some shit instead of lead picrate and aforementiond gelatine did not explode.

freedompyro - 13-2-2012 at 01:34

It's common knowledge (Or so I thought) that blasting gelatine becomes insensitive after a day and after a week cannot even be detonated by a number 10 detonator in some cases.

You can't let blasting gelatine sit and it's not the easiest thing to initiate either with our without a couple percent un-evaporated acetone left in it. Blasting gelatine is kind of a pain in the neck. The best way to make it is really to just heat the NG to 40C for six hours or so to dissolve the NC. (Uh, make sure your PH is perfectly neutral and your NC has stabilizers if you do it this way.)

[Edited on 13-2-2012 by freedompyro]

Ral123 - 13-2-2012 at 01:53

Two drops of egdn turned my ceramic mortal grinder into a spectacular fragmentation device. But only with a tiny organic peroxide piece also. Even the striking part was in at least five pieces. I'm sure NG can't beat that :P

caterpillar - 13-2-2012 at 05:17

In my case I definitely know, that poor primer (I think, it actually was not lead salt of picric acide but some shit) was the reason. But why blasting gelatine may become less sensitive? Acetone evaporates very quickly.

freedompyro - 13-2-2012 at 23:31

Ral123. In my opinion the brisance of EGDN is higher than NG, however... The initiation force required is higher for EGDN. Even though EGDN is harder to initiate the viscosity of it allows it to attain higher explosive pressures in smaller amounts than NG. It's only less sensitive because it's a thinner liquid and moves out of the way of force easier. You'll have to look into the research to see if this is true. That's just my opinion from personal experience.

Blasting gelatine when freshly made is sensitized by micro air bubbles and those go away after a few days.

aaparatuss - 14-2-2012 at 20:03

while pyrotechnics are interesting, I have never gone beyond smoke formulations.

but while brainstorming about the best ultimate use for a bunch of raw glycerine a local biodiesel producer was getting rid off i did catch up on some nitroglycerine points...

its seems a simple robotic flow reactor would be needed for making oneself enough dynamite for construction or personal excavating endeavors.

The real path forward i see is the experimentation of catalysts that preserve acid wastes

Al(H2PO4)3 serves as an efficient solid acid catalyst for nitration of a variety of organic substrates with nitric acid (70%).
www.sciencedirect.com/science/article/pii/S156673670700413X


www.imm.ac.cn/journal/ccl/1304/130412-311-01-484-p4.pdf
Abstract: Vapor-phase nitration of benzene over solid acid catalyst is expected to be a clean process with no sulfuric acid waste


H3PW12O40 catalyzed liquid phase nitration of aromatics —a green process without using H2SO4
School of Chemical and Biological Engineering & Research Center for Energy Conversion and Storage, Seoul National University, Seoul 151-744, Korea



there seems to be plenty of links...









Ral123 - 15-2-2012 at 01:59

There is no sulfuric acid waste in the industry. The question is about home lab. And who cares about more efficient way for NG. We want RDX :D

killswitch - 18-2-2012 at 15:13

Question: What would be the properties of a mixture that was (by volume):
65% nitroglycerin
30% methyl nitrate
5% methyl ethyl ketone peroxide (liquid dimeric hydroperoxide form)

quicksilver - 19-2-2012 at 07:15

How are you expressing "properties"? Do you mean formulation, action as an energetic or chemical activity / storage, utilitarian maintenance? There would be issues if exposed to climatic conditions and this could throw off the percentile relationship. Peroxides are often deliquescent and methyl nitrate may also have several exposure issues as well. Unless absorbed (as per Dynamite) or in a sealed container, atmospheric conditions present problems.
The addition of methyl nitrate and an energetic peroxide do little for the outstanding ability of nitroglycerin to preform work. They seemingly would enhance problems rather than detract from them. However, often to evade an existing patent, materials are added to an existing material so that it can be marketed under a different name and claims made for it, however similar to the basic material, could be enhanced simply from a profit standpoint.

[Edited on 19-2-2012 by quicksilver]

killswitch - 19-2-2012 at 09:05

Quote: Originally posted by quicksilver  
How are you expressing "properties"? Do you mean formulation, action as an energetic or chemical activity / storage, utilitarian maintenance? There would be issues if exposed to climatic conditions and this could throw off the percentile relationship. Peroxides are often deliquescent and methyl nitrate may also have several exposure issues as well. Unless absorbed (as per Dynamite) or in a sealed container, atmospheric conditions present problems.
The addition of methyl nitrate and an energetic peroxide do little for the outstanding ability of nitroglycerin to preform work. They seemingly would enhance problems rather than detract from them. However, often to evade an existing patent, materials are added to an existing material so that it can be marketed under a different name and claims made for it, however similar to the basic material, could be enhanced simply from a profit standpoint.

[Edited on 19-2-2012 by quicksilver]


I mean, would it be detonable from flame? If I'm recalling correctly, MEKP undergoes entropic decomposition, and methyl nitrate is one of the most sensitive high explosives out there. True, the sensitivity would be moderated by the nitroglycerin, but the mixture would be more sensitive than pure nitroglycerin, and could potentially be kicked off by the MEKP which would detonate from flame when confined.

SB15 - 19-2-2012 at 17:01

Quote: Originally posted by killswitch  
I mean, would it be detonable from flame?


Highly doubtful. None of the compounds you mentioned will reliably DDT from flame, and mixing them together is not likely to create a primary explosive.

Ral123 - 20-2-2012 at 00:44

Total madness. The sensitivity of NG but with volatility. One small spark is enough to detonate the methyl nitrate vapours and everyone to die :D

freedompyro - 20-2-2012 at 01:06

Why the hell would anyone want to make Nitroglycerin into a fuse sensitive explosive? Killswitch is smoking some good stuff...

Methyl nitrate synthesis itself with mixed acids is definitely not for the faint of heart and requires better equipment than I have... It doesn't have pleasant runaways like NG! It likes to go KA-BOOM!!!

I don't touch peroxides anymore even though I have synthesized them with no issues many many times. I'm a programmer by trade so I can't afford to have any accidents. I only use NPED's.

[Edited on 20-2-2012 by freedompyro]

mabuse_ - 20-2-2012 at 08:27
Quote:

I mean, would it be detonable from flame? If I'm recalling correctly, MEKP undergoes entropic decomposition, and methyl nitrate is one of the most sensitive high explosives out there. True, the sensitivity would be moderated by the nitroglycerin, but the mixture would be more sensitive than pure nitroglycerin, and could potentially be kicked off by the MEKP which would detonate from flame when confined.

This complete BS.

Since NG is very impact sensitive, you could probably detonate it the kewl way simply by sticking a flashpowder salute to it.
That's what Mr. Nobel did succesfully in the 1860s, a confined blackpowder charge surrounded by NG.
Kind of an NPED... I think thats what you're after.

Bot0nist - 20-2-2012 at 09:40

Yeah, A fast flash salute will shoot NG most of the time. No MEKP or methyl nitrate needed. That's (even more) suicidal. A semi-effective NPED can be made with copper oxide/aluminum thermite and a pellet of ETN wrapped in a layer of foil at the bottom of the paper tube. Works maybe 2 outa' 3 times, IME.

[Edited on 20-2-2012 by Bot0nist]

Ral123 - 20-2-2012 at 13:10

I know a guy that doesn't know what a flame sensitive explosive is. He uses flash from firecrackers to set off NG dynamite. He also says 100g flash sets off anfo :o Who thinks methyl nitrate should be in top 3 most dangerous nitric esters?

freedompyro - 20-2-2012 at 13:38

Methyl Nitrate... Definitely!

You can set off pretty much all number 8 cap sensitive HE's with enough metal confined Flash. Even though flash has a low VoD it packs a ridiculous amount of power.

killswitch - 21-2-2012 at 19:33

Quote: Originally posted by Ral123  
I know a guy that doesn't know what a flame sensitive explosive is. He uses flash from firecrackers to set off NG dynamite. He also says 100g flash sets off anfo :o Who thinks methyl nitrate should be in top 3 most dangerous nitric esters?


100g of flash would be roughly equivalent to twenty M-80 firecrackers going off. That wouldn't just cost you fingers; you could be looking at four inches of soot-blackened radius and ulna where your forearm used to be.

I'm unfamiliar with the acronym NPED.

And if I had to make a list, it would go something like this:

  • Nitric esters

    1. NC ——— 30.19 --F/g
    2. EGDN -— 19.68 –-F/g
    3. NG ——– 15.03 ---F/g
    4. MHN —— 13.42 --F/g
    5. ETN ——- 11.74 --F/g
    6. PETN —— 1.86 ---F/g
    7. MeNO3 — 0.07 ---F/g



    *Units are in Fucks/given.

    [Edited on 22-2-2012 by killswitch]

    Bot0nist - 21-2-2012 at 20:00

    Non Primary Explosive Device. Some people like to use sensitive secondaries (ETN) as primaries by subjecting them to thermal shock, etc, or using a fast burning and confined binary pyrotechnic mixture like flash or Armstrong's mix to initiate. Some would argue that Armstrong's sensitivity and speed is such that it can be classified as a primary explosive

    Ral123 - 22-2-2012 at 01:35

    My sweet EGDN at numer 2? And CH3NO3 safest of all? And you're making a daemon out of that NC :D

    Bot0nist - 22-2-2012 at 05:46

    Um, I believe he is measuring the amount of fucks he gives about the listed explosives, not their sensitivity. I may be wrong though.

    killswitch - 22-2-2012 at 15:33

    Quote: Originally posted by Bot0nist  
    Um, I believe he is measuring the amount of fucks he gives about the listed explosives, not their sensitivity. I may be wrong though.


    The fucks are given by the experimenter in regards to life and property in the process of synthesizing and employing said explosives.

    So, in descending order of safety.

    [Edited on 22-2-2012 by killswitch]

    freedompyro - 22-2-2012 at 19:32

    Your list is retarded... In reality this list in order of most dangerous on top to least on the bottom is like this...

    1. MeNO3
    2. EGDN
    3. MHN
    4. NG
    5. ETN
    6. PETN
    7. NC

    Nitration of EGDN is more hazardous and causes runaways 3x easier than NG. As for NC I am referring to the 12% nitrogen variety. MHN is a pain in the ass to purify properly and needs stabilizers asap.

    All of these nitrations can be done perfectly safely with the proper equipment and methods.

    [Edited on 23-2-2012 by freedompyro]

    Pulverulescent - 23-2-2012 at 10:16

    Quote:
    Nitration of EGDN is more hazardous and causes runaways 3x easier than NG.

    Yes, glycol produces a stronger exotherm with mixed acid than does glycerol but its much lower viscosity allows lower nitration temperatures to be used.
    And its lower sensitivity and extra ooomph and brisance makes it one very attractive HE!

    P

    Ral123 - 23-2-2012 at 12:47

    I did two runaways with egdn on purpose. Both were 60% nitric-2 parts and 95 H2SO4-3 parts. Then I pump the eg and ruuun. In the first-a lot of brown fumes, after witch even the sulphriric acid was vaporised :o nothing left. Second was similar but I think there was some acid left. Will I get a boom if I add egdn also next time?

    Bot0nist - 23-2-2012 at 12:59

    Quote: Originally posted by Ral123  
    Will I get a...


    Darwin Award? Very likely.

    [Edited on 23-2-2012 by Bot0nist]

    Pulverulescent - 23-2-2012 at 16:20

    Quote:
    I did two runaways with egdn on purpose.

    Like ─ deliberately?
    Why ─ 'the big question?

    P

    freedompyro - 23-2-2012 at 17:32

    You are not going to be able to create a dangerous runaway just by tossing tons of EG into the mixed acids without cooling. The acids are just going to burn the material away before it has a chance to be nitrated...

    In order to do that you need to create a runaway in a nitration that is half done or more with tons of nitrated material ready to go up. That is why they use excess acids in NG nitration. No detonation hazard as long as they keep the NG to Acids ratio low enough. As they do acid recovery with NG nitration's in factories it isn't a waste of acid.

    [Edited on 24-2-2012 by freedompyro]

    freedompyro - 23-2-2012 at 17:37

    Quote: Originally posted by Pulverulescent  
    Quote:
    Nitration of EGDN is more hazardous and causes runaways 3x easier than NG.

    Yes, glycol produces a stronger exotherm with mixed acid than does glycerol but its much lower viscosity allows lower nitration temperatures to be used.
    And its lower sensitivity and extra ooomph and brisance makes it one very attractive HE!

    P


    I hate EGDN... It's the only thing that ever gives me headaches... Grrr...

    Ral123 - 24-2-2012 at 10:54

    I think its a good idea to have an idea if things go wrong what and how happens. I know that for MeNO3 and don't do it anymore. I did the runaway test(with like 200ml or less) where I detonate my half a kilo UN mixtures. May be its madness but its a safe madness and not too far from what the concept of the forum is.

    killswitch - 24-2-2012 at 13:23

    Quote: Originally posted by freedompyro  
    Your list is retarded... In reality this list in order of most dangerous on top to least on the bottom is like this...


    I did the list "Least dangerous on top, most dangerous on bottom."

    Soo.....

    caterpillar - 24-2-2012 at 14:17

    During the WWII hungry teenagers made NG. Sometimes they slept, losing temperature control with all corresponding sequences...

    Bot0nist - 24-2-2012 at 14:22

    What?

    Teens in Hungary, or hungry teens? They feel asleep during the glycerine additions:o? I would have to be VERY tired to do that.

    caterpillar - 25-2-2012 at 21:59

    You will, especially if you have very few to eat. I was not hungry, but sometimes at night I slided in sleep, standing before my bench. Not very pleasant feeling, because I had lot of iron that at any moment could smash my legs. (and these teens made not grams, of course).

    textex - 26-2-2012 at 02:58

    Quote: Originally posted by Bot0nist  
    What?

    Teens in Hungary, or hungry teens? They feel asleep during the glycerine additions:o? I would have to be VERY tired to do that.


    I saw a tv show and it was about Alfred Nobels first nitroglycerine plant in the UK. He had several huts where it was nitrated placed on top small artificial hills. Anyways the guy watching the temperature got a one legged stool to keep him from falling asleep. Nobel didnt trust that several kilos of nitroglycerine would do the job itself.

    inspector071 - 2-3-2012 at 12:02

    I successfully synthesized about 15 mL of NG last night. The synthesis went very smoothly with no noticeable spikes in temperature. I washed it quite a few times with lukewarm water, then sodium carbonate, more water, then concentrated sodium chloride to drive off most of the water. I put two drops of it on a paper towel and was able to successfully detonate it with a hammer. I do have a few questions regarding the stuff, though. Should I desiccate it, or is it relatively stable as is (after removing it from the salt water)? For pretty short term storage will HDPE or PETE containers safely contain it?

    dann2 - 2-3-2012 at 13:35


    I once read in "The story of Dynamite" (I think) that the makers of Nitro were very displeased regarding the bad name that Nitro was getting (accidents etc). When they investigated further they found practices that put there hair on end. Sometimes when large quantities of Nitro got frozen it was known for folks to break it up with sledge hammers.
    Also some used it to oil the wheels of squeeky horse drawn wagons when oil was not available.

    I could imagine getting skilled at falling asleep on a one legged stool. What is needed is a NO legged stool. You simply hold up the board yourself:P

    @inspector071
    A great fun experiment would be the old 'drip Nitro onto a red hot steel plate + drip onto a dull red steel plate".
    I have never read of an accound of someone doing it. Seemingly when the Nitro hits the red hot plate is just fizzles. When it hits the dull red plate it dotonates 'with great destructive power'.

    Has anyone ever heard of anyone actually doing this. Surly a drop on Nitro exploding is not going to do much harm.
    A constand row of drops (I would imagine) would be noisey.


    Dann2

    inspector071 - 2-3-2012 at 13:45

    I'll see if I can try that out, Dann2. I did the anvil test again, but put about 4 drops onto a paper towel this time. I could feel the shockwave pulse through my body gently. It really is powerful stuff. I had donned a pair of ear muffs and a full face mask. I shoot firearms for leisure and the noise of the 4 drops of detonating NG was at least as loud as a powerful rifle. I'm working on setting up a testing rig for small amounts of NG so I can be a little farther back. Gotta have respect for this stuff.

    This is really the first time I've been able to test the detonation of an energetic compound, as my picric acid requires a primary. I've yet to get my hands on some silver or mercury to make silver acetylide and mercury fulminate. My next energetics will probably be some more picric acid, RDX, and ETN.

    Heuteufel - 4-3-2012 at 02:52

    I need some Plugins I don´t have the time to install right now to watch the video, but if my memory serves me correctly, the demonstration you talk about is shown in a very entertaining way in one of the two following videos of the university of Tübingen (Germany) under this link: nitroglycerin demonstration
    I think, it is on the first video under "00:09:30 Nitroglycerin, Eigenschaften (Experiment)", but I´m not sure.

    [Edited on 4-3-2012 by Heuteufel]

    dann2 - 4-3-2012 at 07:13


    Thanks alot Heuteufel,

    It's there as you described.
    Well worth the watch.

    Dann2

    Pulverulescent - 4-3-2012 at 07:49

    The drip clip was fun ─ the demonstrator says OK, when finished and then there's that loud chorus of students asking each other; "what'd he say"???

    dann2 - 4-3-2012 at 08:27


    He wore no ear protection, which I found strange. The demonstrator must have been practically deaf after the event.

    I reckon he said: "Jasus I'm stone fu&*^ng deaf"

    Dann2

    Pulverulescent - 4-3-2012 at 08:40

    Climbing onto the bench to fuck around with nitro seemed fairly steely-nerved too . . .
    I'd've had ze hotplate on ze terra firma myself!

    inspector071 - 4-3-2012 at 11:28

    Still trying to get that video to work. Doesn't seem to like OS X.

    What are the safest storage options for nitroglycerine? So far I have a few mL of it in a tiny glass bottle sitting in a water bath in a location where it won't be disturbed. Is putting it in the fridge a bad idea? I've read that nitroglycerine can become extra sensitive as it starts to melt.

    Also, without having a desiccator, what would be the easiest way to drive off the rest of the water in it?

    killswitch - 7-3-2012 at 11:06

    A saturated solution of sodium chloride will dehydrate nitroglycerin via osmosis. This is the proven procedure.
    You can also dissolve the waterlogged nitroglycerin in acetone, with which water is also miscible. The acetone and water will evaporate an order of magnitude more quickly than the nitroglycerin, which has negligible vapor pressure by comparison.

    For safe storage, dilute it with 40-50% of its volume in acetone or methyl ethyl ketone and store the mixture in an airtight container. Add a tiny speck of concentrated ammonium hydroxide or ammonium carbonate, keep out of sunlight, maintain at a low temperature, and it will keep for a year or more. Wrapping the container in bubble wrap and placing it in a cardboard box enables it to be transported with roughly the same need for delicate handling as glassware (though you obviously shouldn't put explosives in the mail; this is for moving it from a home lab to another location such as a ranch for disposal or testing).

    Do keep in mind, however, that even when diluted this way, it is EXTREMELY flammable.

    Also note that adding water to the acetone/nitroglycerine mix will immediately produce pockets of occluded water within the nitroglycerin, necessitating another drying session.

    [Edited on 7-3-2012 by killswitch]

    inspector071 - 7-3-2012 at 20:39

    I did perform the sodium chloride wash. My NG went from being cloudy as described to a paleish clear yellow. Is that dehydrated enough for practical use? It did detonate when hit with a hammer, but sometimes I have trouble getting it to detonate.

    quicksilver - 8-3-2012 at 08:15

    Quote: Originally posted by inspector071  
    I did perform the sodium chloride wash. My NG went from being cloudy as described to a paleish clear yellow. Is that dehydrated enough for practical use? It did detonate when hit with a hammer, but sometimes I have trouble getting it to detonate.


    That's often what happens when some of the glycerin gets oxidized (the yellowing). Impact testing is difficult due to mildly round surfacing on hammers, etc. That is also why materials in the mg weight range are wrapped in Aluminum foil (wear goggles). NG (very soon after it's discovery) was no longer transported or even stored in liquid form. It was absorbed in clay, earth, carbon, etc for many safety reasons. It was not permitted on public transportation shortly after it's discovery and use and the few times it actually was used as a liquid was in unique setting in the petroleum industry. It's likely to be a much safer agenda to make up an anti-acid absorbent-active base than to maintain it as liquid.

    Heuteufel - 10-3-2012 at 16:44

    Quote:

    It did detonate when hit with a hammer, but sometimes I have trouble getting it to detonate.


    I know a teacher, who used to show that demonstration to his students when talking about inorganic esters. To get a reliable detonation every time he hit it with the hammer, he did the following thing: He placed a small pile of finely ground glass on a paper filter, then added the nitroglycerin (some drops) and then hit it with the hammer. Sucking up a small amount of nitro with a capillary tube and holding the capillary tube quickly into the hot part of the flame of a bunsen burner is also a nice demonstration of the explosive properties of the substance.

    TheMessenger - 24-3-2012 at 22:48

    Anyone here have issues getting NG to freeze? I left 10g of perfectly neutralized and clear nitro at 35-45F for a couple weeks with a desiccant suspended above it and it's still liquid with no crystallization whatsoever...

    Perhaps nitro in a clean clear glass cup needs agitation or to be seeded to begin crystallization at these temperatures?

    simply RED - 25-3-2012 at 03:29

    I remember going to detonate clear NG in a cold winter day. I carried the NG in a 100 ml beher glass, sip it into the prepared container and detonated it. The NG that remained after that on the bottom and sides of the beher glass was frozen... The temperature was about -10 Celsius.....

    killswitch - 25-3-2012 at 08:19

    Freezing nitroglycerin is a bad idea, as the crystals of frozen nitroglycerin suspended in the liquid serve as sources of friction that can cause detonation if shaken. If you want a low-temperature nitric ester, ethylene glycol dinitrate is preferable.

    However, it seems that brownish nitroglycerin is significantly harder to freeze than the pure product.

    TheMessenger - 25-3-2012 at 21:30

    Quote: Originally posted by killswitch  
    Freezing nitroglycerin is a bad idea, as the crystals of frozen nitroglycerin suspended in the liquid serve as sources of friction that can cause detonation if shaken.


    Fear mongering nonsense. Partially frozen NG is only a worry if you have like 50g+ of it where large enough frozen chunks can form to get some real friction going. With small 5-25g amounts there is zero danger.

    quicksilver - 26-3-2012 at 08:26

    Quote: Originally posted by TheMessenger  
    Quote: Originally posted by killswitch  
    Freezing nitroglycerin is a bad idea, as the crystals of frozen nitroglycerin suspended in the liquid serve as sources of friction that can cause detonation if shaken.


    Fear mongering nonsense. Partially frozen NG is only a worry if you have like 50g+ of it where large enough frozen chunks can form to get some real friction going. With small 5-25g amounts there is zero danger.


    " 5-25g amounts there is zero danger".......BULLSHIT!
    SO MANY issues depend upon conditions of detonation that all-encompassing statements do little justice to the power of NG. You're not wearing goggles, the material is encased, etc, etc, etc.. Even moderately soft polymer can rip off a cornea. A gram could blind you very quickly. or strip skin much more efficiently than most other 5-6000 VoD energetics and NG detonates at what VoD????? (Generally an optimum is 7k).

    40% stumping dynamite (active base) made in a 1.25" x 8" stick has roughly 50 grams of NG depending upon the maker and design. A n appropriately detonated stick or "Red Diamond" will pretty much tear off an arm. The last years of US production of non-glycol dynamite was in the 1970's. There were some damn good reasons why NG was pulled from both the industrial and (any) military application(s). An old MkII "Pineapple" hand-grenade had 2 oz (that's LESS that 50gr) of TNT as an energetic. Powdered polymer (or glass) would be fairly tough to remove from human flesh. That is NOT fear mongering - it's fact. Blast wave models of a moderate detonation of NG (let's say 4K VoD) at 5 grams might be easily @ 18" enough to shake the brain casing enough to cause a fatality. Simple blasting cap booby-trap telephones are lethal and that uses less than a gram of energetic.

    See: Eric Prokosch, "The Technology of Killing", "The Science of Wound Ballistics" (same author) 1995, ISBN 5571 558,2

    Putting any "weight" on the relational "safety" of an energetic material is uninformed, unprofessional, & illogical..... It's NOT the weight of an energetic materials but the conditions of it's detonation in relationship to a living being that determines it's potential danger.





    [Edited on 26-3-2012 by quicksilver]

    chemicalmixer - 26-3-2012 at 18:07

    Would it be possible to create NG by first forming an alkoxide with lithium and glycerol, and then to this adding a solution of NH4NO3 dissolved in methanol?

    simply RED - 26-3-2012 at 22:08

    Indeed NG is surprisingly more powerul than the other 5-6000 VoD energetics!
    This comes from the higher energy of detonation of NG, about 6.5 MJ/kg compared to 4-5 MJ/kg for TNT, ANFO, etc...

    In fact NG is one of the most powerful chemical energetics that could theoretically exist!

    [Edited on 27-3-2012 by simply RED]

    Pulverulescent - 27-3-2012 at 02:13

    Yes, NG comes quite close to nitroglycol in power, brisance and explosion temperature . . .

    killswitch - 27-3-2012 at 07:13

    Quote: Originally posted by chemicalmixer  
    Would it be possible to create NG by first forming an alkoxide with lithium and glycerol, and then to this adding a solution of NH4NO3 dissolved in methanol?


    Uhh, I think you'd just get lithium nitrate, glycerol, and anhydrous ammonia.

    [Edited on 27-3-2012 by killswitch]

    killswitch - 27-3-2012 at 07:17

    Quote: Originally posted by quicksilver  
    Simple blasting cap booby-trap telephones are lethal and that uses less than a gram of energetic.


    To be fair, phones large enough to cram blasting caps into are pretty much obsolete.

    /I'm feeling old.

    grndpndr - 3-4-2012 at 16:24


    Better Old than Obsolete

    Hennig Brand - 15-4-2012 at 13:54

    Even in some of those new super slim phones I am sure a motivated person with a little ingenuity could find (or make) a cubic centimeter of space to stuff some suitable high powered energetic material. That is really all the space you would need to conceal more than a gram, which would be more than enough to kill given the proximity to the side of the victims head and ear when it goes off. Remember the explosive configuration doesn't necessarily have to be the same as a standard blasting cap either.

    I have been thinking a little bit lately about what a pain neutralizing the residual acidity in NG is. Two summers ago an older relative and I did some granite rock blasting. I made a bunch of ammonia dynamite for the job. I made ammonia dynamite with 15-20% NG, so a little NG went a long way. We drilled bore holes which when loaded and then topped up with crushed rock had perfect confinement. With strong confinement like this even relatively slow dynamite works just fine.

    Anyway, I made a really big batch of nitro because we had a lot of rocks to blast. Each rock was over 15 tonnes and I was using one 100g charge per rock. We didn't want the rock pulverized, just broken into 2 or 3 pieces. The batch of nitro I made was over 200g which was a bit nerve racking, but I was very careful. I remember the worst part was that it took days to get the residual acidity in the NG neutralized, which was very inconvenient to say the least.

    The problem is lack of good agitation of the NG and circulation of the sodium bicarbonate solution. The NG normally just sits there in a blob and only the outer surfaces are exposed to the bicarb solution. I have always done what most everyone else does and do a certain amount of manual swirling from time to time during the neutralization stage of the process. I found with a 200+g batch even with quite a lot of manual swirling it still took days to get the residual acid in the NG neutralized.

    I think I have one possible solution. This may be a little risky because of the possibility of small amounts of NG getting into the pump impeller area, but remember this process could always be turned on and off remotely if it was deemed necessary.

    Basically a small beaker (another type of container may be more suitable) sits inside a larger beaker. The NG sits inside the smaller beaker inside the larger beaker. A suitable quantity of sodium bicarbonate solution is added to the beakers. A small centrifugal pump like the ones used for table-top type fountains pumps the bicarb solution from the larger beaker into the smaller beaker, with the overflow from the smaller beaker flowing back into the larger beaker. There is constant circulation of the bicarb solution and constant agitation of the NG.

    The flow of bicarb solution does an excellent job of rolling the NG blob around exposing fresh surfaces, greatly facilitating the acid neutralization process.

    Again, this may be best turned on and off remotely and kept clear of while in operation.

    BTW, the NG was made today from fertilizer and reddish-orange drain cleaner which is why it has some crap from the
    fertilizer in it and is also colored a bit.


    NG from AN 1.JPG - 210kB NG from AN 2.JPG - 214kB NG Neutralization 1.JPG - 242kB NG Neutralization 2.JPG - 238kB NG Neutralization 3.JPG - 228kB



    [Edited on 15-4-2012 by Hennig Brand]

    Pulverulescent - 15-4-2012 at 14:26

    It might be simpler and safer to run cold water into NG in a tall beaker in the sink, overnight.
    Adjust the rate of flow so that fairly vigorous agitation is provided, but not enough to make the NG rise from the bottom of the container.
    The over-flow water will contain a certain amount of acid and a more complete wash should be achieved.
    Bicarbonate solution removes less HNO<sub>3</sub> than one might expect but replacing the solution every ten minutes isn't practical . . .

    Hennig Brand - 15-4-2012 at 14:58

    I thought of that at first but then remembered NG is actually fairly soluble in water. Nitroglycerin is soluble enough that if put in a beaker with the water constantly being replaced, in short order it would all dissolve and end up down the drain with the water, bummer.

    Solubility information for NG is in this data page.
    Attachment: Nitroglycerin Data Page.pdf (566kB)
    This file has been downloaded 828 times

    Taken from the pdf:

    Water Solubility (g/L)

    Temperature........Solubility
    20C.......................1.38-2
    40C.......................1.68
    60C.......................2.36
    80C.......................3.44

    I am not sure how accurate these numbers are, but even if they are approximately accurate the data illustrates the issue with using a large excess of water.

    The little pump I have has a slide valve type thing on it, so the flow can be regulated. I had it turned most of the way down so that the NG was not flushed right out of the smaller beaker into the larger beaker.

    It’s the residual H2SO4 that we are more concerned with I think, but yes the HNO3 is also a concern.

    With regards to the agitation from the flowing water causing the NG to rise up, I found it wasn't much of a problem at all. At the very start the little bit of NG that was originally floating, floated off into the larger beaker. With a reasonably slow flow rate very little more than what came over at the start ended up in the larger beaker.



    [Edited on 15-4-2012 by Hennig Brand]

    Pulverulescent - 15-4-2012 at 15:34

    Quote:
    Nitroglycerin is soluble enough that if put in a beaker with the water constantly being replaced, in short order it would all dissolve and end up down the drain with the water, bummer.

    Yes . . . Now that you mention it, I can see how that approach would be problematic!

    watson.fawkes - 15-4-2012 at 16:17

    Quote: Originally posted by Hennig Brand  
    This may be a little risky because of the possibility of small amounts of NG getting into the pump impeller area, but remember this process could always be turned on and off remotely if it was deemed necessary.
    I imagine you could use a bubble pump for this, and it has no impeller. Put the inlet in the aqueous phase the mixture and run the outlet into a funnel whose inlet is above everything. Put the outlet of the funnel at the bottom of the mixture.

    Hennig Brand - 15-4-2012 at 17:42

    That funnel idea of yours sounds like a good one, I am going to try that.

    Regarding the pump, the fact that it has no impeller sounds good. I think this is the first time I have heard of one of these, sounds exotic.

    Is this something practical, or a scientific curiosity of some kind?

    The couple examples I came to first while googling bubble pump involved very complex systems with phase changes, vacuum pumps, specially designed chambers and all sorts of neat stuff.

    Did you have something simple in mind? I admit I am not familiar with this at all.

    edit:

    A Peristaltic Tube Pump might be better than the small Centrifugal Pump I am using. No impeller but it might have its own issues.

    Centrifugal pumps come in many different types and made of many different materials. A centrifugal pump that had all it's internal parts covered in teflon would be good, and they do exist.

    The pump I am using is something that was pulled out of a junk pile, but it does work and is cheap. These small table-top fountain pumps are readily available, which is something which should not be discounted either.



    [Edited on 16-4-2012 by Hennig Brand]

    watson.fawkes - 16-4-2012 at 05:27

    Quote: Originally posted by Hennig Brand  
    Is this something practical, or a scientific curiosity of some kind?
    Well, coffee percolators use a bubble pump to move water from the lower chamber to the upper one (see this link), and it's not like they're exotic or anything. In that case the pumping gas is steam, so it can use heat as the driving energy source. Similarly, they're used in ammonia absorption refrigerators, since they're already heat-driven. They're not used widely, since their behavior depends upon pipe dimensions, viscosity of the fluid being pumped, etc. But their ideal scale is exactly the one you're working at, so that's fine.

    A bubble pump driven by an air pump need be nothing more than an inlet tube with an air injection port somewhere above the inlet. The injection port need be little more than a pipette tip. My only particular advice is to have a variable speed air pump one way or another, perhaps with a little pressure regulator, because it's easier to vary the air flow for optimum pumping rate than to vary the pipe diameter or the viscosity of your aqueous phase.

    Hennig Brand - 16-4-2012 at 10:51

    Ok, yeah I am starting to get the idea. This is very cool. I am seeing a lot of stuff online now on air-lift water pumps, I assume this is the same sort of thing. I could probably just use an aquarium bubbler with check valve and a small airflow control valve and a bit of tubing.

    If you have any more pointers let me know.

    edit:

    This afternoon I did a little experimenting. I used an aquarium air pump and vinyl tubing, which does work, but the pump is sort of underpowered and the water is coming out in little spurts. There is probably a way to design this so there is more of a continuous stream of water. I think I read somewhere that the air bubbles should be kept small.

    I used a small air line tee fitting in the following configuration(more or less).

    Return to Reservoir
    |
    |
    |
    |
    |
    |-------From Reservoir
    |
    |
    |
    Air in from aquarium air pump



    [Edited on 16-4-2012 by Hennig Brand]

    Ral123 - 17-4-2012 at 03:37

    Why neutralize that much for 20% ammonium dynamite to be used the next day? I personaly (for egdn) place 20-30ml in a beaker with 100ml water. With 50cc syringe I suck water and blow it fast into the thing.

    Hennig Brand - 17-4-2012 at 09:12

    It wasn't all used the next day, but yeah neutralization doesn't need to be very thorough at all if it is going to be used immediately. It maybe didn't need to be so thoroughly neutralized but it was a safety precaution.

    The rocks were blasted over a 1 to 2 week period, different rocks different locations. The person I was working with was using the rocks for shoreline preservation, or rip rap I think they call it. Any rocks over 12-15 tonnes and dependant on location were just too big for the loader.

    In the end a couple more charges were needed so a little more was made and a very quick and dirty neutralization was done and the NG used on the same day.

    For me the most annoying but necessary part of a NG synthesis, if it is to be stored for any length of time, is the neutralization. A circulating bicarb solution wash & agitation has potential I think.

    I am looking into the bubble pump thing right now because it has no moving parts that could potentially set of the NG. The results of using the centrifugal pump were very positive. When using the centrifugal pump from the table-top fountain a very thorough acid neutralization, of ~15g of NG, was done in 20 minutes or so. I would normally be messing around for a day or more, with occasional swirling, trying to get it neutral with even 15 grams.

    The very first time I made NG I had no clue what I was doing (very bad move!). I made it no problem but I hadn't learned yet that the residual acidity had to be neutralized. I think I washed it once with water or something. When I went out the next morning to check on the 10g or so, it was boiling and spewing red fumes. I immediately disposed of it, and the experience left an impression. If that had been a large amount, it would have been a bad situation.



    [Edited on 17-4-2012 by Hennig Brand]

    Ral123 - 17-4-2012 at 10:18

    Why more west type guys love NG so much and the guys from the east (russian pyros) like egdn much more? :cool: May be no NG with 60% nitric :D

    caterpillar - 17-4-2012 at 12:58

    Quote: Originally posted by Ral123  
    Why more west type guys love NG so much and the guys from the east (russian pyros) like egdn much more? :cool: May be no NG with 60% nitric :D


    My proposition: russian boys live in the cold country, therefore they want to use something with lower melting point, than NG. It may be joke, but my friend (same person, who made 1.5 l of NG at once), used in fact mixture of glycerol and EG to lower melting point of resulting product. It was in a forest in a spring and he used snow to cool basin with mixed acid.

    Hennig Brand - 17-4-2012 at 16:13

    I live in Canada and it gets pretty cold a lot of the time. I have made EGDN a few times, mostly just to mix with NG on those cold days. I like NG, which may be just because I am more used to it. A few positive attributes of NG as I see it are its higher density, higher viscosity, lower solubility and lower vapor pressure. All that being said EGDN is great stuff in colder climates, where pure NG often can't function at all. Apparently EGDN doesn't suffer from low order detonation, which can be a real problem with NG if not initiated properly. They are both good, just different.

    I have seen people write than EGDN is more storage stable than NG. I wonder how much more?



    [Edited on 18-4-2012 by Hennig Brand]

    Ral123 - 17-4-2012 at 20:48

    6 months old sample looked good, till I got rid of it :D NG would be perfect dream if it was stable...

    Bot0nist - 17-4-2012 at 21:47

    Six months with no deterioration sounds stable to me. I think your confusing stable with sensitive to stimuli. Stable implies chemical stability, not susceptibility to explosive decomposition from various stimuli.

    Hennig Brand - 18-4-2012 at 03:08

    So EGDN is known for being less sensitive in terms of explosive initiation, not storage stability? I think I have heard both, but I could be wrong.

    The longest I have ever stored a sample of NG was about 3 years. It was very well washed and ~all acidity well neutralized. When it was made it was nice and clear because I used boiled down electrolyte for H2SO4, HNO3 and nice clear glycerin. It was kept in a fairly dark location with no direct sunlight and kept fairly cool (below 22C at all times). After 3 years it was still perfectly clear and had excellent performance when I did eventually use it. If NG is well neutralized and stored with a bit of care it seems quite storage stable.

    I am in too much of a rush right now to find a reference but isn't there a sample of nitroglycerin that is really old (like 100 years or something) stored by the Nobel scientists at a museum or something. I think it is taken out and checked periodically and any formed acidity neutralized, but it is still really old.




    [Edited on 18-4-2012 by Hennig Brand]

    Bot0nist - 18-4-2012 at 06:28

    Yes, that is correct about the old sample. When properly stabilized and neutral it would seem it could be stored indefinitely.

    Hennig Brand - 18-4-2012 at 07:22

    Yeah, NG is quite stable when treated properly however,

    Regarding EGDN stability vs. NG stability

    This is from Wikipedia, not the best reference but they are usually right, and it makes sense.

    "It (EGDN) is considerably more stable than glycerol trinitrate owing to the lack of secondary hydroxyl groups in the precursor polyol."

    I still like NG though, mostly because of the handling properties.



    [Edited on 18-4-2012 by Hennig Brand]

    Hennig Brand - 19-4-2012 at 09:00

    Here is a snip-it from the section on laboratory synthesis of NG in Nitroglycerin & Nitroglycerin Explosives by Naoum.

    Lab Purification of NG from Naoum.jpg - 51kB

    It sounds like at higher temperatures (40-50C) and manually "shaking" the NG in bicarb solution the acid neutralization is trivial (few minute process).

    Sounds too easy but maybe it is. I think I still like the idea of having an automated acid neutralization process and being well away from it during the agitation.




    [Edited on 19-4-2012 by Hennig Brand]

    quicksilver - 19-4-2012 at 13:04

    In his book ("Nitroglycerin & Nitroglycerin Explosives by Naoum"), I believe in chapter 7 he has some "Plant Lay-Outs" & brings up some concepts that have been used successfully for many decades. The use of compressed air for mixing had apparently been common (& safe) in Europe as well as a contact wash with a carbonate and saline water. There is a sharp separation of the nitrated glycerin and acids even down to 10% (according to Naoum) & apparently this presented a problem during that time as serration funnels had no Teflon for the development of the petcock. However even with such a mechanism I had thought it wise to rotate the valve several times prior to active separation. He quotes 1.6 for NG (at that time) due to fatty acids yet today's glycerin sources may be so pure as to reduce that figure.
    One challenge with EDGN is that it's substantially more viscous (than NG) & separation is somewhat more troublesome without a very bright background light.

    Hennig Brand - 19-4-2012 at 13:34

    Sounds good, I will read those parts right away. I haven't yet sat down and read the whole book, just skimmed it. Reading it all the way through is on my to do list, it is a very interesting book.

    I think NG is more viscous than EGDN though. The more viscosity, or the more resistance between layers if you will, the harder it is to pour etc.


    Edit:
    I see what you mean (I think), the EGDN would be much harder to separate from water because its viscosity is so much closer to that of water.

    I found another NG data page from a company that makes NG amoung other nitric esters.

    Attachment: NG Data Page 2.pdf (17kB)
    This file has been downloaded 767 times

    Notice the viscosity of NG is stated as 36 cP at 20 C, and water is close to 1 cP at 20 C I think. Quite a difference.

    Here is a reference for the viscosity of EGDN.

    EGDN Viscosity:
    4.2 mPa.s at 20 deg C --->(1 mPa.s = 1 cP)
    [Kirk-Othmer Encyclopedia of Chemical Technology. 3rd ed., Volumes 1-26. New York, NY: John Wiley and Sons, 1978-1984., p. V9: 573 (1980)] **PEER REVIEWED**


    And also for NG from the same source.

    NG Viscosity:
    36.0 centipoise @ 20 deg C
    [Kirk-Othmer Encyclopedia of Chemical Technology. 4th ed. Volumes 1: New York, NY. John Wiley and Sons, 1991-Present., p. V10 (1993) 22] **PEER REVIEWED**



    [Edited on 20-4-2012 by Hennig Brand]

    quicksilver - 20-4-2012 at 10:43

    Remember however that's a really old text. (I think) the glycerin was from the soap industry and somewhat impure. It may be that was one reason why we can achieve such a clean final product; in that the starting material has few impurities.
    The toughest separation (visually) I had seen was propylene glycol - unless you have the brightest of lighting it really tough to see the layer. Amyl Acetate and ethanol appear to layer separate double-base smokeless powder However the graphite in some samples make virtually any movement "muddy-up" the division.
    I am guessing at this but I think that the only NG manufacturing done in the USA may be for DBSP. I had a very fine pipette unit that could draw off the layer without disturbing the other materials and the NG blotted in paper as fast as EDGN.

    Hennig Brand - 20-4-2012 at 15:10

    Feel free to point out any mistakes in my theory, there probably are at least a few.

    This is what I remember from a class last year and a little googling right now.

    I don't know that much about it but I think when a liquid blots or soaks up in cellulose material it has a lot to do with the bonding between the liquid and the cellulose.

    As an example, since cellulose is unsaturated and has the hydroxyl groups it bonds well with water. This is primarily because of Hydrogen Bonding between the water and the cellulose. Put a little water at one end of a dry cotton cloth and it will soak or spread along the cloth because of the weak bonds between the water and the cellulose/cotton. On the other hand if you put a little gasoline, which is a saturated hydrocarbon (no hydroxyl groups), at one end of the same dry cloth it will not spread very well because the bonding forces aren't there.

    NG and EGDN both have hydrogen together with nitrogen and oxygen which means they are polar and there is hydrogen bonding between molecules for both esters. There is also hydrogen bonding between them and other polar molecules.

    Maybe what you are seeing has something to do with different bond strengths between the cellulose/paper and the NG and EGDN. I am assuming it would be a little different for NG and EGDN.

    The Viscosity of the nitric ester would also affect the flow rate into the cloth or paper as well I think. Higher viscosity, higher resistance to flow.


    Edit:

    I wasn't thinking. NG has very low water solubility, so I guess that makes it only very slightly polar. EGDN is much more water soluble than NG, making it more polar. It would make sense that EGDN would blot into paper/cotton faster for this reason.

    I suppose the electronegative N's and O's are not bonded directly to the H's in either NG or EGDN.

    The impurities in the old fashioned glycerin would be saturated, very nonpolar, fatty molecules which if present in the NG made from it would cause the NG to not blot into cellulose/paper as quickly or as thoroughly. I see what you are getting at, but it took a while.



    [Edited on 21-4-2012 by Hennig Brand]

    Hennig Brand - 22-4-2012 at 03:54

    You know the more mono & di-nitroglycerine that is present in a sample of NG would also case the sample to blot more quickly into paper. This is basically the same reason the lower nitrates of NG are more soluble in water as well, the hydroxyl groups.

    I guess most of the lower nitrates would be dissolved/ washed away during the washing, but the saturated impurities wouldn't be.


    MNT from NG Synthesis Spent Acid

    BTW, has anyone used the spent acid from NG manufacture to produce Mono-Nitrotoluene. I was reading about it in Naoum, so decided to give it a try. It works beautifully! The nitration of Toluene is not an equilibrium reaction like an esterification reaction is (NG), so the water in the waste acid isn't much of a problem. More than 95% of the remaining nitric acid in the waste acid can be utilized when used to nitrate toluene to MNT.

    I suppose the waste acid from NG manufacture could be used to nitrate other aromatics as well.

    Here is a picture of the MNT made from 75 mL or so of spent acid from a NG synthesis. It is being washed in water. I will probably nitrate it to at least DNT, so the intermediate washing probably wasn't needed. The MNT could be used as is to make a Cheddite or Sprengel explosive (?) with potassium chlorate. The DNT/chlorate explosives are more powerful and make better use of materials than the MNT/chlorate types I think. It is also very easy to get high yields of DNT without the strongest of acids. With TNT it is a little more difficult to get good yields (I think).

    MNT from spent acids.JPG - 213kB



    [Edited on 22-4-2012 by Hennig Brand]

    quicksilver - 23-4-2012 at 10:59

    I've tried a 2-pot synthesis that worked out fairly well (it's posted back a few years ago). Because it's mp was 80C and it had cleaned up a tan-beige, I was surprised. I started out with bright yellow long (2cm) needles that were vivid yellow before a H2SO4 wash. I've tried many one pot labs and never got tri-nitrated material.

    Hennig Brand - 23-4-2012 at 17:51

    Thats interesting. I attempted TNT before using AN and H2SO4, but the product I ended up with had a melting point below 70C. I later read that even very small amounts of DNT lower the melting point of TNT a lot.

    The main focus of my last post was on using the left over acid from a NG synthesis to nitrate toluene to MNT. That is how the MNT in the above picture was made, from spent mixed acids from a NG synthesis.

    Hennig Brand - 23-5-2012 at 08:56

    I mentioned doing some rock blasting on the last page of this thread. I found some of my old pictures. Here are 3 views of one of the more successful blasts. It was a successful blast because the rock was broken into three large pieces and not a bunch of smaller ones. Large pieces were desirable because of what the rock was to be used for. The whole rock was just too big to move in one piece with the available equipment.



    Split Rock 1.jpg - 519kB Split Rock 3.jpg - 473kB Split Rock 2.jpg - 462kB


    BTW, IIRC the granite rock was about 15 tonnes and the charge used was 100g of 20% ammonia dynamite. If I was to do it all over again I would try only 10% ammonia dynamite, which I think might cut down on the amount of smaller pieces produced. This particular blast was successful however, with no excessive shattering of the rock.

    [Edited on 23-5-2012 by Hennig Brand]

    Vikascoder - 2-6-2012 at 09:52

    is it possible to make dynamite with fullers earth by absorbing bitroglycerine in it or by absorbing nitroglycerine in sand which is used for construction purposes

    Hennig Brand - 3-6-2012 at 08:58

    From the little bit I have read about it, fullers earth sounds promising. It is apparently a very good absorber of many things. The COPAE (p 332) implies that diatomaceous earth and fullers earth are the same thing. Reading modern descriptions of both clearly shows that they are similar but not the same. Apparently fullers earth varies in its composition from source to source as well. It does sound like it is used for many of the some purposes as diatomaceous earth though, which is promising.

    Mixing sand with NG sounds like a good way to reduce your life expectancy. Sand has low porosity and absorptive qualities and is also hard and gritty. Mixing liquid NG with hard gritty things is a bad idea!

    There are many materials in modern times that can be used to absorb NG. The first really successful absorbent, which is also naturally occurring, was diatomaceous earth. Alfred Nobel discovered that is could absorb several times its weight in NG.

    The follow is a copy/paste from the Wikipedia page on diatomaceous earth.

    "Diatomaceous earth also known as D.E., diatomite, or kieselgur/kieselguhr, is a naturally occurring, soft, siliceous sedimentary rock that is easily crumbled into a fine white to off-white powder. It has a particle size ranging from less than 1 micrometre to more than 1 millimeter, but typically 10 to 200 micrometres. This powder has an abrasive feel, similar to pumice powder, and is very light as a result of its high porosity. The typical chemical composition of oven-dried diatomaceous earth is 80 to 90% silica, with 2 to 4% alumina (attributed mostly to clay minerals) and 0.5 to 2% iron oxide."

    [Edited on 3-6-2012 by Hennig Brand]

    Vikascoder - 6-6-2012 at 18:20

    Friends i started with 8 ml of normally glycerin to make nitroglycerin . I completly neutralized and washed it with water . But my finally product is 15 ml which also contains water . How could i dry my nitroglycerin completely.

    Fossil - 6-6-2012 at 18:43

    Put it in a saturated salt (NaCl) solution.

    Vikascoder - 6-6-2012 at 23:27

    I have already put it in NaCl solution . After that i got 15 ml of nitro glycerine . Now without further drying or desicating i just tried to detonate it by dipping a piece of 1 cm square of paper . It detonated with a very nice bang when hit with hammer. I think there is no further need to dry it . It is ready to be used as explosive.

    Hennig Brand - 9-6-2012 at 10:20

    I used to use a saturated NaCl solution to dry NG, but I find now that it is usually just extra bother to do so. If one is not too impatient, simply exposing an open container of the wet NG to the open air for a while will dry it fairly quickly. NG is very non-polar, and bonds only very weakly with water. I usually just leave some NG out over night in a beaker and by morning it is nice and clear and dry. Don't worry about losing NG, as it has very low vapor pressure at room temperature.

    [Edited on 9-6-2012 by Hennig Brand]
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