Sciencemadness Discussion Board

nitroglycerin

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andrea - 21-9-2003 at 03:17

Hi guys, I'm gonna make some nitroglycerin for the first time. I've got only 65-70% concentrated HNO3 and 96-98% concentrated H2SO4. In the megalomania's procedure they use 98% HNO3 and 98% H2SO4 in a 2:3 ratio. I wanna know if using a nitrating mixture with a different ratio of HNO3/H2SO4 I will be able to get successfully some NG. If yes what ratio of HNO3/H2SO4 should I use (with 65-70% HNO3)? Thanks for your answers

Basement Chemist - 21-9-2003 at 04:28

How much do you consider some? You can get a little, but if your just doing it on guessing, I would recommend planning it out first or just synthesize something else... because if you mess up that synthesis....

andrea - 21-9-2003 at 05:39

I don't wanna do too much NG. For the first time 2 or 3 ml are enough. I'm not gonna make it without a precise plan. Indeed the only thing I've to know is (if it's possible) the HNO3/H2SO4 ratio if my HNO3 is 65-70% concentrated (and, of course, the related amount of glycerol I should use)

palpy - 21-9-2003 at 08:52

use 30ml of HNO3 (65%) and 45 ml of H2SO4 for every 10ml of glycerine

and make it at least of those 10ml glycerine - the risk would not be considerably higher
2 to 3ml NG is nothing ;)

andrea - 21-9-2003 at 11:14

Thank you for the advice. But I considered it and your ratio is the same of Megalomania's. In fact 200:300 = 30:45;
the only difference is that megalomania's method uses 98-100% pure nitric acid while you use 65% NA. Are you sure it's the same thing? I thought the HNO3/H2SO4 ratio should change when acid concentration changes...

palpy - 21-9-2003 at 13:46

haven't done it myself, but a guy i know synthesized NG succesfully with this ratio.
the hint is intensive cooling and adding the glycerine DROP BY DROP
the yield should be about the volume of glycerine you started with (i'dont have the specific masses here at the moment, but i'm sure you can handle this :)

DDTea - 21-9-2003 at 18:46

Not related to the Nitric Acid... but just some common safety tips. 10 ml of Nitroglycerin can kill you, so be careful. Neutralizing the Nitroglycerin is extremely important- as I'm sure you know already from reading Megalomania's synth. Nevertheless, I still feel it necessary to hammer the point in :).

If the synth goes wrong and the reaction overheats, chances are it won't explode- you'll just get some nasty NO2 fumes. And finally, be patient with the Glycerin! Adding drop by drop does get boring, and can take a while. But for the sake of your safety, don't rush.

a123x - 21-9-2003 at 21:37

I thought that NG would work fine with around 68% nitric acid. It works okay with mixed acids although the yields aren't spectacular(around 22g using 1.5 times the amount of acid stoichiometrically necessary for 40g and the stoich amount of glycerin for 40g). If your acid doesn't work just try mixed acids.

Microtek - 22-9-2003 at 02:50

Using the ratios given by palpy may give an undesirably high concentration of glycerol dinitrate in your product which will look like NG and explode if whacked with a hammer, but is quite inferior to pure NG.
For this reason, I recommend these ratios: 1 mL glycerine to 4 mL 62 % HNO3 and 6 mL 96 % H2SO4.
This corresponds to directions given by one of the old timers on the EW forum who was working in a lab that would sometimes need a little NG for unspecified testing.
They used 1 mL glycerine to 4 g NH4NO3 and 6 mL H2SO4 ( but this mix tends to freeze when cooled to around 0 C ).
Anyway, a good process for neutralizing NG is to add the crude product to about ten times its volume of bicarb soln and let it sit for a day with occasional swirling.
After this period, the NG will have absorbed considerable amounts of water and will appear milky. This is fixed by adding it to a saturated soln of NaCl in water and swirling it occasionally until clear.

the timeless - 24-9-2003 at 00:59

Do this synth in a well ventilated place or outside. This will reduce drastically your first-timer headaches. And by the way, you can do it with much smaller amount of H2SO4 if you have lots of time to wait the reaction to complete. If I remember right in nitration processes the sulfuric is always used only to start the reaction and tho catalyze it. So the amount is only a matter of time.

Microtek - 24-9-2003 at 04:34

The amount of H2SO4 should not be decreased. In nitration reactions of this kind, the sulfuric acid serves to dehydrate the nitric acid ( and to scavenge the water that is produced in the esterification of the glycerine ), thus effective ly increase the concentration of the nitric acid. As you know, HNO3 in high conc. is a nitrating agent, while low conc HNO3 is mainly an oxidizer.
So, using too little H2SO4 will lead to more oxidition and, at best, an inferior product or, at worst, a runaway with NOx plume, acid splatter, etc.

andrea - 26-9-2003 at 11:35

Hi! Today I've made 3ml of nitroglycerin (or what I think it was) using Microtek's directions (1ml of glycerol in 4ml 65%HNO3 and 6ml 96%H2SO4). After adding all the glycerin I allowed the mixture to sit for 15 minutes monitoring the temperature at all times. I washed it as explained in Megalomania's method and I obtained a clear oily liquid. I drained off the water but didn't dry my NG, only drained off all the water I was able to drain off (I thought that the NG collected on the bottom of the cilinder was water free, specially after having washed it with a concentrated sodium chloride solution). So I tested it.
At first I put a drop of NG on a flame; it didn't burn unless I kept it on the flame: indeed while I was keeping it on my "Bunsen" a blue flame formed but only for fractions of a second. "Perhaps it is too a little amount of NG" I thought.
Then I let a drop of NG fall on the ground from a height of 5 feet: nothing happened.
At the end, raped by desperation, I tried to hammer it six or seven times: it detonated only twice. I worked always with a drop of NG: is this the matter? What should happen if a drop falls on the ground? Should it detonate? And what should be the behaviour of NG on the flame? Had my NG a normal behaviour? If not, why?

Haggis - 26-9-2003 at 12:58

Nitro should NEVER explode when a drop falls all of 5 feet. Also, here is a nice page with NG burn tests. http://www.geocities.com/brainfevert/tests.html

Microtek - 28-9-2003 at 07:56

When doing the hammer test, the NG must be absorbed into a piece of toilet paper. Otherwise, the hammerblow will more likely just scatter the NG as little droplets.
Generally, people who have experience with organic peroxides are surprised at how relatively difficult it is to make NG explode.

vulture - 28-9-2003 at 12:19

Andrea, you mention you "washed" your NG with sodiumchloride, but it's not clear if you neutralized your NG, which is EXTREMELY important.

andrea - 1-10-2003 at 11:27

Of course I did it. I think I've found NG particularly difficult to set off perhaps because I was used to work with acetone peroxide (the first and last explosive I've ever made) which was much more sensitive (and dangerous I think...)

Nevermore - 2-10-2003 at 11:21

I am planning to make NG too however i have to make it with NH4NO3 and sulfuric acid because is extremly hard to find nitric acid here. I was looking for some webpages that show step by step about the nitration of glicerine, i dun wanna start with a runaway nitration!
Beside that, i will try to nitrate sugar, mannitol, and glucose too, but like before, i don't have a good web guide to help about that..

I will start tonite, i hope i won't drown in deep brown fumes!

[Edited on 2/10/2003 by Nevermore]

andrea - 3-10-2003 at 11:09

Where do you come from? {Da dove vieni? (se preferisci l'italiano...) Forse ti potrei dare qualche informazione su dove trovare l'acido nitrico} Perhaps I may help you to find some nitric acid!

Nevermore - 5-10-2003 at 03:19

dal sud, isole.
credo che mi arrangero' con il nitrato di ammonio e l'acido solforico..cmq se sai qualcosa...

im coming from the south, islands.
i think i will just go on with AN and sulfuric acid...

NG and diatomaceous earth

chemoleo - 5-10-2003 at 16:14

Hi,
I found a source to obtain diatomaceous earth from. REalising that it has been used as the first dynamites ever, when soaked with NG, I wondered whether anyone has experience with it. Diatomaceous earth is a zeolithe, a SiO2 based substance with an extraordinarily high surface area, thus it is extremely capable of absorbing virtually any material, in this case NG. Also, I read that it sweats NG after a number of months (hence it is not used anymore these days), but for immediate use it is apparently totally safe to use.
Anyway, did anyone have some experience with it?
Cheers

Nevermore - 9-10-2003 at 13:14

I need some info about which temp to perform the synth, i planned to use a small becker inside a large ice bath, but the freezing point of the NG scares me, it is just 13C so most probably i will end up below that temp. Is that safe to nitrate glycerine at that temp or should i care not to go lower than 15°C (that will be much harder)? Also should i avoid to mix with a glass rod, or use a wood one, or just swirl around? i will be using 58% HNO3 since i can't access higher conc one..

Iv4 - 13-10-2003 at 02:38

I think I can help out a bit here.On BS theres a thread dedicated to this and I know how some of you feel about it but theres a lot of experiance with it at this link.

Also h2so4 and nh4no3 seems to give better yields and were looking into using nitrogen dioxide.

Nevermore - 13-10-2003 at 06:25

uhm my opinion is that HNO3 gives better yelds for sure than NH4NO3..
Anyway, is worth a trial.

Iv4 - 14-10-2003 at 04:37

I have a rough theory since sodium nitrate is better than potasium(it was tried out along time ago-bad ideas).I think that metal's interfere with the reaction.That would explain NaNo3 working better than KNo3 and nh4no3 woeking better than both.Though it could be a side effect of the the heat.THis line of thinking sugest like you sai than Hno3 would wok the best.But I really dont know much about chemistry.

Theoretic - 14-10-2003 at 06:27

By the way, if anyone is interested in how to get the precursor glycerine, it goes (supposedly) like this:
(sunflower) oil+Ca(OH2)=>
=>glycerine+calcium soap
(water- insoluble, so I suppose
glycerine-insoluble as well).:cool:

chemoleo - 14-10-2003 at 07:52

of course, this is how glycerol is obtained industrially. They use di/tryglycerides from vegetable fats, and boil it with NaOH, causing the ester bonds to be hydrolysed. The resultant glycerol is distilled off, and thus obtained at relatively high purity...

Backyard Blaster - 14-10-2003 at 10:40

Pardon my lack of knowledge, but is vegetable glycerine the kind you would look for when making NG? I notice that's its readily available, at least here in Canada.

Nevermore - 14-10-2003 at 12:14

i think is readily available almost worldwide, i don't see how can they take out of free market a so common substance!

Backyard Blaster - 14-10-2003 at 15:05

Yeah that would seem kind of ridiculous, but the way things are getting legislated these days, it wouldn't surprise me.......

Theoretic - 15-10-2003 at 04:37

What I wanted to say is just that the Ca(OH)2 method is more convenient for laboratory preparation, since all you have to do after the reaction has finished is pour off the glycerine.:cool:

Nevermore - 15-10-2003 at 11:42

well, as long as the glycerine will be available is cheaper to buy it. It will be already pure and dehydrated, comes in very convenient tanks, and has lotsa of use, i used once to make soap!

Mumbles - 15-10-2003 at 13:25

If you use vegetable glycerin it should make any difference. The animal/plant/wherever else its made is just the source. Just make sure its dry. Theres a method on Rhodium's site in the making Formic Acid from Oxalic Acid and Glycerin file.

inkognito - 22-10-2003 at 05:28

guys , i need some help . i am going to make NG , in small amounts . about 7.5 grams . well i will try to make it with DavidThePyro's procedure , he uses

30mL 95% H2SO4 (sulfuric acid)
20g NH4NO3
5mL glycerol (pure glycerin)

well , he still didn't try to make it , so i want to ask you guys is this ok ? can i use smaller amounts of NH4NO3 and H2SO4 ???? becose i have small amounts of this at home , and getting it in my place is realy hard .

Theoretic - 22-10-2003 at 06:32

Not that I actualy used the method, first I came up with the idea, then I searched the net. Nothing definite, just bits and pieces and hints. A minute ago I repeated the search - nothing definite again, but hints that the process goes. :):(

inkognito - 22-10-2003 at 07:15

ok ,so this synth is ok. i wanted to be sure becose nitroglycerin isn't stuff to play with . thanks

inkognito - 23-10-2003 at 03:12

im interested in EGD, can you give me some link where i can find a procedure . good that i checked sciencemadness before just before i wanted to make NG. how is EG extracted from antifreeze ? did you make it ? i found some info on mr.cool's site , but there was still no procedure .

Iv4 - 24-10-2003 at 23:25

NG is less sensitive than AP.I probably made less than 100 mls of NG in total but have enough experiance with AP to say that your fears CycloKnight are unjustified.

Propylene glycol dintrate is similer to EGD and non toxic?That would be prety interesting.

I know this might sound gay and all but how does the NG reaction work?

Nevermore - 25-10-2003 at 02:46

Quote:
Originally posted by CycloKnight
Ethylene Glycol dinitrate is used as a NG substitute in industry. Why all the fascination with NG? EGD is almost as powerful as nitroglycerin and much more stable. The process for making it is similar to NG, but ethylene glycol (extracted from EG antifreeze) is required rather than glycerin.
But anyway, EGD is a good substitiute, better safe than dead.



Well EG is definitely widely used, but i don't see what could be the advantages compared to glycerine but its lower freezing point.
I see only disavantages: EGD is more volative and more toxic than glycerine.
The power is comparable being NG slightly more powerful, and the sensitivity is comparable too, being EGD very little less sensitive..
Is not the holy grail..

trinitrotoluene - 25-10-2003 at 12:27

EGD gives worser headaches, and I thought it was weaker than NG. I think the synthesis of NG is more easy than EGD, ethylene glycol from antifreeze is not aways pure and had to be purified by distillation verses glycerol you can buy 99.9% medical grade.

palpy - 25-10-2003 at 12:55

it makes sense, that EGDN is more powerful than NG - it's practically the same thing, only that EGDN has zero OB :)
BTW in my country antifreezes are sold that can be used straight as they are - they are the cheapest ones and should contain just EG and a little (<0,5%) NaNO2 IIRC

vulture - 25-10-2003 at 15:50

Please use paragraph breaks!

People don't like reading long rants, especially when they're so cluttered like yours.

vulture - 26-10-2003 at 09:52

I'm not saying ranting isn't allowed.

It's just that such a big chunk of unformatted text is a pain in the ass to read and will deterr most people from reading it.

Nevermore - 26-10-2003 at 10:22

i am absolutely against that post, first of all, if someone is experimenting with explosives then doesn't need that kinda advice, should already know how dangerous they are. second, people won't listen about what you said, most won't even bother to read a so long post, since there isn't much interesting to read.
Why people keep making NG instead of something else is its ease of manufacture and the extremely long experience behind that reaction. NG is well knows at least from 100 years, good thing RDX, but when you can't get the extremely high conc acids? or when you can't get hexamine?
I think we don't need another hero to save us.
Better ppl to play with NG than with AP.
that's my point of view, if you have experience to share, or some ideas about more safe explosives, then welcome, noone of us is manufacturing anything over here, we are discussing energetic materials, or should we open a ethic forum? :o

[Edited on 26/10/2003 by Nevermore]

civility, please

Polverone - 26-10-2003 at 13:43

CycloKnight, you are correct that there's little novel or heavily chemistry-based in this discussion of nitroglycerin. According to my rule of thumb the topic should've been closed at the beginning. However, the discussion is now entering the theoretical realm, so I'm reluctant to close it.

A quick web search reveals that nitroglycerin is still used to make dynamite. Dyno Nobel at least still makes nitroglycerin dynamite. All the genuine explosives literature I've read (as opposed to fringe stuff) indicates that nitroglycerin can be safely manufactured, stored, and used, both on a lab scale and an industrial scale, if it is treated respectfully.

Nevermore, you say "noone of us is manufacturing anything over here" yet the very first post starting this thread is from you, saying that you are going to make nitroglycerin for the first time! I don't encourage discussion of the practical side of making/using energetic materials, but let's not go into total deception mode and pretend that every experiment is done by acquaintances or in dreams, a la the Hive.

Everybody who's going to experiment with explosives should have a healthy respect for the materials they're working with, as well as good knowledge of their preparation and properties, but that doesn't mean that they will have that respect from the get-go. A fool who can follow instructions and a Ph.D. chemist are equally capable of making simple nitric esters.

While I think CycloKnight's advice was a bit frothy around the mouth and hyperbolic, everyone who works with such materials needs to keep in mind the potentially grave consequences of a single mishap or moment of carelessness.

Edit: I just considered - maybe Dyno Nobel describes dynamites as "nitroglycerin dynamite" even if they contain EGDN instead of actual nitroglycerin, so long as they have similar performance. CycloKnight, do you have some references about the non-use of NG in modern dynamites?

[Edited on 10-26-2003 by Polverone]

Nevermore - 27-10-2003 at 00:55

@Polverone:
I just had an sudden idea of self protect so i thought better to write down i never manufactured anything. I absolutely agree that nitro ester can be performed by anyone that is able to get reagents and follow the instruction of any book or online website he can find. And i agree that everyone should respect what is working with, since before working with explosives, we are working with highly concentrated acids, toxic fumes and so on..For what i know those kinda advices bring the ppl in thinking that IT IS COOL to make, since explosives are cool for definition (i can't negate indeed, still cool for my age), and most of the people start manufacturing when they don't even have idea of what a reaction is..beside that, i didn't want to flush in the toilet the NG after 100 years of duty, and for what i know, is still highly appreciated.

@cycloknight:
from your word i feel like you had an accident and wish to try to save someone from having the same, or maybe you know someone that had an accident, i think i would like to know what happened, it could be useful to avoid the same situation, if not, then sorry maybe i was wrong.
Is good you wanna keep people away from nitro, but be realistic, they won't stay away, i would rather give out tons of hints to ensure safety, since i already know they will try to make, beside that, considering which other are so easy to manufacture, as i said before, i prefer if people try to make Ng than Ap or HMTD, i can't compare them, but i saw main charges made with Ap and ammonium nitrate, and i wondered how come there are still people that do those things whatever so many advices have been given out, maybe because accidents always happens to others (or for ease of manufacturing)..well, id prefer them to make NG, or EGDN than Ap, if you are sure that the egdn is more safe than ng and should be encouraged, then its good, but in my idea the difference is small, and being realistic is not worth the more toxic product. I can say that the folks that don't know what they are doing will try anyway, for sure better they try with something easy that doesn't involve too toxic fumes and so on, for sure better they try with something more safe, but the reality is that they try with ap, the worst ever chance. It is advisable to gelatinize NG, but before doing it is needed to make Ng no? even if i still prefer to absorb it somewhere than gelatinize, it makes me feel safer, than mixing with Nc and warming it..
I case you find a patent about better gelatinization, i would like to know, i don't feel too happy of having liquid pure NG, neither of knowing is rather sensitive..

Nevermore - 27-10-2003 at 13:58

I am sorry for the problems you are experiencing, i am graduating in engineering too, nuclear, i am using in handling dangerous things, but not explosives. I never ever work with more than .5 grams of primaries, or 10 grams of main charges, no matter what, if i have to try something bigger i make many smaller batches and then strip together ON SITU.
Blackpowder burned heavily some friend that were trying to make it, they were grinding it with a manual coffee grinder, when got on fire and splattered on their face. not good either, if not caring about the simply safe measurements..accidents are more likely to happen with primaries, since for their nature they are more sensitive..Ng is not that monster, i think your dad friend could be killed if using rdx or whatever powerful explosive..
Anyway kinepack is great! if only i could get nitromethane..
for removing spent acids, first of all is good to wash a few times, 2 should be enough, then wash with a bicarbonate solution, caring that no bicarbonate is left undissolved, keep wash till bubbling, then test with litmus, if neutral or little basic, wash with water, if still acidic, keep washing with bicarbonate. Some time i thought it was better to use a very diluite ammonia solution, but i think it will reach the same point, neutrality, is what we want.

[Edited on 27/10/2003 by Nevermore]

blip - 27-10-2003 at 16:42

It's interesting that you handled hazardous materials with your left hand, I would've thought it would create more spills. I don't make explosives (seriously), but if I did I would use many safety precautions. For example, I normally wear three layers of different types of gloves just in case. You are not going unheard, I often listen to those experienced because I know they probably wouldn't lie. My chem teacher was pretty paranoid, but she <i>did</i> have some nasty stuff lying around and many mischevious students had probably gone overlooked. I actually knew one of them and his friend could have easily died from drinking a lead compound (the idiot said it looked like egg yolk, so it must not be that bad :o).
Quote:

...though I’m left with permanent tinnitus (non-stop, persistent ringing of the ears) and it drives me nuts to this day, and there’s no cure.


I have it too, maybe I was born with it, I honestly don't know. It gets worse when I listen to loud music, but I learned early how to control the volume. I am also partially deaf in my left ear due to a non-pyro related accident (poorly made ear product, let's say). When I'm older, however, I'll likely have some of the best hearing in that ear around after the damage clears up (blockage).

Iv4 - 2-11-2003 at 05:34

I understand your point Cyclo and its a noble thing to do :D but seriosly of al the thousands of people who work with AP only a few have had accidents and like you said they deserved it.Stupid things like keeping large amounts of AP in one place and such is just asking for trouble.

I'm not into 400 gram batches and all but usually work in the 30 gram range(drying time...).Its always used in amounts well under 2 grams like in salutes and such.

On a sidenote when mixed with ammonium nitrate AP tends to behave very diferently above 1:1 APAN by weight it needs a shock in order to detonate.

Anyways I was wondering if glycerin can form an explosive peroxide.

Polverone - 2-11-2003 at 14:24

Quote:
of al the thousands of people who work with AP only a few have had accidents and like you said they deserved it

I think you underestimate the number of people who've had accidents with acetone peroxides. When I was a freshman in high school, before information on peroxides was widely available through the internet, I was part of a circle of people who learned to make acetone peroxide, from a hand-typed "recipe" handed down by someone older. Of the 6 people I knew who personally made it, 3 had accidents at one point or another. Mine was the least serious; I just suffered some broken lab equipment. One had his hand bruised through from side to side and the skin lightly torn. The last had his hand mangled so badly that what remained had to be amputated at the wrist. I think I behaved the most cautiously of anyone I knew when using it, but with hindsight I can see situations where I could've become Stumpy. I shudder at the thought.

If you read the threads about accidents that sometimes come up on the E&W Forum or other electronic discussion forums, you'll see that a lot of people suffer minor (non-permanently-disabling) accidents that they never mention online except in those accident threads. People who make a pound of acetone peroxide at a time might be rendered incapable of reporting back if they have an accident.

Minor medical emergencies - even where "minor" is the loss of an eye or some fingers - rarely make the news. It's even rarer for the injury/death to be so spectacular that it's widely reported. If you just go by what you can glean from electronic news sources, large-circulation newspapers, or TV news, you'll probably think amateur pyro injuries are pretty rare. I think they're actually frighteningly common, relative to the population of active amateur pyros.

People may "deserve" their injuries in the sense that you can't fool nature, and hazardous behavior leads to accidents. They don't necessarily "deserve" them in the sense of being blatantly reckless or lacking in moral fiber. The individual who lost his hand is one of the brightest people I've ever known. It only took one poor choice to lead to months of physical therapy and nightmares, and being one-handed for the rest of his life. With hindsight, what he did was reckless and he "deserved" what happened. Right now maybe your behavior doesn't seem reckless at all. You "only" make 30 grams of acetone peroxide at a time, not the hundreds of grams that reckless people make. That 30 grams would be quite enough to cost you a hand, if it detonated at an inopportune moment. The two grams that go in a "salute" could deprive you of a finger or two.

Nevermore - 2-11-2003 at 23:58

i agree about RDX but not about EGDN.
If you make NG or EGDN you will get very similar products, both in power than in sensitivity, being EGDN very safe is just another hoax.

Nevermore - 8-11-2003 at 07:59

Those things will help little if a big charge explodes next to you, because you were performing a synth in the wrong way..
The biggest concern with AP is its sensitivity, with NG is working with concentrated acids and the risk of a runaway..
well, every thing has drawbacks. RDX and PETN are tricky to make if you don't have the correct equipment (include in that the correct % of acids and starting materials.).
I suppose is better to start with something easy in dropwise quantity, then more to bigger scale, then go on something tricky only one you have gained enough experience.

Mumbles - 8-11-2003 at 11:02

I'm going to recomend the Urea Nitrate proceedure proposed by Mr. Anonymous a while ago. Its in the thread "From a Secret Admirer". Its about 3 or 4 post down, just search the page for Urea Nitrate. Cut the ratios, by about 10 though, you'll get ~80-90g of product.

It's fairly simple, the chemicals involved arn't too dangerous, or exotic. It can handle deviations in reactant amount. Its not very sensitive either.

Blackpowder would not be a bad option either. It has all the above feactures, but it is sensitive to flame. This means you could test the product without the danger of dealing with more dangerous initiators. Personally black powder is still one of my favorite things. It's just so useful.

Before you do anything, do yourself a favor and read as much as you can. Knowing what, or why it happens, can be just as satisfying and rewarding as a good product. It also helps to identify, and fix, possible problems that may occur.

Microtek - 9-11-2003 at 04:11

Having energetic materials as a hobby is indeed less forgiving than most other passtimes, but your ( cycloknight ) argument about the inevitability of accident doesn't hold. First of all, there is probability of accident in every undertaking imaginable, but many people go through their lives without ever crashing their cars or being injured from climbing trees. What is important is recognizing the big risks, which in our hobby means work with primaries or unstable compounds. These risks can be minimized simply by choosing the most stable primaries around and using as small amounts as possible.
I have had a few accidents in my younger days when I still used AP, but as I prefer the challenges of producing small devices and therefore only work in sub-gram quantities, I have no scars to show for it.

And this brings me to my point; there is much more safety to be had in working with moderately sensitive compounds in small amounts than in using insensitive explosives. Things such as ANFO or urea nitrate require so large quantities of primary that an accident with the detonator will be capable of removing fingers. Also, because the detonator needs to be so large, the main charge "needs" to be large and will accordingly surely kill you if it goes off in your vicinity. Finally, the disadvantage of LEs such as BP is that they require confinement which will often produce shrapnel with a much greater lethality radius.

Sorry for the delay

Iv4 - 17-11-2003 at 01:12

I guess I did go overboard and for that I must apologise :)

I still think that AP accidents are opurely the users fault but after a recent incident hapening to a friend of mine(budget pyro,bryan)I guess its only arrogant of me thinking it could never hapen to me.

Even with bridgewrire detonaters you have the danger of massive shocks but hey you coud use paper or plastic casings for your BP :)

Nevermore - 18-11-2003 at 04:33

Quote:
Originally posted by CycloKnight

I absolutely never said that EGDN was completely safe, no explosive is. But it is safer than NG, and the larger the quantities being made, the larger the difference. But if someone is only making a few cc, then the difference is quite small, but if someone is intent on making a litre of it, that?s another matter.


Hello
i wish to have some data about EGDN since the things in my hands says it is very little less sensitive than NG..also in case you have the physical properties of both, IE: the boiling point, the vapour pressure, sensitivity to hit and friction, decomposition temp, decomposition rate at 20°C, freezing point and so on..
They will be really useful for me.
Thanks

Iv4 - 18-11-2003 at 23:58

I meant ,CycloKnight, that I still think AP wont go of without provocation,but I've realized that even the best of us will eventually do somehing to provoke it.

Here's all I could come up with concerning EGDN.It's not much but has a few tests(hint:just skim through it).

vulture - 19-11-2003 at 03:59

I'd like to point out that EGDN is much more toxic and volatile than NG, thus posing another extra hazard.

Microtek - 19-11-2003 at 11:35

Actually I was not contradicting myself, but I think a crucial point went missing, so just to get that straight:
- Regarding the inevitability issue, while having a non-zero probability of accident does mean that it will happen given enough time, it does not mean that it will happen to a certain individual because no individual exists forever.
This is why I claim that your argument doesn't hold.

The point that went missing in my first post was that you can't live a risk-free life - and if you try to do so you might very well end up as a very old man who has done and seen very little.
Of course, it is quite allright to decide for yourself, that explosives is not one of the things you want to have "done" in your life.

All this aside, I think we probably agree on the practical side of things regarding risk management, etc.

Nevermore - 19-11-2003 at 14:10

more, the probability of a small event is far larger than the one of a major, beside that we must consider that we are not sleeping with the chemicals so the probability must be calculated only for the time we are directly working with them.
exceptional safety procedures can ensure a safe hobby, exceptional dumb people not observing them are candidate for Darwin award.

Iv4 - 28-11-2003 at 22:37

PGDN thread.Not so great.

Heh 21!?Thats it?I make like 30-40 on BS.

chemoleo - 29-11-2003 at 08:21

Iv4, your link makes both Mozilla and IE crash.... strange sense of humour you got :o:o:o

Mumbles did you count to find your position on the all time poster list? Lol happy counting :D
(unless there is some hidden function I am not aware of :o)

[Edited on 29-11-2003 by chemoleo]

Evaporation

tom haggen - 29-11-2003 at 15:54

is it possible that when your done washing your NG with sodium bicarbonate that you can put your NG out in a small dish and simply let the excess water evaporate out of it leaving you with pure NG?

-Tom

Iv4 - 3-12-2003 at 09:26

I guess sos but I for one wouldnt try to heat up NG.

The links work fine for me on IE.Try copy/pasting them?

IgnorantlyIntelligent - 12-1-2004 at 16:36

Sorry if this is a stupid question but how could Ng detonate while making it? Ive had one runnaway while making it and evrything caught on fire. I calmy pourred cold water over everything and all was fine. Had I not extinguished the flames so fast, could it have detonated somehow?

chemoleo - 12-1-2004 at 17:10

In fact, today I read somewhere that people tried a deliberate runaway reaction (in a professional lab). yet they they did not achieve a detonation. Presumbably this is because pure NG amounts are not large enough, and not coagulated enough to form the quantities necessary for true detonation. Up to a certain point, you only have an emulsion of NG and reaction mix. Only if you let it setlle, the NG forms an immiscible layer at the bottom, clearly thats not going to happen at the beginning of a nitration.
Anyway, the critical diameter for NG is around 5 mm, so NG blobs would have to be pretty large and noticeable before you'd get detonation.

Edit: Oops, to answer your question, I doubt therefore that your runaway would have resulted in a true detonation. Rather, things would spew out more and more (still its nasty hot acid so watch it) until none was left.

[Edited on 13-1-2004 by chemoleo]

IgnorantlyIntelligent - 12-1-2004 at 19:16

I have always thought that NG was hard to make and dangerous but after making it, testing it, storing it for five months, and testing it again I have relized that even a novice chemist can make a good pure product that is safe unless mistreated.
I dreamt of using up the rest of the Ng(about 20ml) on a tree where I go shooting. In the dream I was out of dets so I just used a 10/22 to shoot it. First shot it detonated destroying the small brach I had it taped to and doing damage to the surrounding branches.:)

[Edited on 13-1-2004 by IgnorantlyIntelligent]

IgnorantlyIntelligent - 25-1-2004 at 16:23

Is it possible, when making NG, for the NG that has formed in the acid/nitrate/glycerin solution to disolve in the acid? I have been told that after adding the glycerin, and letting it sit for about 20 min if you dont add it to double its volume of water the NG will start to disolve in the acid. I dont believe this though because I've put NG in a small amount of sulfuric acid and it did not disolve it. I want to start leaving my Ng in the solution longer because several batches of NG that I did didnt work. No glycerin was nitrated.
Another question I have is can you use too much Xnitrate? I use Ammonium nitrate. I normaly use about 40g ammonium nitrate, 50ml sulfuric acid(95%), and 10ml glycerin. Sound good??
I use Ng for sensitizing AN/DBSP in my claymores and it is getting too expensive when half my NG batches dont work! Thanks for any help.

guaguanco - 26-1-2004 at 09:30

Quote:
Originally posted by IgnorantlyIntelligent
First shot it detonated destroying the small brach I had it taped to and doing damage to the surrounding branches.:)

In the dream, did you feel bad afterwards for damaiging the tree for no good reason? (1/2 smiley)

IgnorantlyIntelligent - 26-1-2004 at 16:21

Well niether of those posts answered my question.
No, sorry but I didn't feel bad for damaging the tree. There alota trees out here.
I didnt say NG was absolutely safe. I simply said that even a novice chemist(me) can make NG without a problem. Didnt say it was fool-proof. Half my batches dont work but I think Ive solved my own problem. Speaking of which I have a batch outside nitrating as I speak so bye. -in a dream I mean...

I have gotten many different types of NG even though I follow the same precedure every time. I think I'm getting trinitroglycerin because it matches all the characteristics of it. My last batch was clear, detonates with a hammer blow, and is VERY powerful(twice what AP seems to be). Ive gotten NG that was dark, tan, white(water in it), clear, Each with different power and sensitivity.
I think these are all triNG but Im not sure.
Would monoNG even precipitate out of the liquid once added to water?
Even when following the same synthesis precedure, I will get different yeilds, and different product. It seems very unpredictable.

[Edited on 27-1-2004 by IgnorantlyIntelligent]

Batch failer

IgnorantlyIntelligent - 2-2-2004 at 09:19

I recently made another batch of NG(well tried too) and it went very wierd and wrong. I put 160g AN intoa beaker with 200ml of sulfuric acid 95%.
About 1 hour later I added the glycerin. I slowly poured 50ml inot the solution wihtout much temperature raise(stayed under 10c) I maintaned a temp between 15c and 30c for aboput 10 min then let it sit at room temp for 20 more min. The mixture was VERY thick and turned darker and darker in color every min. I then poured it into a beaker of twice its amount of water and NO2 appeared while pouring it(very litle though) The yeild was about 5ml NG. I normaly do this exact same precedure but I do not allow the acid/nitraet solution to become so cold and I add the glycerin slower. My normal yeild is about 50ml NG
Any ideas what the hell happend?

[Edited on 2-2-2004 by IgnorantlyIntelligent]

Nevermore - 4-2-2004 at 01:17

probable oxidation of glycerol by H2SO4=
too large excess H2SO4, too high temperature, your AN was not really what you thoght it was..
Alot of other reasons, but those are the most probable that bounce in my mind.

IgnorantlyIntelligent - 5-2-2004 at 09:52

I have followed the same precedure before with great results. Why would it change? IS NG that unpredictable?
I dreamt of using the rest of my NG and DBSP to make some blasting gelatin sticks for this weekend. I guess more trees will suffer.

[Edited on 5-2-2004 by IgnorantlyIntelligent]

Polverone - 5-2-2004 at 12:10

Quote:
I have followed the same precedure before with great results. Why would it change?

Your materials changed, your methods changed, or your reaction conditions changed (or more than one of the above). That's it. The nice thing about science is that if you perform an experiment exactly the same way twice, you will get the same result twice. Of course that doesn't mean it's always easy to figure out what has changed when an experiment doesn't go as you expect.

Purifying Nitroglycerin?

hightechstuff - 12-2-2008 at 15:27

Hi Everyone,
I recently synthesized 10 ml of NG from Rooto drain cleaner, ammonium nitrate and glycerin. Now, I know this is a pretty $#!tty way to synthesize NG but it did work. I am a little concerned about the purity of the final product though. The AN was fertilizer grade and had some impurities in it and the 93% H2SO4 is obviously waste acid from some industrial manufacturing bottled up and sold as drain cleaner. The NG has the color of olive oil with only a slight haze. A major concern for me is that these impurities will make the NG more unstable and possibly react negatively unprovoked. Is their a way to purify my NG? Do I have a ticking time bomb on my hands? Any comments and suggestions would be greatly appreciated.
Thanks!
hightechstuff

ScienceGeek - 12-2-2008 at 16:32

The hazyness is not a problem, as this is just a hydrated form of the nitroglycerin. This can be removed by desiccation.
The color, on the other hand, indicates (most likely) unwanted metal ions, probably from the H2SO4. This is a big problem when it comes to stability.

If it was me, I wouldn't dare desiccation, as it could detonate all on its own.

hightechstuff - 12-2-2008 at 16:50

Hi ScienceGeek,
Thanks for the info. I figured the haze was water. I dessicated the NG in a petri dish with a sodium chloride solution for 12 hours which obviously didn't remove all the water. It seems I have a potential problem on my hands then. Should I deflag the preparation immediately or do you think it would be safe to store for a week or so? I believe the H2SO4 is the culprit for my impurity problem as well. Is their a way to purify my drain cleaner acid? Is their a way to purify my ammonium nitrate? Purchasing technical grade sulfuric and nitric acids is expensive I'm trying hard to avoid it but it may be the only way to do it right.

Fulmen - 14-2-2008 at 04:08

Actually I think you're in good company, Sobreros first batch of NG was also described as olive-colored ;)

Any metal salts should be easy to wash out with water, other than that I don't know. Davis does not mention anything about instability or potential causes, but I won't guess if this is an omission or if there really isn't anything that can cause instability.

S.C. Wack - 14-2-2008 at 05:36

Drain cleaner? Technical grade materials too much?
For nitroglycerin?

Call me a crazy old crank, but...well you can probably guess where I'm at with this.

Just for hahas, drop an oxidizer in your drain cleaner (that many here think is pure as snow except for the color) and see what happens on heating for a while. I suggest Cr+6, because of the nice green color of Cr+3, compared to the less dramatic change with permanganate. The most favored brand here (Rooto) will reduce a lot of chromate, and thus isn't even fit for cleaning glassware. I sure as fuck wouldn't use it to make unstable explosives, but I'm just an anal overly-cautious wet blanket.

a_bab - 15-2-2008 at 06:30

10 ml of NG is roughly 15 grams.

5 grams are able to vaporise your palm to the forearm bones and possibly blind you.

I'd get rid of it ASAP; even burning it may cause it to explode.

If ordering reagent grade acids is avoidable, just ask yourself: "what do I need my NG for?"

It's something you make, make sure you don't miss the additional headache, ddt it and you go for the next on the list :D

pdb - 15-2-2008 at 13:23

Hi a_bab, do you think of someone in particular :D ?

Yes, I'm the one who lost one hand and one eye with approx 10ml of NG when a runaway took place at the end of the synthesis, although the temperature was so far under control (<15°C).

Zinc - 15-2-2008 at 14:57

Did you use HNO3/H2SO4 or XNO3/H2SO4? And did it first start to give off NO2 and heat up or did it just explode for no apparent reason?

The_Davster - 15-2-2008 at 17:54

So sorry to hear of your accident, pdb. Like Zinc, I would be interested in hearing more about what caused your accident.

IIRC you are more active on roguesci than here, is there a thread there where you posted details that could be linked to?

pdb - 16-2-2008 at 02:57

The_Davster: No, I didn't give any details. My memories of this event are focused on the "after" story rather than the "before" one, and thus are bad memories. However, I've been reading a lot since (and before) about NG and in particular reports of manufactoring accidents over the world, but didn't reached any satisfactory conclusion. Some accidents remain uncleared, mine is such...

Fulmen - 16-2-2008 at 04:22

I took a peak in Urbanski, and I really can't find any reason for this batch to be dangerous. Not saying it isn't, I just can't see why.

The commercial product is usually yellowish (of straw yellow colour) or pale brown depending on the purity of the original raw materials and on the conditions of manufacture.

Acidity affects stability, but no other sources for instability is mentioned. I agree that reagents of unknown purity are ill-suited for explosive manufacture, but as far as I can tell there's not much cause for concern:

Acids for nitrating glycerine must be as pure as possible. Nitric acid (sp. gr. 1.50) should not contain more than 1% N204. Sulphuric acid (sp. gr 1.84) and oleum (20-25%) should be virtually free from lead sulphate which is liable to be present in old installations constructed of lead, and also from sulphates of iron, as these substances hinder the separation of nitroglycerine and acid.

The sulphates could make it harder to remove all traces of acid, but a litmus test will reveal that.

a_bab - 16-2-2008 at 23:00

Hi pdb, long time no see.

Well, that was a general statement, although I did think of you. It could happen to anyone.

Check your PM please.

hightechstuff - 8-3-2008 at 21:36

Hi Everyone,
Thanks for your input. Please excuse the delay. My post was put in detritus and I figured that was the end of my posting here. Since then it was merged with another NG post.

Fulmen,
I emulsified the NG with water using a magnetic stirrer and was able to remove a small layer of unknown white/brown sludge after the separation. However. the NG still remained yellow in color. Obviously whatever the contaminant, it is not soluble in water.

S.C. Wack,
I completely agree. Use $#it = get $#it. ;) I figured I'd nitrate what I believed to be a small amount of glycerin and see what comes out. Obviously not a pure form of NG however it seems fairly stable..... for NG.... You know.

I don't plan on making NG ever again. I just wanted to see if it could be made with AN and drain cleaner which I confirmed. I did however follow your suggestion on the Rooto H2SO4 and it did seem to clear up the acid to a point. Here is what I did...

I poured 200ml of "Rooto drain cleaner" into a 1000ml beaker containing 50ml of 30% H2O2. After about an hour of reacting, the acid appeared as a clear oily substance versus the yellowish cloudy substance.

I then boiled this mixture down to 200ml to obtain the original H2SO4 concentration. The preparation is now clear accept for a few suspended, small, grayish globules of ????


This acid "seems" to be much cleaner than the original drain cleaner form however I would like to also remove the grey material which I believe to be some kind of metal. What would be the best way to filter this acid?

Subsequently I have also devised a way to clean up the ammonium nitrate. Here is my procedure.

In a flask I created a high concentration of AN solution using water. I added fertilizer grade AN prills to the water until the remaining prills would not dissolve. I then took the murky liquid and filtered it three times at room temperature creating a clear solution.

The AN prills I have don't appear to have a calcium coating however I may be wrong. The sludge removed from filtering is a brownish white sludge.

I then took the clear solution and boiled it under vacuum on a hot plate until the solution was devoid of water. The concentration was poured into a dish, solidified and ground into powder. The final product now appears to be fairly pure ammonium nitrate.

pdb,
Damn! That sucks. Sorry to hear about your experience with NG. You seem to be taking it well though and moving on with your life. Good for you! :) I truly wish you the best.

Thanks Again!
hightechstuff

Zinc - 23-3-2008 at 13:30

Today I tried to make NG (again). I mixed 75 ml of H2SO4 with 50 g NH4NO3. After it cooled down to around 15 C I started to slowly add 12.5 ml of glycerin After I added all the glycerin I waited around 15 min and then diluted the mixture with water. I could see that there is some other liquid that doesn't mix with water in it but it never collected on top or at the bottom. I diluted the mixture more and separated one part of it and neutralized. Still no NG. This is the third time it happened!! Does anyone know why?

There is one possibility why it happened. Somewhere I have read that iron or lead sulfate dissolved in sulfuric acid might cause difficulties in the separation of NG from the spent acid. I used boiled down acid from a old car battery.

Boomer - 26-3-2008 at 06:26

" ... from a old car battery."

That's it, you want a new (or at least still good) battery, fully charged. Discharged = acid is mostly present as sulfate.

Bert - 26-3-2008 at 11:42

Here in the US, you can buy a 5 gallon carton of NEW 30% battery electrolyte at many auto/truck parts stores, probably for less than $20.00. An old electric deep fryer from a garage sale makes a useable sand bath for dehydrating acid with a large Pyrex beaker or coffee pot set in it on a layer of sand. A 1,000 watt unit set at 450 F. has been seen to concentrate a 4.5 liter batch of 30% electrolyte to a specific gravity of 1.8 in less than 24 hours.

Zinc - 26-3-2008 at 11:47

Yes I have heard that it is also available in my country. I searched but didn't find it yet. I will continue looking.

Bert - 26-3-2008 at 19:42

Look where the parts and batteries for large trucks are sold. Diesel trucks have LOTS of batteries, and they are generally not the sealed units used in passenger cars. Hence the need for their mechanics to be able to maintain electrolyte levels-

StevenRS - 19-4-2008 at 16:11

I have a problem. I ran out of nitric acid, so I will improvise. If I were to use KNO3 and Sulfuric to make Nitroglycerin, would the ratios be 5 ml glycerin, 30g KNO3, and 46 ml H2SO4? Someone tell me if I did my math right.

[Edited on 19-4-2008 by StevenRS]

Sickman - 20-4-2008 at 02:12

Quote:
Originally posted by StevenRS
I have a problem. I ran out of nitric acid, so I will improvise. If I were to use KNO3 and Sulfuric to make Nitroglycerin, would the ratios be 5 ml glycerin, 30g KNO3, and 46 ml H2SO4? Someone tell me if I did my math right.

[Edited on 19-4-2008 by StevenRS]


StevenRS,

You need to be very, very well informed and prepared, before making any attempt at making NG. Not only that, but you need to be willing to lose your body parts/body part functions and your life for that matter, depending on the amount you plan on making and the material(s) that make up your reaction vessel.

NG synthesis is very hazardous and makes me question wether or not the risks are actually worth it. Nitric esters like ETN or PETN are far more predictable (safety wise) in their synthesis, and in my opinion are a more profitable pursuit than NG. I'm not saying this to mean that NG isn't a very useful explosive to mankind, and that it's hazardous manufacture cannot be carried out, but think about the lives destroyed, disrupted, torn apart, and simply wasted, because of the accidental detonation of NG during it's manufacture and handling.

Don't think that accidents will never happen to you! That's how accidents happen most of the time!:o

The dangers of synthesis aside, you need to go back and reread my postings in the thread entitled "Nitration Calculations".

To double check your above math you will need to double check your reactants. Ask yourself is my KNO3 anhydrous? Have I taken any steps to insure and confirm this fact. Ask yourself is my sulfuric acid anhydrous? What about your glycerin. It very likely contains some water even if it is just a little.

The truth is the more you know about your reactants (what you are actually using), the more you will be able to accurately predict the products and yields for the reaction.

Water is one of the products of NG synthesis (wether or not your reactants are anhydrous or not) and if your reactants themselves contain water you need to figure this into your balanced equation as well, so that when you end up with a lower yield of NG than expected you will know why.

NG is a trinitrate, so you will need three NO3 groups per one glycerin molecule. In other words you will need three moles of anhydrous KNO3 per every one mole of anhydrous glycerin. During the manufacture of NG 3 moles of H2O is produced for every one mole NG. This will heavily dilute your acids if they are not in excess.

You will also need to be practical. To acheive a high yield you will need an excess of NO3 groups in the reaction zone to increase the likelyhood that each hydroxyl group on each glycerin molecule (there are three on each one) will be replaced with an NO3 group.

Besides having a balanced equation to work with, part of being practical is knowing how much heat is liberated during the reaction and how this can trigger a runaway reaction among other factors. Ask yourself questions like: will I need to use an ice bath to moderate the reaction or perhaps a dry ice/acetone bath to cool the reactants and products. Would some form of stirring be appropriate during the reaction? How long does the reaction take to go to completion and how does temperature and acid concentration effect this? What about addition rates? How will I plan ahead for a worse case scenario (accidental detonation)? What precations have I taken and what steps will I take if a runaway is detected or some other hazard?

If you have done the math correctly and honestly and truly know your reactants and products along with their properties and hazards. If you have been practical in designing your experiment to counteract the factors working against good yields for the end product (NG) and taken every measure to insure your own safety and well being and those of others as well. If you are willing to suffer the potential damage or loss of life or function during an unexpected event. If everything is in place, then I think it is very possible, you may end up with a very decent yield, and possibly a rewarding experiance, if the unknowns keep their distance and leave you without any ill effects. Otherwise, do yourself a favor and leave NG alone.

[Edited on 20-4-2008 by Sickman]

StevenRS - 20-4-2008 at 11:21

Thank you for the advice and warnings, I will be making a small (but still dangerous amount) of 10ml. I have a magnetic stirrer, and a large amount of water to dump the reaction into if it goes bad. I have prepared along time for this, I just wanted to make sure I had my ratios right. I believe I do. All the ratios I posted are for anhydrous chemicals, I have already figured the difference for my chemicals, and still use a little extra. I also have decided to use a greater excess of H<sub>2</sub>SO<sub4</sub> to make the mix more fluid and easier to stir.

For cooling, I am using a homemade forced water/antifreeze cooling system that has several glass spirals in the reaction mix itself, in addition to an ice bath. I have to be careful I don't freeze everything with this!

I have already set everything up, outside, and now I am putting my face shield and gas mask on... Here goes...

Bert - 20-4-2008 at 11:34

Quote:
Originally posted by StevenRS
Thank you for the advice and warnings, I will be making a small (but still dangerous amount) of 10ml.


Sigh. Damn straight "still dangerous ammount".

Boomer's freezer NG method with sulfuric acid and nitrate

Sickman - 20-4-2008 at 12:56

StevenRS,

Don't rely on your magnetic stirrer to get the job done! A KNO3/H2SO4 mixture can get very thick, espeacially below 0 degrees Celsius. Suppose your stir bar stalls out and then you have to try and stir manually around these glass cooling coils. You could have problems.

Make sure you have a backup plan for every possible thing that could go wrong.

A high velocity peice of glass or metal WILL go right through your face shield if it has enough mass (a half gram fragment is all it takes). A one gram fragmnent with a high velocity has proven itself over and over again on the battle field to penetrate body armor and cause lethal wounds. All wounds from such high velocity fragments are well known for causing wounds that bleed profusely and it can be extremely difficult to stop the bleeding. Bleeding to death is a real factor here. Along with blindness and getting your eardrums blown out.

It would be best to design a very robust shield of plexy glass around the entire reaction vessel no less than 3/4 of an inch thick and large enough to shield your entire body and you still might lose a hand reaching over the shield during the synthesis. Ear plugs with a high decibel reduction covered by high decibel ear muffs is smart. Also your eyes are very precious and are worth every effort to protect against high velocity fragments.

10 ml of NG can change your life if you let it! Just ask pdb, a member here who had just such an experiance.

He says and I qoute:
Quote:

Yes, I'm the one who lost one hand and one eye with approx 10ml of NG when a runaway took place at the end of the synthesis, although the temperature was so far under control (<15°C).


and
Quote:

The_Davster: No, I didn't give any details. My memories of this event are focused on the "after" story rather than the "before" one, and thus are bad memories. However, I've been reading a lot since (and before) about NG and in particular reports of manufactoring accidents over the world, but didn't reached any satisfactory conclusion. Some accidents remain uncleared, mine is such...


Like I said "is it really worth it?"

Pulverulescent - 21-4-2008 at 08:34

I used a thermometer to mix the reactants when I made nitro and I remember the slight worry that too-vigorous mixing could cause detonation by shock or friction.

In a runaway, with already formed nitro at high temperature, the slightest jar (a thermometer dropping into the mix?) might be enough to set it off.

No one wants to repeat pdb's experience (however heroically he's dealing with it!) so all eventualities should be considered.

If I ever make a liquid explosive again, it'll be nitroglycol!
Its reduced sensitivity certainly commends it!

P

Pulverulescent - 21-4-2008 at 09:00

Oh, and drain-cleaner + nitrate salts will have no part in it.
The H2S04 will, hopefully, be the stuff that comes in an amber safe-break bottle.

Or I could try distilling what I've got!

P

Pulverulescent - 21-4-2008 at 12:10

Pdb, I should just say I'm not insinuating any bad practise on your part.

Some accidents are inexplicable!

P

StevenRS - 21-4-2008 at 17:32

I added an excess of sulfuric acid to the mix to reduce viscosity, and yes, the glass coils would make manual stirring impossible. If the stir-bar stopped, I was prepared to dump it.

But I didn't have to, everything went fine, I now have a decent 5ml of nitroglycerin, completely neutralized, and stored in a plastic bottle.
Definitively worth the effort and worry, but only once, just to say I did it.
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