Nitroglycerin with pics

[ALENGOSVIG1]

Today i made some NG with some freshely distilled nitric acid. I dont know the exact conc. of the nitric but probally 90-95%. Im not sure, but i didnt re-distill it becuase im getting low on H2SO4.

I used 100 ml of 90-95% nitric acid, 200 ml 98% of sulphuric acid and 50 ml of glycerin.

You must copy and paste the pictures into your browser.

Picture of the precurors:
<a href="http://www.angelfire.com/linux/aleng/NG1.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NG1.jpg</a>

Picture of the acids mixed:
<a href="http://www.angelfire.com/linux/aleng/NG2.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NG2.jpg</a>

Picture of acids after glycerin addition:
<a href="http://www.angelfire.com/linux/aleng/NG3.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NG3.jpg</a>

Picture of the unwashed nitro:
<a href="http://www.angelfire.com/linux/aleng/NG4.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NG4.jpg</a>

Final yeild was about 100 ml which is should be around 159 grams.
When i get some more KNO3 (mabe tommorow) i'll do the KNO3/H2SO4 method.

[Madog555]

nice, thats a big ass load of nitro.

if i could only get some glycerin...

[ALENGOSVIG1]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> if i could only get some glycerin </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">I've never heard of glycerin being hard to obtain. What country do you live in? In most countries you should be able to buy it at a grocery store.

[NoltaiR]

I could get the materials easily but because my HNO3 is made from my H2SO4 in the old IM style, I don't think I would trust it in the manufacture of something like NG. But if you do the H2SO4/KNO3 method, I will probably try to reproduce it and post my results.

And yes that is a lot of NG, I assume you are going to make some sort of dynamite mixture with it (or maybe that is just something I would do).

Anyways, how did you wash your NG (I have just never heard of a method of washing a liquid).

<small>[ March 17, 2002, 07:19 PM: Message edited by: NoltaiR ]</small>

[Madog555]

i live in USA, i think i just need to look harder, i was in Wal-Mart in the beauty section and couldn't find it. im gona check CVS next.

[ALENGOSVIG1]

I'll either use it straight or make some ammonia dynamite.

To wash the NG, add it to some distiiled water in a RB flask, swirl it around for a min or two end let it sit for an hour, while swirling occasionally. Then extract the NG with a seperatory funnel or turkey baster and add it to more water, and repeat the process 2
or 3 times.

Agin, extract the NG layer and add it a sodium bicarb solution. Let it sit in the solution for 6 hours, swirling once in awhile. Repeate the sodium bicard wash 2 or 3 times, then do a final saturated salt solution wash. Let the NG sit in the salt solution for a day before extracting it. Finally, the NG sit in a shallow dish for a couple days to evapourate any water.

Be sure to wash the sep funnel or tunrkey baster (whichever you used) Between each extraction.

[DBSP]

I'm interested in AN sensitized with NG, would you mind testing some ammonia dynamite or similar? Anyway nice job. Have you got any info on the yield, weight, volume etc

[ALENGOSVIG1]

What do you mean by test? I've made ammonia dynamites before so if you have any questions i may be able to answer them.

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> Have you got any info on the yield, weight, volume etc </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">As i already said, around 100 ml which should be 159 grams. Ng has a density of roughly 1.59, so 1.59 x 100 = 159 grams of nitro.

<small>[ March 17, 2002, 10:34 PM: Message edited by: ALENGOSVIG1 ]</small>

[nbk2000]

(Mr. Burns)
Excellent, Mr. Alen.
(/Mr. Burns)

Good pictures Alen. In the third one, I can see the NG layer floating on top of the spent acid. I would have gotten a closeup of the boundry layer, but it's cool.

Did you do dropwise addition, or use the capillary wick? Magnetic or air stirring? Or just manual swirling?

You'll find the glycerine in the pharmacy, not cosmetics, section. It'll be with the clove oil, tincture of iodine, mercurchrome, and other such things. But it's expensive that way.

If you're planning on making a lot of NG (aren't we all? <img border="0" title="" alt="[Wink]" src="wink.gif" /> ), then go to an agricultural/feed supply store. They sell glycerine by the quart or gallon. It's in the horse liniments section. Around $40 per gallon. That may seem like a lot, but that'll make about 12 to 13 pounds of NG. That's a lot of nitro. :D

[NoltaiR]

And just to think of all the dynamite I could make... just a mix of sawdust and NG would be sufficient and I could sell it to my not-so-savvy friends for quite a hefty profit... <img border="0" title="" alt="[Wink]" src="wink.gif" />

[ALENGOSVIG1]

I did take a closeup, but it was kinda blurry so i deleted it. Im using a video camera from 1992 and a Asus TNT video card that just happens to have capture capabilies. Its not a real video capture card :(

I didnt have any string laying around, so i tediously added the glycerin drop by drop from a syringe. A buret would have made things alot easier, but i'm too cheap to buy one. Stirring was done by rotating the RB flask at a 45 degree angle as describes in uncle festers home workshop explosives.

Kinda off topic, but i just nitrated 10 grams of cotton and i have some pics to show. Not worth starting a new thread but i'll post em here for you all to see.

Picture of cotton/acid:
<a href="http://www.angelfire.com/linux/aleng/NC1.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NC1.jpg</a>

Picture of cotton/acid from overhead view:
<a href="http://www.angelfire.com/linux/aleng/NC2.jpg" target="_blank">http://www.angelfire.com/linux/aleng/NC2.jpg</a>

Copy and paste them into your browser.

<small>[ March 17, 2002, 11:31 PM: Message edited by: ALENGOSVIG1 ]</small>

[nbk2000]

I just had an idea based on flash chromatography.

Pack a glass or plastic tube with powdered KNO3. Mix the glycerine and acid together. Pour this mix into the column. The nitration reaction should only take place at the interphase of the nitrate and the glycol/acid mix.

As the G/A flows through the tubing, it's continuously exposed to fresh nitrate.

Once the reaction mix has started to flow out the bottom end, you flush it with solvent to purge out all the NG.

You may wish to enclose the nitration tube in a water jacket. But that may not be necessary if the rate of flow is slow enough to prevent sufficient heat build up.

Who knows, this may allow for unattended and safe nitration.

Looking forward to the KNO3/acid NG pics.

[VX]

Yeah that would be cool.

The pics are very good also. How long did it take you to add 50ml of glycerine?

P.S. what happend to the 'DDNP with pics' thread? :confused:

[DBSP]

Sorry bout that post I woke up in the middel of the night and got online for half an hour. I kinda fucked up :o .

Anyway I would like to now of the percentage NG needed to sensitize the AN and sensitivity of it.

Sorry again.

[mr.evil]

When i hit the links, the pics don't appear, only the icon of angelfire... what's my problem? :confused:

Thnx

<small>[ March 18, 2002, 01:54 PM: Message edited by: mr.evil ]</small>

[ALENGOSVIG1]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> When i hit the links, the pics don't appear, only the icon of angelfire... what's my problem? </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">As i said, you have to copy and paste the urls's into your browser. I dont see how you could have missed that the first time i wrote it.

<small>[ March 18, 2002, 02:10 PM: Message edited by: ALENGOSVIG1 ]</small>

[ALENGOSVIG1]

VX: it took me about 25-30 minutes to add all 50 ml of the glycerin.

Does any one knoe exactly how sensitive partially frozen nitro is? I mean, in books they say its extremely sensitive but they say the same thing for AP. I want to know because I stored my nitro outside (undercover ofcourse) and it got real cold and snowed last night. The nitro is partially frozen it looks like so im wondering how dangerous it is.

[mr.evil]

Hey,
yes, i have read that. But what exactly do you mean? (sorry!)

[Pu239 Stuchtiger]

Sorry to disappoint you nbk2000, but that idea would simply result in runaway nitration. There probably wouldn't be a large explosion, but as the H2SO4 / glycerine mix comes in contact with the alkaline nitrate salt, the temperatures would rise out of control causing instant runaway nitration. The method of droppering glycerin into mixed acid is the only way to go. If this explanation is not clear enough, I'm willing to clarify more. I just didn't want anyone to possibly harm themselves. :-)

[00Buckshot]

Nice pics! I can't wait to see the KN03 method.

I'm curious if the reaction ever produced any heat? I guess you don't need an ice bath? And did the mix puff out much nasty fumes?

Thanks

[Pu239 Stuchtiger]

I believe that partially frozen nitroglycerin is unstable because of the chunks of a solid present. I hear (I can barely believe it!) that frozen nitroglycerin cannot be detonated; that sticks of completely frozen dynamite have been recovered after a failed detonation having bits of the detonator implanted in the dynamite. I would assume that your partially frozen nitroglycerin is about as unstable as nitroglycerin with some rocks, pebbles, and sand tossed into it.

00Buckshot, of course it produces large amounts of heat... it obviously requires an ice bath and does produce poisonous fumes...

[NoltaiR]

Well he got to post before I did, dammit :p
Anyways, when it comes to using acids in the synthesis of just about any energetic material, an ice bath should be used unless otherwise stated.

And alen, why on earth did you store it in its pure form? What you should have done is already planned what you were going to do with it before you made it. I would advise just carrying it very carefully, if you don't shake it around then the crystals shouldn't produce enough friction to detonate, and at freezing, molecular movement is less than at room temperature so sensitivity SHOULD be less--don't hold me to that.

And yes, all your chem books will overexagerate when possible about an explosive being sensitive because they believe that by stating this, then you will put more care into handling it than if they said something like "just do not shake it around too much.. this has been known to lead to accidental detonation". I mean I have heard all the stories about AP being sensitive, and before I knew it I was playing with it and molding it into creative shapes before detonating it.. but then again it was always damp... which leads me to an idea.. possibly adding cool distilled water to your container of NG would melt it and should prevent the risk of detonation.

[ALENGOSVIG1]

The ice melted and its fine now. Oh and i dont have a probelem storing it in pure form. I dont find it that sensitive.

[nbk2000]

70/30 ratio of NG/Acetone. Said to be sensitive to #8 cap, but safe for rough handling.

For what it's worth, you're milage may vary.

Soundtrack for this post provided by RUSH "By-Tor and the Snowdog" (kick ass song!)

[00Buckshot]

Could someone tel me if NG will explode unconfined? I've read that it will just burn with a blue flame. If this is true then NG shouldn't be that explosive when making it, right?

Furthermore does the ice bath help reduce the toxic gasses produced in the reaction? And is NG produced in cold tempratures considered more stable than NG produced at room temprature, similar to dimer and trimer a type of peroxide?

Thank you

[Pu239 Stuchtiger]

The problem with having small amounts of a solid present is the formation of points of extreme pressure, which can easily cause detonation. Firstly, liquids cannot be compressed much at all; they are very close to being fully compressed (assuming realistic terrestial conditions, noone tell me about how liquids can be compressed in a black hole or the like <img border="0" title="" alt="[Wink]" src="wink.gif" /> ). This means that any compression of an explosive liquid between two solid surfaces will result in one of two responses: (1) the liquid will be displaced (2) the liquid will decompose (explode) any slight increase in pressure will greatly increase the frequency of collisions between molecules, eventually causing decomposition. Dynamites are not dangerous because the liquid can pass through the solid; it is absorbed by the solid. Therefore an escape route through the solid is provided, preventing decomposition. Nitroglycerin cannot pass through solid nitroglycerin; this is what causes partially frozen nitroglycerin to be so frighteningly unstable. Religiously avoid bringing nitroglycerin near to its freezing point (especially when you're working with 100mL of it!). I recommend to everyone who prepares nitroglycerin explosives to add ethylene glycol dinitrate to the explosive. This is used industrially to lower the freezing point of the nitroglycerin in dynamite. In the past, before ethylene glycol dinitrate was added, there was many terrible accidents where people inserted detonators into partially frozen dynamite, resulting in the instantaneous termination of lives due to detonation of the dynamite.

[ALENGOSVIG1]

I looked closely at the nitro and some is still froznen. What should i do? I placed it outside. Should i just leave it alone? The temp is around 0 outside and is slowly rising.

[Pu239 Stuchtiger]

It depends on how patient you decide to be. The freezing point of nitroglycerin is 13.1 Centigrade. I would wait until the temperature outside is around 15 Centrigrade... that will be a while. If you decide to be less patient, drown it in a deluge of warm acetone (maybe 25 Centigrade).

[ALENGOSVIG1]

Do you think it would be safe to gently pick it up and place it inside?

[Pu239 Stuchtiger]

That would be a matter of how fate decides to treat you. If you could pick it up so gently and delicately that the solid nitroglycerin inside wouldn't move at all, then it would be safe... otherwise, it is taking a risk that is not worth taking (I have no doubt that 100mL of nitroglycerin exploding in your hand would kill you). It would probably be best to just be patient... if you're not patient, and your luck plays out poorly, you won't get another chance.

[megalomania]

If you have to ask that question, then the answer is no. It's up to you, but I wouldn't move it. You can try placing a clear plastic container or bag over it, that's a gardners trick for keeping plants safe from frost. This assumes your beaker is in a place where the sun can get to it.

[ALENGOSVIG1]

I moved it about 50 feet away from my house. With my arms nearly fully extended, I Picked up the beaker with some large tongs and very slowly walked it to a safe spot. The tongs were Like the kind used for picking up garbage.

I was wearing a full face sheild at the time. The beaker the nitro was in was plastic. I wouldnt have moved it if it were glass, becuase of the shrapnel if it went off.

[Pu239 Stuchtiger]

That still wasn't a very good idea to do that. 160g of one of the most powerful high explosives known is not something you want to have go off anywhere near you! The tongs would have been torn to pieces and launched at you at tremendous speeds; that would surely have killed you.

<small>[ March 19, 2002, 08:16 PM: Message edited by: Pu239 Stuchtiger ]</small>

[0EZ0]

That's what i call a bloody gutsy effort! :D
Hehehe. Bet you won't be doing that again in a hurry. <img border="0" title="" alt="[Wink]" src="wink.gif" />

[ALENGOSVIG1]

Not all 159g was in the beaker. I had dissolved some in acetone. there was probally only like 90g of nitro in the beaker. I dont think it would kill me if it went off. The tongs were around 3 ft long plus the length of my arm almost fully extended is enough distance to be considered "safe". Well not safe at all but i doubt that i would be killed if it detonated. The part of the tongs that touched the beaker was made of some kind of flexible plastic covered in rubber, so no deadly shrapnel there.

[Pu239 Stuchtiger]

Then you would have been impaled with two 3ft steel rods. Certain death.

Anyways, please don't do something like that again. It simply isn't worth the risk.

[ALENGOSVIG1]

Well, thats not how the tongs are built. there is barely any metal on them at all. And yes i know it was not safe to pick it up, but the beaker was not in a safe place. I was planning on moving it in the morning but little did i know the temp would drop below 0. We are having renovations done in my house and i didnt want some dumbass worker to bump it or try to move it not knowing what it is.

According to the weater forecasts the temperature will drop below 0 again tonight. Im just going to let it freeze since its in a safe spot now.

<small>[ March 19, 2002, 08:59 PM: Message edited by: ALENGOSVIG1 ]</small>

[ALENGOSVIG1]

On another note, i just made 100 grams of some dynamite. The dynamite consists 70 grams ammonium nitrate, 10 grams corn starch, 20g nitro and some sodium bicarb. Ill Probally detonate it in a day ot two. Ill let you all know how it went.

[nbk2000]

90 grams of nitro is equal to .36 pounds of TNT. At three feet you'd have been exposed to 263 psi of overpressure. At 5 feet, 56 psi.

50 psi is the LD50 for blast exposure, so you'd have been killed most likely. Throw in the fragments from the beaker (plastic isn't safe either) and the tongs....death.

I'd have suggested setting up some plastic baggies around the flask and filling them with hot water, then covering with a box to keep it warm till the nitro melted.

Or adding warmed acetone by flowing along the side of the flask, NOT POURING IN! The splashing could cause an event.

Can ethylene glycol be mixed with glycerine for nitration? Or does it need to be seperate?

[Pu239 Stuchtiger]

The reason I considering pouring the acetone in to be a good idea is because he would want to dilute the nitroglycerin very quickly... slowly pouring it down the side of the beaker would have caused movement inside the beaker also, but it wouldn't melt the nitroglycerin nearly as quickly, nor dilute it as quickly. However, your idea of placing plastic baggies filled with warm water around the nitroglycerin was probably the best idea.

Yes, the ethylene glycol could be mixed with the nitroglycerin.

[nbk2000]

If you poured it in, that would have caused that NG immediately under the stream to partly melt, creating a slurry (momentarily, anyways) of NG crystals in the NG/acetone melt. These NG crystals would be bumping and grinding each other in the turbulence created by the pour.

Not good.

Best thing is to avoid the freezing in the first place.

[00Buckshot]

When you made that dynamite, how did you mix the NG with the AN? Or Sawdust if someone used that instead?
What would someone use to mix the nitro slurry up? Not a COFFEE GRINDER!....jk heheh

How sensative do you think the dynaite you made is? Also I assume that it could be set off without at detonater?

Furthermore is NG considered a high explosive? Or a primary?

Thank you

[DBSP]

HMMMM, how old are you 00? both primarys and secondarys are HEs there just two kinds of explosives, primary explosives and secondary explosives.

New in the buisness of explosives are you?? :D

[ALENGOSVIG1]

Well i just wrote a massive post but it didnt show up, so ill summarize what i said here.

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> At three feet you'd have been exposed to 263 psi of overpressure </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Yes but i wasnt 3 ft away from the beaker. 3 ft plus my arm extended. But your right, it was dangerous and i knew it when i did it.

Not all of the nitro was frozen, Just small bit. I didnt notice it at first because the amount was so small. Not saying that made it safe, but safer when compared nitro thats has more frozen particles.

The dynamite was made by carfullykneeding the ng/acetone into the AN/corn starch for 25 minutes then i let the acetone evapourate. The dynamite is insensitive to steel on steel hammer blow but a no.6 should detonate it reliably.

<small>[ March 20, 2002, 02:25 PM: Message edited by: ALENGOSVIG1 ]</small>

[Microtek]

On the subject of NG, you might consider reading the Tales of Destruction. It's a number of pages on the net that describes in detail a number of accidents involving NG. It's useful for discovering some of the pit-falls concerning NG.

[Zambosan]

Just a note... LD50 represents a 50% statistical probability of death. These types of figures (for blast exposure, toxin exposure, etc.) are either determine empirically over a wide sampling of actual events, or determined analytically through physical or computer modeling. Either way, they are a generalization created by discarding lots of information... in this case, effects of blast exposure *other* than death. If you held the beaker 8 feet away, you might be less than 50% likely to die, but you would almost certainly still be horribly disfigured. And the material making up the shrapnel has much less to do with its kinetic energy at point of impact than does the energy impulse that is accelerating it. The velocity it attains from the force of the explosion contributes exponentially to its ability to cause damage, while a difference the mass of the projectile (which is affected by the material density) can only have a linear mitigating effect.

[mark]

Id figure that much nitro would turn the container to dust. I know comparitivley tiny amounts of ap have that effect on their containers.

[drstrangelove]

Hello,I was wondering if you used the whole Uncle Fester formula for the entire experiment or just the mixing of acids?Is the Uncle Fester book the goods?I downloaded the text version from thr forum ftp and want to try my own experiment a.s.a.p <img border="0" title="" alt="[Wink]" src="wink.gif" /> This thread is a real inspiration! :cool:

[nbk2000]

Zambosan, I detect techno-babble. :rolleyes:

Anyways, even if the flask turned to dust, that dust would be flying at several time the speed of sound. And the 50 PSI exposure at 5 feet means blown out eardrums and (likely) permanent, and total, deafness.

You're wearing a face sheild, but that may not stop the fragments from penetrating. Even if they did, the radiant heat pulse could cause permanent damage or blindness to your eyes. Add in burns, etc. Nasty bit o' business, that.

Typical military hand grenade has 50 grams of HE.

Also, I was at one of those yuppie "Everything for your overpriced tract home" stores and saw a Kitchen-Aid mixer that'd be perfect for mixing explosive compositions remotely. It cost almost $250, uses a gallon sized steel or rubber (YES!) bowl, and has rubber paddles that intermesh (without touching) to mix doughs and such. Variable speeds from snails crawl to tornado. Built like the proverbial brick shithouse.

Put your absorbants in the rubber bowl, turn on to a slow mix, than start an NG drip. Use a really long extension cord and a big sandbag barricade and your personal explosives mixing plant is set to go. :D

<small>[ March 21, 2002, 01:19 AM: Message edited by: nbk2000 ]</small>

[RTC]

Look on the box to see where it was manufactured. Then either visit there web site (well let's face it, everyone and everything has a web site now) then either buy one from the manufactures for much cheaper or find who they sell them to, and go hunting for the cheapist one.

[Zambosan]

"Technobabble" is using complicated-sounding words to fool someone into thinking you have a point. I have a point, sorry if my choice of language wasn't to your liking. Alen was asserting that he was safe because the tongs were made of plastic. I imagine he thought as much because plastic is less dense than metal, which would of course be unsafe. My point? Energy = 1/2 mass * velocity^2. A broken piece of metal will be more massive than the same volume of plastic, therefore it will have less energy. This effect is linear; reduce the density by 1/2, reduce the energy by 1/2. However, the dominating factor is the velocity... which is why shrapnel is shrapnel, metal or plastic. The explosive force of nitro is going to accelerate any fragment of matter to a sickening speed, and it's going to tear you to shreds.

As far as the LD50 comment; statistics like that can convey a false sense of security, since they're stripped of so much information for sake of compactness... e.g. "If the LD50 for blast exposure is 50 p.s.i., then as long as I'm under that limit, I'm safe". Statistics are often either intentionally or unintentionally misused because people don't understand the data they really represent. I don't know Alen, but from his posts I gather that he makes a decent number and amount of high explosives. If he's rationalizing his actions because he was actually *6* feet away from a beaker of partially frozen nitro he was handling as opposed to *3* feet away, it sounds like he doesn't have a healthy enough respect for it. And I'd hate for him to suddenly, quietly disappear from this forum for no apparent reason.

[Mr Cool]

I have often heard people say that they handle explosives wearing a face shield. If you're loading dets from a few feet away, then that's good. But 90g of nitro?! I imagine that the face shield will act like the fragmentation sleave of a grenade, and it's sitting only a few inches away from what I assume is your only pair of eyes...
And obviously, face shields used for DIY or whatever are only useful when mixing acids etc. - they will offer little to no protection from shrapnel. Get some 1/8th" polycarbonate sheeting, and make a layered shield out of that. Then you will have some protection.

[Zambosan]

I've been looking into getting a spare set of eyes myself... :D

[Jack Ruby]

I take it the term "Techno Babble" means the same thing as Meta-Communication.

Meta-Communication is used in the in doctrination of Cults and other religions. What it does it makes the subject feel stupid but not wanting to look stupid by asking the just assume that the words were used in Context propper.

[drstrangelove]

What is the best and safest way to store nitro?Or what are the options availible for storing this explosive?

[nbk2000]

In the synthesis of <a href="http://www.orgsyn.org/orgsyn/orgsyn/prepcontent.asp?print=1&showprint=1&prep=cv2p0412" target="_blank">Methyl Nitrate</a>, they use a 22% solution of salt for the wash. This is the ideal concentration to prevent the formation of emulsions, which are a really bitch to seperate again.

As for storage, cool but not cold (don't want to freeze it), dry, in the dark, and in as small of a container as possible. Ideally, you'd divide it up into small (under 1 ounce) quantities and store them seperated by several inches of sand or pumice so if one explodes (for whatever reason), the whole lot doesn't blow. Avoid metal. Use only glass or plastic.

Or you can make a 70% NG/ 30% Acetone solution and store that. It's much safer for handling and storage, while still being explodable by non-boosted detonators.

[drstrangelove]

From everything I have read about nitro it would seem to be a good choice of explosive for my needs but the problem is I think I would need around 1 kg. Is the homemade nitro out of the question for these larger type jobs? Is the nitro more sensitive in larger amounts? I would make the nitro in ten small batches but I want to detonate it all at once.Once you have purified the product can you pour one 100ml batch into another 100ml batch to have 200ml and so on? Or is this madness? What about transportation of nitro? Can you take her in the car? What are the main reasons for nitro detonating by accident?

[kingspaz]

ahahahhaha......sounds like madness to me! i don;t think their is one main cause for accidental detonation. i beleive with improvised nitro a greater risk would arise from improper neutralisation leading to greater sensitivity. wouldn't it be a better idea to mix it with PETN to make some sort of dynamite while still maintaining its high velocity of detonation? or mixing it with acetone and detonating that if you require a liquid explosive?

[Madog555]

mixing it with PETN would make a very powerful explosive, just think, two of the worlds most powerful explosives, MIXED!

<small>[ March 23, 2002, 05:44 PM: Message edited by: Madog555 ]</small>

[kingspaz]

hey i also just realised when PETN is mixed with water its velocity of detonation increases, right? i'd guess this is due to it creating a uniform density so the shockwave can propagate thoughout the charge in a faster, more uniform manor. NG would have a similar effect due to its liquid state. this stuff would be amazingly powerful! :D :D :D

[nbk2000]

If you need a truely safe form of nitro for transport, just mix one volume of NG with 2 volumes of acetone. This will render it almost totally inert.

Once you're at the job site, you leave the mix in wide, shallow, pans to evaporate off the acetone. Once it's down to a third of its original volume, you've got straight nitro again.

Course, this may take a long time if you're in freezing cold or rainy weather.

You could probably eliminate the wait by pouring the NG/Acetone mix into warm water, thus diluting the acetone suffiently to seperate the NG which would form a layer at the bottom of the water. Seperate and use.

BTW, a kilo of NG is equal to almost 5 pounds of TNT. That's a lot so be careful.

You'd want to be at least 20 yards away, and behind solid cover (boulder, concrete, etc) to avoid dangerous concussion. Let's not forget eye and ear protection, eh? <img border="0" title="" alt="[Wink]" src="wink.gif" />

[da man]

I know this is a bit of a newbie question but when making nitro how concentrated do the acids really have to be? i've made a small amount before (5ml) from the KNO3/H2SO4 method but it is very inefficient. In a couple of days i will be getting heaps of 70% nitric acid and i already have 99% sulphuric, so would a mixture of these do for nitro? The acids couldn't have to be too concentrated if the KNO3 method works, which would have a significant percentage of KHSO4 impurities.

[00Buckshot]

These are the "Tales of Destruction" Its about NG use along time ago.
Someone mentioned it before.
<a href="http://www.logwell.com/tales/menu/" target="_blank">http://www.logwell.com/tales/menu/</a>

[VX]

Is it possible to leave the Nitro in the mix for too long? I mean, as long as the temp doesn’t rise can the acids mix be left for a few hours? I ask this because I have no good way to mix it, but I want to ensure that all the glycerine is fully nitrated.

Also I assume that the nitration of the glycerine proceeds via mono and dinitro glycerine, so if not left for long enough is their a chance that the product could be mostly mono and dinitro glycerine? Therefore making it advantageous to leave the mix reacting for longer than necessary.

Edit: Alen what happened to the dynamite that you made? Did you detanate it? Also have you still got plans to try the Sulphuric/Nitrate method?

Thanks, VX

<small>[ March 28, 2002, 06:43 AM: Message edited by: VX ]</small>

[andreas]

<a href="http://www.angelfire.com/mac/detonation/MVC_096F.JPG" target="_blank">http://www.angelfire.com/mac/detonation/MVC_096F.JPG</a>

A photo of what 1 gram of mhn can do to a can.
think of what 90 grams of ng can do to YOU

[mike]

For those of you who were talking about the nitro/PETN explosve, I just read a little info about it in "the chemistry of powder and explosves". It is under the PETN section and basically, this is what it says:
density: 1.65 (80% PETN 20% NG)
dynamite-like
can be 10-30% nitro
a plastic mass
doen't separate into its components
suitable for loading dets or shells
initiated w/ .04g of lead azide

If you want the whole thing just ask, but I coverd most of it there

[mike]

btw, you need to use white nitric acid for NG, right?
peace out.

[Pu239 Stuchtiger]

Red nitric acid will suffice.

[Microtek]

Actually, 62% nitric is sufficient if using a little more sulfuric. Concerning the PETN/NG explosive, I have done a little experimenting, and I don't think it will form a homogenous, flexible mass simply by mixing. I think you need to either heat it up or add a little acetone to help dissolving the PETN. Then when the acetone has evaporated, reasonably plastic material is left.
On the subject of storing NG I prefer to dissolve it in ethanol as that is less volatile than acetone.

[randomquestion]

This is the shit they use in those racing cars...Like in the movie "The Fast and the Furious"...Not worth hooking up to any old car. It would probably blow after a couple of seconds. :D <img border="0" title="" alt="[Wink]" src="wink.gif" />

seriously, *do not* make posts like this! It contains no useful information and makes no sense. Neither NG or PETN are used in any car, nor ethanol, nor acetone. The closest with is methanol, which was *not* used in The Fast and the Furious.

<small>[ May 29, 2002, 08:20 AM: Message edited by: Anthony ]</small>

[mike]

while were on the topic of NG mixes, have any of you heard of a mix of NG and Dinitrotoluene? I read about it in that tales of destruction site. It says there that it was nick-named "red glycerine" or as Dupont named it "EL-389-B". If anyone has any information on this explosve, it would be greatly apreciated.
Btw, could the PETN in the petn/ng explosive be substituted for RDX? Also, I've read in the uncle fester's h.w.e. book that the petn/ng plastique is more powerful than c-4!
peace out.

<small>[ May 29, 2002, 09:43 PM: Message edited by: mike ]</small>

[cutefix]

I think I hear of this long time ago,but not that name but the composition looks similar.
A blend of 20-40 dinitrotoluene and 80-60 nitroglycerine.I cannot just remember its specific properties except that it is indeed less sensitive than pure nitro.

Regarding this PETN/NG it will indeed be more powerful than C-4 because you are using an energetic plasticizer nitroglycerine which does not diminish the power of the main explosive but supplement it.It s VOD is roughly 8200 meters per second .
Compare that with C-4 which gives an average of 8000 meters pre second, because
The polyisobutylene binder is inert and does not contribute any energy to the plastic explosive…..

<small>[ May 30, 2002, 07:20 PM: Message edited by: cutefix ]</small>

[VX]

Randomquestion, in "The Fast and the Furious", are you refering to NOS? If you are, then the substance is actually Nitrous Oxide, N2O.

Go <a href="http://www.chm.bris.ac.uk/motm/n2o/n2oc.htm" target="_blank">here</a> for more info.

[mike]

would this petn/ng plastique work with rdx insted of petn? thanks!
peace out.

[Microtek]

No I don't think you could use RDX instead of PETN. The NG would probably not be able to plasticize the RDX, so you would end up with a slurry instead of a plastique.

[mike]

hmmm, slurry eh? what do you think some of the other ingrediants would be to make this military-sort of slurry? I'm guessing maybe guar gum or borax but then again I don't know much about slurries. thanks!
peace out.

[cutefix]

A slurry is less plastic and more fluid ,and usually contains water.Its not very important from military standpoint except maybe for the fabulous daisy cutter which is very different from typical military explosives.
Its more related to commercial blasting explosives in composition.
Meanwhile a slurry method can be used in the fabrication of well known plastic explosives in which a self-explosive(or a unitary explosive such as RDX/HMX or PETN) is wet with water and coated with combination of structural binders and softened by plasticizers in a granulator(mixer).
I think you can find more info about this elsewhere in the High explosive section(related to C-4).
If you want to make this slurry method in making plastic explosive there is no need for gums and crosslinking agents as the result will be waterfree composition-a plastic bonded explosive.
In your previous post where you want to know if RDX can replace PETN:
If you want to use RDX in your NG/PETN ,you can add 0.5-2.0% nitrocellulose to the Nitroglycerine so that it will bind it to the cyclonite.
A combination made with RDX or PETN and NG will not make a a very stable plastic explosive.It would appear loose and tend to flatten out on storage.It should be bound with a portion of nitrocellulose which serves as structural binder between the nitroglycerine and cyclonite/or even Penthrite.

[Microtek]

This was what I was referring to; as there is no binding action between the NG and the RDX, you will end up with a high explosive sludge which will certainly be powerful but the handling characteristics will not be so good.

[mike]

ahh, I see (said the blind man to the deaf dog). I'm guessing that the good ole kewl ping pong ball method for NC will be suficient for turn the NG into kind of a blasting geletin. thanks!
peace out.

[ALENGOSVIG1]

I've gotten a few emails asking about nitro synth so i decided put my method on my website.

<a href="http://www.angelfire.com/linux/alengg/NG.html" target="_blank">http://www.angelfire.com/linux/alengg/NG.html</a>

Tell me what you think.

[cutefix]

That is cool Alen.This will helps would be new NG experimenters in obtaining the proper result.
As you have good presentration skills why not post your other explosive synthesis graphically as this one.

[ALENGOSVIG1]

I have. I just havent posted the links until now :)

I dont have alot done but im working on it. I've gotten 4 done so far. Soon i'll have picric aid and hexamine dinitrate done.

<a href="http://www.angelfire.com/linux/alengg/AP.html" target="_blank">http://www.angelfire.com/linux/alengg/AP.html</a> - Acetone peroxide
<a href="http://www.angelfire.com/linux/alengg/anmnn.html" target="_blank">http://www.angelfire.com/linux/alengg/anmnn.html</a> - AN/MNN/C
<a href="http://www.angelfire.com/linux/alengg/mnn.html" target="_blank">http://www.angelfire.com/linux/alengg/mnn.html</a> - MNN
<a href="http://www.angelfire.com/linux/alengg/NG.html" target="_blank">http://www.angelfire.com/linux/alengg/NG.html</a> - Nitroglycerin

[cutefix]

Most of these links are informative.....It would be best if explosion pictures can be added for dramatic effect... :D

[Zambosan]

Nice pics!

<small>[ July 18, 2002, 01:01 AM: Message edited by: Zambosan ]</small>

[00Buckshot]

Great pics, they make the synth much easier to follow.

However, does anyone have any dealings with the KNO3 method? Pics for this NG synth would be ideal.

[DBSP]

I could give the H2SO4/XNO3 method a try if you think that it would work with diethyleneglycol. The bottle says 100% I don't belive that but maby it's worth a try, what do you think I'd supply pics.

[andreas]

What's up with the black color off you're sulphuric alen

[VX]

He (along with many others) uses drain unblocker for his sulphuric acid. It's very concentrated, and cheap but most importantly readily available. Anyway the black/ red colour is due to the dye that the manufacturers put in it.

[Zambosan]

Why do they want to add dyes in the first place? It's a cleaner, isn't it???

<small>[ July 18, 2002, 12:58 AM: Message edited by: Zambosan ]</small>

[PYRO500]

I have bought similar brands (exact same container same location and style of content labels but only one of the 3 gallon jugs I can remember buying had no dyes and was just about clear.

[andreas]

Whell the ones I can get are 97% pure and contain no dyes at al.
It's a power drain opener also.

[00Buckshot]

The first bottle of H2SO4 drain opener I bought was a rather expensive name brand and it was red, then I bought some much cheaper no name opener in a white bottle and it isn't red at all. So try the cheap stuff.

[Madog555]

andreas, you live in a good country. thats probaly why

[andreas]

Whell I must agree that holland is a country where there is much less controlled sales and so on. But after september 11 and the torrorist with bombed shoes things here are increasingly difficult to find. Afterall this is a strange hobby that people don't or don't want to understand except you're friends. They love it when something goes off and is followed by a large flash and bang.But if the die doesn't interfere with reactions than I think there shouldn't be a problem and if it does try activated charcoal(norit) it can remove dies from most substances and can be reactivated.

<small>[ June 27, 2002, 08:03 AM: Message edited by: andreas ]</small>

[Celtick]

Andreas can you give me the brand name or store name of the drain opener you’re talking about? In the local stores I can only get HG opener witch is a NaOH solution and some other solid opener witch is also NaOH.

[andreas]

Whel I don't know where you live but It's called MEGA super ontstopper. It is produced by a company called mega cleaning products bv.
in Roosendaal. if you need more info contact me on this email: kramrak@hotmail.com if you have msn you can add mee to you're list.
Ps also buy the prilled NaOH you'll need it sooner or later. P.S. I've made some NG with the ammoniumnitrate sulphuricacid method but the yeild seems rather low how long to react this to get max yeild?

[mr.evil]

Alen,
Do you have the pictures of the Detonation of your NG?
Didn't you got a (horrible) nitro headache??

Last night i was watching a Medical program, and there was a man who just gotten a hartattack, so they gave them Nitroglycerine.. It was a little bottle with about 10ml of NG in it, and she shaked it a little bit!! <img border="0" title="" alt="[Eek!]" src="eek.gif" /> But anyway, i think the man with the hartattack did get a big nitro headache!

edit: some spelling errors

[Anthony]

What was in the bottle was probably &lt;5% NG solution.

[xtreme]

Celtick:

I have found H2SO4 in the Netherlands by a shop (ned. =Bouwmarkt) called "Big Boss". It is a drainopener called "Ultra Ontstopper, vloeibaar" and it contains 96% H2SO4 in a clear solution.
I have paid 7.15 Euro for 500ml

I haven't tested jet, but have a good feeling about it.

[mr.evil]

that's about the same price of MEGA super ontstopper, i've paid for that stuff 14€ per Liter.

I suggest you go to Belgium, there are lots of Chemical shops that sell 98% H2SO4 for 4€/L. Vulture, Brainfever, Philou do get their chemicals also from that shops.

[ALENGOSVIG1]

No, I dont have any pics or videos of nitroglycerin detonating. I'll try to get some though.

Also, i finally have pics of the KNO3/H2SO4 nitro procedure. Tonight ill put the KNO3/H2SO4 method with pics on my site.

[mr.evil]

I Can't wait to see them, does the NG/Acid mix get kinda thick? i noticed that when i make MNT with the KNO3/H2SO4 method.

i'm a chicken, i'm scared to make NG :D

[ALENGOSVIG1]

Yes it gets kinda think. Especially when using potassium nitrate which is less soluble than ammonium nitrate.

<a href="http://www.angelfire.com/linux/alengg/NG2.html" target="_blank">http://www.angelfire.com/linux/alengg/NG2.html</a> - nitro using the XNO3/H2SO4 method.

Its just my rough draft. Im going to update it later and add a few things. Im not really happy with the pics either. I was in a hurrey and they didnt turn out. I think i'll do the process again and take better pics.

as usual, the yeild was pretty bad compared to when using good nitric acid. I used 100g of sulphuric acid, 40g of ammonium nitrate, and 22g of glycerin and got 21g of nitroglycerin before it was washed.

You dont really have anything to be afraid of mr.evil. NG is much less sensitive than AP. If you are carful and treat it with respect you wont have problems.

<small>[ June 28, 2002, 05:31 PM: Message edited by: ALENGOSVIG1 ]</small>

[mr.evil]

Hey,
Alen; Very nice...
I think i will try to make NG tomorrow, as i'm now busy with to distillate my HNO3. I will start with not much Glycerine, about 1-2ml.

Why is the Forum so quiet the last few days?

BTW.
Didn't your NG/Acid mix get thick, like honey?

[ALENGOSVIG1]

I wouldnt say it was as thick as honey, but it was quite thick.

One thing I forgot to mention is that when using ammonium nitrate or calcium nitrate to make nitro you end up with solid byproducts in your nitro. The best way to get it out is to pour the nitro through a seive to filter off the solids.

I dont really recommend you use potassium nitrate. The mix will get very thick and it'll be harder to contol the temperature. If you do use potassium nitrate, (you'll have to calc how much is needed) use a bit excess sulphuric acid so the mixture isnt so thick.

<small>[ June 29, 2002, 04:20 PM: Message edited by: ALENGOSVIG1 ]</small>

[mr.evil]

yeah, i used KNO3 when making MNT. There were some pieces floating around in the Acid/MNT. But after a night the pieces were disappeared :rolleyes:

Here you can see my MNT: <a href="http://www.geocities.com/tshadowpp/MNT.html?1025250302490" target="_blank">http://www.geocities.com/tshadowpp/MNT.html?1025250302490</a>
also see this: <a href="http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=1;t=000520" target="_blank">http://www.roguesci.org/ubb/ultimatebb.php?ubb=get_topic;f=1;t=000520</a> thread.

i've just distillated some HNO3 so i will make more MNT (for DNT and TNT) and maybe some NG. (when i have enough aspirin and coffee to kill the pain caused by the NG, alen; can you give me some tips etc. about the nitro headaches? Maybe some Details?)

Cya :)

[ALENGOSVIG1]

The nitroheadaches are bad at first, but you become immune quite quickly and you'll no longer get headaches when exposed to NG.

2 or 3 aspririn and a cup of coffee will kill the pain.

[kingspaz]

wouldn't the aspirins be a bad idea? apsirin thins the blood as does NG. NG + aspirin = piss thin blood which cannot be good for you...

[Anthony]

IIRC, either heroin or cocaine is a vaso-constrictor and so will counter the effects of the NG - they keep it behind the counter at Eckerds so you need to ask the asistant for it :)

[Madog555]

i use KNO3 for MNT too. i wrote a method in a PDF on Rack-a-Rock. the ratios are wrong though. they are close.

[mr.evil]

i've read that PDF madog, very nice...

Sorry for going off topic..

[ALENGOSVIG1]

The pdf looks good. I'll have to make some MNT soon.

I just detonated the nitro a few minutes ago. I made some dynamite and detonated it with 1g of AP. The dynamite consisted of 20g NG, 13g AN, 4g corn starch, and .5g sodium bicarb. I drilled a hole in a 1.5 ft. diameter rotten stump and placed the charge inside. Upon detonation, the stump was blown to bits :D

[mr.evil]

that's cool alen, did you take any pictures?
Can someone please mail me the PDF, because i don't have it on my computer anymore and it looks like it isn't on the forum FTP anymore...

Thanks :)

[DBSP]

How concentrated must the glycerine be in order to function well?

[mr.evil]

well i guess 98-100% as the water in it dilute the acids.
Just heat the glycerin in a beaker, and let al the water eveporate off at 100degrees C.

Damn, just breathed in some NO2, headache :rolleyes:

[HOOPS123]

Today I had a dream. I drempt that I made NG via ALENGOSVIG1's .pdf (NG 3) using Ammonium Nitrate from cold packs, 98% Sulfuric Acid, And glycerin. I stepped down the expierament to 1/4 the size on the pdf (It called for FAR more glycerin than I thought I would be comfortable with). I Followed the instructions exactly. Several minutes ago (I just woke up) I added 250 ml of water to honey-like mixure. After letting it settle I took theses pictures.

<a href="http://image1.villagephotos.com/pubimage.asp?id_=425366" target="_blank">http://image1.villagephotos.com/pubimage.asp?id_=425366</a>
<a href="http://image1.villagephotos.com/pubimage.asp?id_=425367" target="_blank">http://image1.villagephotos.com/pubimage.asp?id_=425367</a>

As I have never drempt of making NG before this, I am wondering if you guys think that it looks about right. I am aware that the bottom layer should be the NG, which I have partially extracted. What are the other layers? Im curious about the red "beads"

EDIT: The off white liquid that was at the bottom of the jar has disappeared. The Red "bead" like formations appear to sit on the bottom now but I can't be sure. Also, there is a continous stream of bubbles to the top. Is there anything I have to worry about?

EDIT: Spelling

<small>[ July 12, 2002, 04:28 PM: Message edited by: HOOPS123 ]</small>

[nbk2000]

You're not supposed to let it sit overnight! Only 15 minutes or so.

Red indicates excess NOx, and the off-gassing indicates decomposition. Dump it in a river or deep ditch and try again because your batch is dangerously contaminated.

[HOOPS123]

All of this happened within 20 minutes, which confuses me. One second the NG was there, then next, it was slowly disappearing.

[ALENGOSVIG1]

I'd say either you left it for too long or the reaction temperature was too high.

[HOOPS123]

I was very careful to keep the temperature under 15 degrees. During the whole reaction process the temp was about 5 degrees... could it have been too low?

[nbk2000]

Nitro will redissolve in the acid if left sitting too long. Once you have seperation, you dump it in water. Let it sit and it'll disappear just like you saw.

If the temp was too low, the reavction wouldn't have happened at all.

As an aside, anyone trying the xNO3/H2SO4 method may wish to add enough methylene chloride to the mix to make it a free flowing fluid, rather than the honey consistancy it normally has. This improves mixing and contact between the reactants.

Also, a fish tank aerator pump hooked to a piece of PTFE or LDPE tubing (end flame sealed and with many pinholes melted in it) as a bubbler would help with frictionless stirring and flushing out NOx from the mix as it's formed, thus improving safety by reducing acidity..

[DBSP]

Ok folks I need some QUICK help, I've just made some NG with the KNO3/H2SO4 method, what I need to know is how I shuld remove the KHSO4 from the NG. I havent seperated it from the water yet but I will after I'm finished writing this. I'll add it to some dest water and NaHCO3 right after the seperation. I'll be using the NG as soon as I can so the storage time will be very short.

And I've got some pics but I'll put them up later.

[ALENGOSVIG1]

Pour the nitro through some kind of a seive. Use whatever you can find. One of those "tea ball" things will work.

<small>[ July 27, 2002, 01:53 PM: Message edited by: ALENGOSVIG1 ]</small>

[xtreme]

Is there anybody on the forum who mades NG and have an accident ?
I'am a little bit scarred of making NG seeing al the warnings :rolleyes:

On the other side.....it's so easy to made and so powerfull.

I will try to make NG or MN (Methanol Nitrate) someday (...this weekend perhaps :) )

The properties (vaporation/storage) of NG looks better than MN.

[ALENGOSVIG1]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> I'am a little bit scarred of making NG seeing al the warnings
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">Its not that sensitive when compared to primaries like HMTD or AP. Just wash the NG properly and be carefull with it. You wont have any problems. I dont think anyone here has had accidents with NG. If they have, i'd like to hear about it though.

[xtreme]

Happy to hear that.

I have no problems with the sensitivity of AP/HMTD.
Just don't put a beaker containing AP/HTMD on the corner your desk <img border="0" title="" alt="[Wink]" src="wink.gif" />

Than perhaps I try this weekend to make some NG and put it in AN to make it (more) stable. Or in some wood meal to make Dynamite :D

[kingspaz]

wait a second....i'm confused! NH4NO3 &lt;=&gt; HNO3 + NH3 strongly to the left BUT this means some acidity will allways be present...H+ ions sensitise NG right? or is it safe because AN is so dam insensitive the extra sensitiviy of the NG just makes the mix detonable?

[xtreme]

NG is used to make AN sensitive.

You can find this in the book "Kitchen Improvised Fertilizer Explosives" (downloaded PDF) by Tim Lewis
This book full of AN based explosives including all data (VOD, sensitivity, ....)

4% NG in AN: requires 1/4 stick of dynamite
8-15% NG in AN: requires blastingcap #6 :D

That would be nice for detonating ANFO explosives....isn't it ? <img border="0" title="" alt="[Wink]" src="wink.gif" />

<small>[ July 27, 2002, 05:48 PM: Message edited by: xtreme ]</small>

[kingspaz]

xtreme, i know its used to sensitise AN! of course i understand that. the thing i am wondering about, as i said in my last post had you paid more attention to what i was saying, was that NH4NO3 is slightly acidic and acidity makes NG unstable. if the AN/NG mix is left and some of the NG ouses out then that NG may be more sensitive since it could contain some HNO3 from NH4NO3 &lt;=&gt; NH3 + HNO3.

[xtreme]

ok.....it gone be wood meal ?! Making my first classic dynamite :rolleyes:
Or are there better options to stablize NG ?

[ALENGOSVIG1]

Powdered ammonium nitrate with some fuel and a bit of sodium bicarb.
That way the absorbant actually detonates, unlike with wood meal.

[xtreme]

Sodiumbicarbonate with AN/NG

I don't think that wil do the job. Or you must put a lot of sodiumbicarbonate to the AN/NG what makes it less sensitive.

Other options......bird sand ("silversand"). or the stuff that they use to catch cat-piss/motor-oil ?

Or somethink what absorbe real good and getting hard (without creating heat)

Edit: I was thinking.....nitrated cotton-wool (NC)
Is that not an option ?

<small>[ July 27, 2002, 07:32 PM: Message edited by: xtreme ]</small>

[ALENGOSVIG1]

Why not just stick to making ammonia dynamite instead of things like bird sand etc. Bird sand doesnt detonate, but AN does.

The sodium bicarb is added to neutralize any acid.
You only need a pinch of sodium bicarb in the dynamite. Around .5% is a good amount.

Adding NC to NG creates nitro gelatin.\

<small>[ July 28, 2002, 12:08 AM: Message edited by: ALENGOSVIG1 ]</small>

[Pu239 Stuchtiger]

If anyone who used to post here had an accident with nitroglycerine, we aren't going to hear about it, because they're dead.

I have made nitroglycerine, and several other alcohol-nitrate esters before. I have never had a nitroheadache.

[BrAiNFeVeR]

Well, I had a runaway nitration once, but that can't be considered an accident (no I didn't do it on purpose!!)

About the nitro-headaches, some people don't seem to be affected all that much, nad some get it from sniffing a bit of vapor.

I only get a mild headache when I taste a bit when biting my nails or something. I even tasted it on purpose once (a very small drop on my finger) and the headache was far from my worst headache ever !!

BTW: I like the taste :D

[xtreme]

Pu239 Stuchtiger

Why should somebody who have an accident directly be dead.
It's not that easy to KILL a human.

Watch the news. Somebody walks with his body full of explosives (kilograms of C4/Semtex !) into a shop or bus and most people survive this. Yes, a lot of people are injured (fragments (glass,..) into body, damage on ears from blast,.....). I only say....it's not that easy to KILL somebody.

If the army used an explosive with the goal to kill people they surround the explosive with fragments of glass, metal or stones. And there goal is mostly not to kill somebody but to injured somebody. It takes 2 other man to take care of the victim...so that's three men out of order! A dead man is "only" one man out of order.
If the army used only the blast to people...it's mostly "just" to scare the enemy, to demotivate them, to keep is head down so they can't shoot that moment. A granate with this goal contains something of 500....600 grams of TNT !!

(sorry....the army have teach me some bad (=unconventional) thinks :( )

[nbk2000]

If a couple of ounces of NG explodes in your hands, you're going to:

A) Be minus two hands to type with

B) Minus two eyes to see with

and probably

C) Locked up where there is no internet for the next few years.

So, yes, you can survive an accident with NG, but you're not to likely to be in any condition to tell us about it here.

[xtreme]

Here in the Netherlands you get (almost) everything you want in jail (tv, dvd, women, ....) :) .....if you come in jail (to less place)

But that is realy not my goal ! <img border="0" title="" alt="[Wink]" src="wink.gif" />
No hands, eyes, ..... , = can't see or touch women = better be dead. :D

[andreas]

Think I found the reason caffeine works against nitro headages.
I don't know who told that heroine and so would help.
qoute:"Caffeine is an addictive drug. Among its many actions, it operates using the same mechanisms that amphetamines, cocaine and heroin use to stimulate the brain. On a spectrum, caffeine's effects are more mild than amphetamines, cocaine and heroin, but it is manipulating the same channels and that is one of the things that gives caffeine its addictive qualities. If you feel like you cannot function without it and must consume it every day, then you are addicted to caffeine." and asprin is a drug that makes the blood more flowable <a href="http://www.howstuffworks.com/caffeine2.htm" target="_blank">http://www.howstuffworks.com/caffeine2.htm</a>
A real interresting read :D

<small>[ July 30, 2002, 04:36 AM: Message edited by: andreas ]</small>

[DBSP]

Everything fucked up when I started adding the NG/water to the bicarb solution, I added it carefully but it started foaming like hell and I lost most of my NG. It seemed like the NG left dissolved as I nutrolised the remaining acid and I ended up with nothing.

This is how much NG I had from the beginning(about 10ml):(including the KHSO4)
<a href="http://w1.478.telia.com/~u47804009/E&W/NG_at_the_bottom_with_the_KHSO4.JPG" target="_blank">NG at the bottom with the KHSO4</a>

I will try it with 62% HNO3 next time, the yield might be porer buth I don't have to mess with the KHSO4, after the addition of KNO3 to the H2SO4 it was just a hard lumb, so I added a bit extra H2SO4 to make it more liquid, this is what I don't want to deal with.

<small>[ July 31, 2002, 12:42 PM: Message edited by: nbk2000 ]</small>

[rjche]

In USA you can buy 99.5% pure glycerine by the gallon at veterinary supply houses. It is used a lot by horse farms, as a topical sweating agent for poltices to help remove fluids from inflamed and swollen areas, and as a skin softner. You got horses right? They got bruises Yes? Then you need glycerine, in large amounts yes? Act knowledgable and they ship it but you pay shipping. It is NOT a hazmat item, but is heavy.

One supply house which sells online or by phone with charge card is:

Jeffers, 1 800 533 3377

Glycerine, 99.5% pure, cat No. NR-G5-17, Gallon, FOB 10 lb, $22.50

Propylene Glycol Cat No FQ-A6-17, Gallon FOB 10 lb, $10.95
Cat doesn't spec purity, probably near 100% though, ASK via phone if concerned.
NG is one of the easiest primaries to make, IF you know how to use it.

For experimentation it is easiest used in empty 22 LR hulls. Fill hull half full of cotton not packed add enough drops NG to moisten cotton not flooded. Slide into hull piece of RG58 coax used on CB antennas, avail at Radio shack or other electronic places, and ham flea markets, Cut the end of the cable square flat with large sissors or cutters. Make sure the inner conductor is centered and not touching any fine wires from sides shielding. Crimp it same as a blasting cap.

This is about a #3 blasting cap alone.

Put this into a larger hull, say an SKS empty round, again using cotton, moistened but not flooded with NG. Seal end of large cartridge with bondo. Do keep NG off the inside edges of the hull where bondo must bond and off the coax. It washes off easily with alcohol dipped Q tip.

This sks hull almost filled with cotton and with about a cc or two of NG absorbed is way more powerful than numbered caps, and will make most lazy explosives go.

To fire the cap, separate the other end of the rg58 cable into shield and inner conducter for a distance of about 6 inches. Hook one to frame and other to spark plug wire and crank engine. OR&lt; use a stun gun one pin to shield, one to center wire, it will spark over in the small cap, and away she goes. No waiting, instantenous, which is quite valuable to the experimenter. Can time it to follow along with a loud thunder, to conceal the experimenting. This cable is very safe because it takes about 6000 volts across the center conductor to shield to make it go. That's a lot. The shield protects the inner concuctor from that from lightning strikes. Also keep the far ends connected so no matter what happens there can be no static electricity build up on the cable. separate them only for the firing.

NG Wetted Cotton is a very sensitive explosive, takes only a #1 cap to set it off, or a smack with a hammer, or rock, etc.

Shrapnel from the 22 hull is usually about 15 pieces, if fired in a pint of sand, and sifted to see the shrapnel sizes. The base of the 22 hull will have deep indentations of grains of sand that the end smacked into.

Easy way to do experimental blasting without having a source of caps.

Nothing around that LOOKS dangerous to spies IF YOU KEEP THE NG well hidden. Remember it stinks a lot. Dog can smell it easy as you smell a skunk. MUST be contained in metal paint can with zero of it on the can. Any rubber or plastic gasket will leak fumes, and bow wow wow, gotcha. Remember fumes or contact with skin causes drastic drop in blood pressure and major headaches. Antihistamines help elevate pressure back. You do get adjusted to it no headaches with regular exposure.

Handling dynamite out of its wrapper by a non accustomed blaster can send you to the emergency room.

Fellow once made a big ball of 75% stuff by unwrapping and wadding it up using bare hands, and about 5 minutes later was unable to continue work, and swore off dynamite, between uttering prayers like a hoe pukeing into a throne, after a major load of rot gut.

Other than that minor problem, its a dandy explosive to make and use.Its sensitivity to accidental explosion is wildly exaggerated.

For years it was shipped in bottles via rwy express as a medcine, till one super hot day, a clerk dropped a pint of it on the loading dock, where it fell about 10 feet onto hot concrete. Apparently a piece of glass violently scratched some pavement wet with NG and it took out a fair size bite of the dock. Caused major amens, and regs later about shipping it. It takes a cap to make it go frozen, and thawing does not represent any hazard, IF you do not do it by putting dynamite near a hot stove up close, so the temp of the surface can get to god knows what. That led to several cabin removals of miners blasting for GOLD, et al. Those removals led to wild stories about dangers of frozen dynamite. Actually its much less sensitive when cold as are all explosives. Remember they take bombs down to liquid air temp at which neither caps nor explosives will detonate, and usually all one can get them to do is burn.

All that is by way of informing the experimenter so he won't be so scared of the stuff that he makes mistakes and gets into trouble.

If it turns yellow, when brewing it it is likely to puff of and throw very hot acid everywhere. Watching a 250 CC beaker of it perking once, early experiments without cooling it turned light yellow, in about 5 seconds darker yellow, with minor bubbles in it, and about 3 more seconds red, with red fumes, at which time the experiimenter dumped it into a bucket of water. Lucky SOB. Dump it while its still yellow if you try that. IT CAN DETONATE... A table spoon of it can put you in the emergency room, if you get that far. IF you're holding it when it goes, and it decides to detonate, expect no hand or hands, maybe blindness, some hearing, maybe serious lung and gut bleeding. Really a bad hair day. Best to NEVER pick it up if hot at all, but use some kind of holder to keep distance. You need a thermometer in it at all times and keep it stirred so hot spots don't develop. They can not be noticed till one goes yellow, and you might not be looking right then. At temps above about 60 F it is too close to running away to trust that. It can go from 60 to past 200 in seconds. Above 200 it is anybody's guess what the hell it will do.

In factories they had a slide chute like emergency exits for airplanes. If temp went up alarms sounded, and if the pot turned yellow it meant time to quit trying to fix it, and they pulled a chain on a valve which dumped it into a pool of water below.

Everyone jumped into the slides which in seconds took them about 100 yards distant behind a barrier down hill from the plant. It was steep then more shallow at the end. They hit the end straw pile going about 20 mph. The plant had strong walls, very weak roof, to point blast upward. They didn't take all those precautions for the hell of it.
BE CAREFULL WHEN MAKING QUANTITYS OF IT.

STORE IT DISSOLVED IN ACETONE OR ALCOHOL, 70% NG 30% solvent is safe to ship and drop, and all such stuff. Evap solvent when needed for use.

A drop on paper burns with blue flame much like alcohol. You can make dinitro instead of trinitro, Density is best way to tell, or freezing point. Di takes a bigger whack to get going, and not as powerful. Same headaches, look same, smells same. Di comes from too much water in mixed acids.

[Richy]

i purchased some glycerin from the supermarket a while back... cost about $3.50 AUS for a 200ml bottle it states on the bottle that its used for application on dry skin, as you said. making an educated guess, would you assume that this is high enough in concentration to synthesise NG? if not, can i compensate with stronger concentrations of acids? or could i simply boil of the remaining water?

[ALENGOSVIG1]

Heat the glycerine to to about 120-150 celsius for about 30 mins.

[Richy]

thanks a lot, ill start the synthesis as soon as i get my hands on some KNO3 (to make HNO3)..... i tried the synthesis with soil but the yield was shit and the final product was impure..... bloody anarchists cookbook...last time i open that file... i suppose ill just check out the chem companies or the hydroponics store. gettin ure hands on chemicals isn't the easiest task in AUS...

[da man]

Richy if you live around Sydney i can give you the name of a hydroponics place that sell ammonium, and potassium nitrate. They only sell chemicals for hydroponics, you can just walk in and ask for a few kilos of ammonium or potassium nitrate. And for ammonium nitrate, its only $1.50 per kilo!!
I looked for ages at hydroponics stores before i found this one, i just emailed all these hydroponics stores with a phony email adress. But this was the only one that sell the nitrates in Sydney!!
If you would like more info, email me at the_negotiators@hotmail.com

<small>[ October 04, 2002, 08:05 PM: Message edited by: da man ]</small>

[xyz]

Check agricultural supplier as well richy, I get KNO3 for $2.00AUS a kilo and my Ammonium nitrate for $1.00AUS a kilo from a shop which sells agricultural products and fertilizer. The hydroponics shop near me also sells 50% Hydrogen peroxide (very good for AP and HMTD).

[ALENGOSVIG1]

This isnt a thread about finding sources for nitrates. All of the sources for nitrates you guys posted have already been mentioned on the forum countless times. Keep it on topic!

[vir sapit qui pauca loquitur]

I was wondering...

Would anyone consider it a terrible risk if some homemade NG (well washed and well made) was absorbed with diatonatious earth (i believe that its used in proffesional grade dynamite) and i was to store it for a short time ? I'm thinking of about 2 1/4 sticks

anyone think that i'm crazy ?

I wont be able to make it closer to the time of usage (in my dreams you understand <img border="0" title="" alt="[Wink]" src="wink.gif" /> ) but from what i've read it seems to be very stable (compared to what i imagined it to be!)

[ALENGOSVIG1]

That would be fine. Ive made mutli pound batches of pure NG and ive stored a few pounds homemade dynamite for a week or so.

But i wouldnt use diatonatious earth, But rather ammonium nitrate, some flour, and a pinch of sodium biarbonae.

Nitro isnt as unstale and unpredictable as most people think. Its alot less sensitive that AP, plus pure nitro can be diluted with acetone to make it completetely safe to store.

[vir sapit qui pauca loquitur]

From everything that I have been told in every chemistry class, I imagined that it was taking your life into your hands making even a few grams of NG! But today I learned that this forum is better then any teacher could hope to be (i've made up a whole stick with DE and one with AN) and both are stored in a dry and well reinforced area (it happens to be a good area, i didnt build it to be)

it's great to learn something new each day. :p

[ALENGOSVIG1]

Yeah well i remeber being told that a hydrochloric acid (15%) will burn your hand off if you get some spilled on you. I also remember being told that a small lunch bag full of oxygen/acetylene will shatter a metal lab table. Teachers always exaggerate when doing something even remotely dangerous.

Have fun with your dynamite. Awhile ago i detonated 3 lbs of 60% equiv. ammonia dynamite 3 ft underground. It made a 5ft wide, 4 - 4.5 ft deep crater! Its fun stuff and its quite cheap to make.

Make sure you keep your dynamite dry though. Its good to add .5 - 1% soy oil to your AN before you mix it with the other components to keep it from absorbing moisture. I read it in federoff i believe.

<small>[ October 05, 2002, 05:00 PM: Message edited by: ALENGOSVIG1 ]</small>

[EP]

</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> But i wouldnt use diatonatious earth, But rather ammonium nitrate, some flour, and a pinch of sodium biarbonae.
</font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">What is the purpose of the flour? Shouldn't the AN do a good enough job of absorbing the NG?

3lbs?! <img border="0" title="" alt="[Eek!]" src="eek.gif" /> Must have been fun! From your pictures I'm assuming you always use good HNO3 to get that much, the yeilds are very low using AN right?

[ALENGOSVIG1]

The flour is just fuel. You can use anything that burns really. Powdered corn flakes, coal, etc.

And no i dont use nitrate/sulphuric to make NG when i can just use HNO3. The yeilds arent that bad when using nitrate but the yeilds are great when using HNO3.

[BrAiNFeVeR]

And so what IF yields are a little lower, all the precursors are dirt cheap (to me at least)

If you use the x-nitrate + H2SO4 method to make this, better use a nitrate that gives a soluble sulphate, otherwise, the mix gets very clumpy, and hotspots can really get an issue !!
With KNO3 for example, you get K2SO4 cristalising out while the KNO3 is still dissolving (especially with low T)
NH4NO3 doesn't has this problem, and the reaction stays nice and liquid :)

If you want to see another pictorial (though not as good as Alen's),
go ahead and click the link in my sig ...

[carbonated]

Does sodium nitrate (NaNO3) have this problem brought to my attention by brainfever?

[vonK]

Indeed it does, much worse than KNO3 (in my experience).
I have a question about the yeilds of nitroglycerine.
I use 200ml 98% H2SO4, 100ml 70% HNO3 and 50ml pure glycerin. I keep the reaction between 10C and 15C the whole time and basically follow the Alen's pictorial instructions to a "T".
The first time I did this reaction, about 6 months ago, I got 50ml of nitroglycerine, no problem. Lately, however, I have been getting yeilds of only 40ml, I've made 4 batches in the last 3 weeks like this.
I do leave my HNO3 on the floor of my bedroom, it's not really in direct sunlight and there is no redness to it but I wonder if it has decayed a little and this is the problem (it's been there since last Christmas).
I would love to know what kind of yeilds other people get and if I should find a real storage place for my HNO3.
Thanks for any help.

Kurt

[da man]

Vonk, i use the exact same procedure to make my nitro, and i also get pretty poor results, about 60g, from 50ml of glycerine, which is about 40ml. I don't think it has anything to do with your nitric, unless its gone red.
I think you just can't help getting poor yields with so much water in the reaction.

I though i should mention this really great plastic explosive that someone posted in the PETN thread a long time ago. I've tried it, and it works REALLY well! Its easy to make, has good plastic consistency, and is made of 100% energetic materials.
All you do is make blasting gelatin by mixing 46g of Nitroglycerine, with 4g of cellulose nitrate. You may need to heat it gently to get them to gellitanise. At this point i add a bit of acetone to make it easier to mix. Then add 50g of PETN bit-at-a-time, and stir it around real well. Then just dry off the acetone, and you have a very powerful, good plastique.

[Trinitrotoluene]

I am wondering about my idea of the 50/50 nitroglycerin and TNT mixture. To get them to get togeather dissolve them both in acetone and pout the mixtures togeather then let the scetone evaporate.It should be stronger then stright NG.But im uncertain about the stability.Any thoughts?

[kingspaz]

why would it be stronger than straight NG? TNT has a lower VoD than NG so if anything it will be less strong. the oxygen balance will be improved however.

[Argy]

Hum, i have a problem, i tryed to make NG with ammonium nitrate, i disolved it in the sulfuric acid i added the glycerin blablabla... but when i add water the ammonium nitrate precipitate and it's realy boring because the NG stay on the filter, i think my ammonium nitrate isn't enough pure... so i have a question, is it possible to make NG with 58% nitric acid and, if yes, witch proportions should i use?

[0EZ0]

Argy, If you want to use the Nitric acid route I would suggest that you need to distill your acid.

If there is too much water in your acid, then you will end up with dinitroglycerine instead of the usual trinitroglycerine. Another member may be able to explain it better to you hopefully.

[Argy]

Bahhh distilation is realy boring, i have only a 500ml ballon :p but i'll probably do it... :( damn i only want nitro to make detonator (with some cellulose) because i don't like AP. I made lead azide but it's realy BORING to get it dry and if it isn't it's hard to detonate :/

[Mr Cool]

Argy: it is generally boring to distil things, but it is an essential lab skill. Drying lead azide isn't boring, just leave it overnight in a warm place and it'll be dry when you get up in the morning.

[Argy]

Hum? what did u said?!? drying LA is close to be impossible for me :/ i made my LA 1-2week ago and it isn't dry, it's a paste (with the dextrin) and it's realy hard to detonate it in this conditions, i asked for the 58% nitric because it work with PETN (thanks BLASTER :D ) so i thought that could have gone with the NG.

EDIT : maybe should i put my LA in my furnace ? (60° C) i did it with my PETN but i don't know if the LA is stable enough for it.

[Mr Cool]

You could store LA at that temperature for months without any problems.

[Argy]

ok then i will try to dry it in the furnrace =) thx

[dave]

Hello, everyone I would just like to post about my first NG attempt with some problems. I went the sulfuric acid and NH4NO3 route.
First I boiled down my black H2SO4 down to higher concentration and with the hope of the black additive disappering, this didn't happend but I went ahead to proceed with my attempt. First I let my acid cool down until the jar of warn acid could be held with a little discomfort due to heat. I then added 40 grams of dry NH4NO3 to 60mL of acid and this released alot of white fumes which I think is nitric acid because it burns when inhaled. The temperature raised alot but I let it cool down to room temperature and nitric acid fumes were still coming out. I put the jar in an ice bath but fumes were still coming out of the jar so I then had to do the synthesis in the garage.
Now this is the part of the synthesis I thought was a little weird. I added 10mL of glycerine with little rise in temperature. Reading from other peoples' results I got the impression that the temp must be watched carefully. I added 10mL of glycerine with a pipet in about 4 minutes and the temp went from 8*C to 10*C in that time. I let the jar sit in the ice bath for 5 minutes. Next I looked In the bottom of the jar, I could barely make out the glycerine settled at the bottom of the jar. I assumed this to be my NG. I then went to decant the mixture careful not to pour the product out. I looked again and I was sure the NG was still at the bottom. Ok here is something weird, I walked with the jar to my garage and the NG was gone:confused: . I thought it was really perculiar since NG was not soluble in water. I decided to let the jar sit for 15 minuted to see what would happen. I came back into the garage later and it looked like water with some solid crap from disolving the NH4NO3 in the acid that was in there during the whole synthesis. The only problem I could think of is that maybe the glycerine was not pure. But I think it was since it was pretty thick. Could someone please help me out? Any would be appreciated. I am trying to move away from APAN as my main explosive to a more stable one. TNP seems to be something I will be cooking up soon. Sorry for boring anyone with my long post.

[rooster]

I walked with the jar to my garage and the NG was gone . I thought it was really perculiar since NG was not soluble in water.

First of all: If the NG is dissolving, remember that it is not dissolving in WATER. It is a mixture of nitric acid/ammonium nitrate and sulfuric acid. However it should settle out of the solution. Maybe you made dinitroglycerine? Anyone knows if its more soluble in the acid mixture than its trinitro brother?

Is it right to assume that it would be more soluble than NG, but less than glycerine? Since it is lying between them?

[Arthis]

Don't you think the concentration of nitric acid was too low, considering a great part of it was "distilled"/evaporated ? This would prevent a total nitration thus obtaining dinitroglycerine.

Did you try to recover your product from water with another solvent ?

[Mr Cool]

OK, I haven't checked ratios, but that seems like too much glycerol to me. It might not be, but if it is then it's possible that it was only nitrated to the di- or even mononitrate, which would make it much more soluble. Also as has been said, it sounds like a lot of your nitric acid evapourated. You must cool the sulphuric acid to room temperature or slightly below before you add the AN. Also make sure that the AN used has been dried totally.
Did you stir the reaction? You didn't mention it. You [b]must[/b stir it to allow the reaction to proceed faster. Otherwise your glycerol will just sit there, without dissolving, and the reaction can only happen at the interface between the two liquids.
That temperaure rise is smaller than I would have thought from a reaction of that size, but it depends how you did it. When I make EGDN (or NG) I do it in a high-volume beaker, so that the reaction is in a thin layer on the bottom, which makes cooling much more effective. I mix it buy swirling it around rather than with the thermometer, since with the reaction in a thin layer, it is hard to stir it without continuously bumping the bottom of the beaker. I generally swirl it two or three times, then check its temperature, then add more alcohol if necessary, swirl again, etc.

[dave]

I did everything you mentioned Mr. Cool, I will try again but adding the nitrate when the sulphuric is slightly below room temperature. The evaporating nitric was really annoying because I kept inhaling it when I was doing the synthesis. Let's see, I did stir it around at a good speed like when Im doing AP with 93% sulphuric acid to keep the temp down. When I first started the synthesis I thought the temp would rise like AP synthesis would with strong acid. I did try to swirl the beaker around but the glycerine from the thin top layer got on to the sides of the jar so I then had to push it back down into the mixture. I stopped swirling at this point. The ratio I used was 60ml of boiled acid, 40 grams of NH4NO3, 10mL of glycerine. I got this off of http://www.geocities.com/brainfevert/index7.html.

[kingspaz]

'The evaporating nitric was really annoying because I kept inhaling it when I was doing the synthesis'

the answer to this is do it outside and work upwind or go down the army surplus shop and buy yourself a £20 gasmask and a spare filter.

i recomend the gasmask. it will filter out all the nasty shit you're likely to encounter AND protect you somewhat if the world decends overnight into an inferno of chemical/biological and nuclear war.

[vonK]

I might be wrong but shouldn't nitroglycerine float on top of the acids as it is less dense.
I thought nitroglycerine was about 1.5g/ml, 98%H2SO4 was 1.85g/ml and my 70%HNO3 is 1.42g/ml
I make my nitroglycerine using mixed acids and the glycerine\nitroglycerine always floats in a layer on top once it has been left to settle. If you have a layer on the bottom then I would say your acid is not concentrated enough.
Before I sourced my HNO3 I tried to make nitroglycerine using 98%H2SO4 and KNO3. It never worked, I always got a beaker full of solid crap (K2SO4 I believe).
I think if your glycerine wasn't pure then there would have been a larger rise in temperature as you added it to the acid Like adding water to H2SO4, the temp rises a lot.
If you try again, when you try again, I would recomend that you cool your H2SO4 right down before adding the NH4NO3. This should reduce the amount of HNO3 lost as fumes.

[rooster]

NG has a density of 1,6. It is probably too low conc. of the acids then.

[Argy]

Hum, following my test with ammonium nitrate + H2SO4 i get somes ml of what i supposed being nitroglycerin, but when i tryed to burn it, it burned REALY slowly, i think it's a good thing for the fuses lol so it's not nitroglycerin, i think it's only mononitroglycerin.

Ammonium nitrate + H2SO4 is definitively a bad method.

[ALENGOSVIG1]

Ammonium nitrate + H2SO4 is definitively a bad method.

It seems to me its only newbies that are having trouble with this method. If it didn't work the first time, try it again. Why don't you heat your H2SO4 to drive off water right before making the NG. Same goes for the glycerine and nitrate. All three of the reactants are hygroscopic! Or why not adjust the ratios?

[nbk2000]

This guy's been here all of two months (at most) and has the gall to say that a process that's been photo-documented, and that dozens of people have used successfully, is "definitively a bad method".

:rolleyes:

When they're ignorant, they're still "All Knowing", until they learn enough to know that they don't know shit-all. ;)

Argy, follow the procedure EXACTLY as detailed, and read the whole thread before coming here and saying "I dont' know squat, and can't follow simple instructions, but I know this doesn't work because I couldn't do it!".

You'll get along much better that way. :)

Oh...wait...I forgot...he won't be able to see this for a week because he's restricted to the watercooler for making too many lame posts for the week. :p

[blindreeper]

Indeed some newbies do have difficulty performing various synthesis, but even now I am still trying to master distillation. But back to the nitro, I was thinking about making it, I have the H2SO4 (batteries) and 13-00-46 fertilizer (I think thats the purest you can get?) and my glycerine is thick, a bit thicker than boiled down H2SO4, it kinda behaves like oil. The only thing that is stopping me is that there is a hype that seems to have evoled about sensativity, like AP. I found AP to be insensative and never had anything go wrong. But NG is a new dimension. So for those of you who have accually made it can you give me some ideas on storage and such?

[rooster]

Some places tell you to add 25% acetone, and some tell you 75%. At least thats my experience. This will improve stability, and you just evapourate the acetone (for example on a hot water bath), and use it. Of course you can also use it with the acetone, it will be a good fuel for for example AN/acetone.

If it turns yellow during storage, you still have traces of acid in your NG. You should dispose it,
or neutralize it with bicarb solution.

[Mr Cool]

If you know how to handle AP, then you know how to handle NG. The only difference is that NG can be stored for as long as you want, for several years if you like. If you don't want to store it pure, dilute it with an equal volume of acetone. The NG can then be recovered by dumping the acetone solution into a load of water, and stirring well. The NG will sink to the bottom, where it can be sucked up with a pipette.
I store mine as a roughly 50% v/v solution in acetone, with some anhydrous urea in the bottom. This should help get rid of any NOx that might slowly develop over time, although with good washing your product will be as pure as commercial stuff, and thus will not evolve NOx. But it's a precaution that can't do any harm, so do it. I keep the solution in a brown glass bottle in a dark corner of my lab, you could keep it in a bottle in a cupboard. Keeping it in the dark is a good idea though, as with all explosives.
Just make sure you wash it well and you will have no problems. Suck the product out of the acid, and wash it a few times with distilled water. Then a few times with 5% NaHCO3 solution. Then a few more times with distilled water. Each time, you want to stir it well, so that the globs of NG break down into very very fine little droplets, for more efficient removal of acidity. If you get an emulsion, you will find that it does settle out eventually. If not, adding a load of salt to the mixture (enough to form a near saturated solution in the water) will help to drop out the NG droplets.

[blindreeper]

Thanks for that Mr Cool. I suppose there is not much risk of it detonating if wash properly and stored with urea as it isn't primary. I am getting nerves cause i have over 100ml of MEKP (Anhydrous) in the cupboard. I think I'll have to make some AP and get rid of it all at once. Is glass fine for storing NG in?

[Mr Cool]

No problems.
I don't think it would just detonate all by itself even if it was unwashed. It would just gradually get more and more red, and less and less stable. I think it would still need something to set it off, although that something might not need to be much if it's really full of NOx. I don't know how much sensitivity increases with acidity/NOx, I've never wanted to find out for myself!
Glass is perfect for storing NG.

[Iñaki]

just a question nbk2000 (or anyone who knows) how do you calculate the psi overpressure (regarding distance and mass of explosive)? it´s just for knowledgement, thanks :)

[Sonny Jim]

Originally posted by Mr Cool
If you know how to handle AP, then you know how to handle NG.

Actually I don't find NG that sensetive. The other day I put a drop on a coin, placed another coin on top, and beat the hell out of it with a hammer. I hit it so hard the paving stone it was standing on broke. No detonation. I agree that it is wise to handle NG with great care still, but I think the horror stories about NG sensetivity are

1) possibly due to acidic NG

2) the product of a 14 year old boy trying to make a dramatic website to impress all his friends.

[vulture]

and 13-00-46 fertilizer (I think thats the purest you can get?)

You have to purify your fertilizer first, unless it turns into a very wet bag when stored for a few days. Ammoniumnitrate fertilizer is coated with insoluble CaCO3 to keep it from absorbing water and to achieve slow and controlled release to the environment.

You DON'T want CaCO3 in your nitrating mixture because it will neutralize all your acids!

[Anthony]

I'd bet that the raised image on the coins gave the NG a partial refuge from pressure. Smooth metal discs might be different, but then you still have the same problem of the NG being scattered without being detonated that usually requires it to be soaked into paper for the hammer demo.

[Sonny Jim]

Ah. Next time I try something like that, I don't think I'll use any two small metal objects. I'm becoming more wary as time goes on and I'd really hate to get hit by a speeding coin :eek:

I reckon next time I do something like that, i'll place it on one of my 20KG weight disks. It would take some force to blast one of them at me, plus the surface of them is flat.

BTW, I should also mention that I don't think the NG I tested that way was up to scratch, due to my failure to extract all the water out of it properly :rolleyes: , so I'm going to do the test again to obtain some more reliable results.

[Trinitrotoluene]

I dreamed about making nitroglycering, using brainfever's method I used 60ml 98% H2SO4, 40grams of powdered NH4NO3, then 10 ml of glycerin. Everything went well and got a 8ml yield. I then extracted the crude nitroglycerin with a pipet and transfered it to another beaker with sodium bicarbonate and NaCl soloution, there was a little bit of nitroglycering as well as little bit of impurties leftover in that beaker. The stuff was poured out. Some nitro and impurties was stuck to the wall of the beaker, I cleaned it off with denatured alcohol and my bare hands. 15 minutes later I feel a head-ache. It lasted for 6 hours, after 5 hours it got really intense I felt like crying to my mom, but didin't, so I went to sleep and the next morning I was ok.
My advice if you can't take the nitro head-aches wear full protection. Therefore minimizing the exposure.

[blindreeper]

I think ALENGOSVIG1 recomends taking an aspirin and a strong coffee to fix those damn head aces - really thats the only reason why I don't want to attempt to synthesis NG. Does any one know if there are any long term effects of NG exposure, I guess they can't be serious as they use it in medicine. (sorry about the spelling mistakes I am having a brain fart)

[vulture]

Long term effects of NG would be wear on your heart and blood vessels because they are really being stressed when they expand so much. Furthermore, organic nitrates will be degraded to carcinogenic nitrites and possibly nitrosamines in the body.

[Trinitrotoluene]

I don't think aspirin is a good idea, aspirin thins blood, so expanded blood vessels plus thinned blood I think a deep drop in your blood pressure, and I don't think the outcome is good. Coffee speeds up your system, I think if you blood vessels are expanded already that will put extra stress on them. Not good for the longterm effects on your bloodvessels.

[knowledgehungry]

Use tylenol instead, or advil.

[BrAiNFeVeR]

Wedging this tread back on topic here:

I made a new NG pictorial (I found the pics somewhere :) lucky me) , this time using 65% HNO3 method instead of the xNO3 method that is normally used by SWIM.

Click here to view NG pictorial (http://www.geocities.com/brainfevert/NGsynth.html)

While the actual product is still containing water, you can allready tell that the yield is not what it should be.
Or at least not what some claim to get when using the HNO3 + H2SO4 method.

I was expecting higher yield then with the NH4NO3 method ...

[Arthis]

I just tried today to make NG with 58% NA and 92+ % H2SO4 :) Well, it seems to have worked, but though it's not finished yet (need to dry it), I guess I will get <1ml NG, and I used 4 mL glycerol.

I confirm Brainfever's results, the more water in the less NG you get.
It's always fun to try. But it's even funnier to use conc. acids. Next time..

[Trinitrotoluene]

I too had a dream today of prepearing nitroglycerin using the HNO3/H2SO4 method. 50ml 98% H2SO4 added to a beaker, then 35ml of 90%+ HNO3 added to the H2SO4, the temperatured was cooled in the freezer to 7*C. Then 11ml of glycerol was slowly added, it took 20 minutes. It was dumped in 500ml of cold water, the nitroglycerin extracted with a pipet. It was neutralized with sodium bicarbonate,yield 18ml, then it was placed in a sealed can in a small beaker containnig the nitro. After being dehydrated it was mixed with an equal amount of acetone, 50/50 ratio, and stored in a test tube with stopper.

[frogfot]

Here it goes.. All preparation methods for NG on the net uses an ice-bath to cool reaction mix, but in literature it say that too low temperatures are not good for some nitrations since reactants can accumulate resulting in fast increase of heat.
Then I found a page (http://mihailru.freeservers.com soz it's in Russian, UTF-8 encoding), they used a 10-15*C water-bath with continiously flowing tap water to prepare 16-20 ml NG. Since page is decently written I thoat to write this.
Preparation from Stettbacher was also mentioned where he used 12*C water-bath to prepare 269ml NG. So, this doesn't have to be applyed only to small batches..
Now, this continiously flowing water-bath is simple to set up (it could be simply a deep plate under a tap). Since you people are familiar with how much heat will evolve in reaction, will it be ok to use water-bath? or, will this require unresonably slow addition of glycerine?

[ALENGOSVIG1]

The method of cooling doesn't matter. As long as you can keep it below 20 degrees you'll be fine. Why not just use the icebath and add the glycerine quickly?

[frogfot]

Hmm, you're right, and then again one can simply take out baker from ice-bath to prevent overcooling...
Another thing bugs me, i've compared different synthesises by checking how much mol HNO3 everybody uses to one mole glycerine. Below i'll give the ammounts

>Stettbacher:
156 ml 86,5% glycerine
1300 ml 100% H2SO4
750 ml 62% HNO3

Thats 5,7mol HNO3/1mol glycerine

and
159 ml 100% glycerine
544 ml 100% H2SO4
333 ml 100% HNO3

3,65 mol HNO3/1mol glycerine

>From abovenamed dude:
20 ml 100% glycerine
150 ml 100% H2SO4
70 g NH4NO3

3,2 mol HNO3/1 mol glycerine

>Mega:
112 ml glycerine
300 ml 98-100% H2SO4
200 ml 98-100% HNO3

3,1 mol/1 mol glycerine

Does this difference depends simply on water content of reactants?
When using lots of nitric as Stettbacher will this yield only tri nitro isomer? I'm just concerned that if i use theoretical ammount (3 mol HNO3/1 mol glycerine) wouldn't this form lots of unwanted mono and di nitro glycerines?

Sorry about questions. Btw, i made small batch of NG, about 1h went and still no headache.. I want my headache! :(

[knowledgehungry]

Rub some NG on your fingers, you will get one soon enough.

[kingspaz]

'When using lots of nitric as Stettbacher will this yield only tri nitro isomer? I'm just concerned that if i use theoretical ammount (3 mol HNO3/1 mol glycerine) wouldn't this form lots of unwanted mono and di nitro glycerines?'

you are right. so just add a bit more HNO3 so you'll have an excess. the differences in HNO3 content are probably due to the reactions being calculated and each person using what they would think to be a suitable excess. also isomer = same chemical formula but different arrangement of atoms. so dinitro glycerine is NOT an isomer of trinitro glycerine, they are distinctly different chemicals.

[frogfot]

Oh, thanx for correction (i always used to say isomer when having in mind closely related structural forms..)

Finished second batch using ammounts from my above post (with 62% HNO3). Though I changed it a bit, used 10ml 96% H2SO4/5ml 70% HNO3/1,2ml 86,5% glyc. Ammount of glycerine in first batch was dubbled (2,8ml). Total reaction times was approx. same (45min). The final product was colorless liquid.

Both samples was tested with hammer on an iron anvil. The second one recuired noticeably less shock than first, this may be indication on that first one was not fully nitrated.

To my surprise pure NG was extreamely unsencitive, it required a really hard blow to go off much stronger than for MEKP. (They defineately exagurated sencitivity of NG in MacGyver, but thats another story :rolleyes: )

[Imperial]

I have never actually bothered freezing any nitro I have made, nor has any which I made during producing it frozen (I have always tried to keep the temperature cold but reasonable (5ºC-10ºC), and I added just a little more glycerin to speed the process up whenever I detected a hint of dropping below 5ºC).

I find that nitro is best used/incorporated into other explosives straight after it has been made. That way, there will be no freezing, as well as no premature detonation. Keeping nitro cool is important though since it has been known to detonate at about 30ºC.

As for stirring, I find that adding glycerin in drops with an eyedropper or pipette, and using a glass stirring rod to gently stir the mixture is the best. I have never made an amount which is even close to 100mL, but I have used the same proportions as you (50mL nitric acid, 100mL H2SO4 sulfuric acid, 25mL glycerin, with the nitric and sulfuric acid being 90% and 95% pure respectively) and I have not had any problems, but I only got about 35mL each time.
I have used more pure acids (98% I have tried) but those only increase the final volume by about 5mL.
Are there any other factors which may contribute to my relatively low yield? The acids, etc. I am using are always reasonably new and I use the standard procedure (not the KNO3 method) for synthesising the nitro.

[ALENGOSVIG1]

Perhaps impure glycerin is your problem. Have you tried heating your glycerine to drive off any water?

I find that nitro is best used/incorporated into other explosives straight after it has been made

Umm no. Nitro can be safely stored for years. I believe the first sample was stored in the lab for 10 years. I have personally stored nitro for 1 year without any signs of decomposition.

it has been known to detonate at about 30ºC.

NG doesn't even begin to decompose until 50 or 60 degrees celcius. Infact, its recommended in some publications to use warm water to neutralize the NG as warm NG is less viscous and therefore is easier exposed to the wash solution. And i wouldnt say gentle stirring with a glass rod is the best method of mixing when making NG. Gentle stirring doesn't allow you to safely stir as vigorously as you should be. Unless your a pro with the stirring rod like me ofcourse. :)

I find swirling in a rb flask is best. That way you can just swirl the hell out of it and theres no chance of any acids splashing out of the flask.

[Mr Cool]

I'm a fan of swirling instead of stirring with glass rods. Using a thin layer of reaction in a big flask not only helps with the swirling, but it helps keep the cooling efficient.

Sorry, no idea why you might have a bad yield, except for the glycerine, like ALEN said. It's quite hygroscopic, so maybe it has water in it..?

[DNA]

I was wondering....
I made NG twice now...both fuck ups...
I'll tell you guys what I did....

Concentrate my 37,5% H2SO4 to 98% I heated it for 4 hours...until I measured it should be around 95%+ and then after 10min or so white fumes appeared so I was sure I had highly concentrated sulfuric acid....
Then I added 99,999% pure NH4NO3 bought from the pharmacy....
60ml H2SO4 and 40 gr NH4NO3, then ofcourse added the glycerine (85% can't get higher %... :( )
Well anyway I made an icebath and all and well added 10ml glycerine in about 40 minutes....
The nitrating bath with glycerine was brown when all the glycerine was added before any glycerine was in there it was kinda yellow....well I stirred well after every addition of glycerine...
all the glycerine in there stirred for about 1-2 minutes...and then poured it in the double volume of cold water....and well some NG stuck to the bottom of the glass I made it in...so I added some water to it and swirreled and it disapeared for a bit...poured that in the big volume of water...and no NG was left everything dissolved...the liquid was yellowish....and no NG at the bottom....I wanted to decant but there wasn't any NG this happend twice to me! :mad: I didn't use any distilled water though but I doubt that has effect on the NG that it will dissolve completely!
Now for the second time I put the liquid in the fridge...and well I think 0,25 ml white stuff is on the bottom but it is sooooooooooooooo little NG (if it is NG it isn't normal)

WHAT WENT WRONG??????

thnx in advance DNA...

[knowledgehungry]

You poured the misture int water too quickly, you need to wait a little bit for the NG to form, most organic reactions will not occur in 1-2 minutes, next time let the AN, sulfuric and glycerine sit together for maybe 30 minutes before pouring into the cold water.

[ALENGOSVIG1]

Using 85% glycerin will give you shitty yeilds. Heat it for and hour at 100 celcius or so. It doesnt really matter how hot just hot enough to heat off the water but not hot enough to decompose the glycerin. I think i've said this a couple times in the thread already! I feel like a fucking parrot.

I'd heat the H2SO4 for a little longer too. I usually heat it for about 20 mins after fumes START to appear. It's fuming like all hell after 20 minutes though. Wouldnt want to breathe in those fumes. :)

You, should be stirring throughout the entire process to avoid hotspots from forming. And you should stir for an additional 5 minutes after all of the glycerin has been added. After that, let the nitration mixture warm up to room temperature by removing the flask from the ice bath an let it sit for 10 or 15 mins THEN dump it into water.

It should also be noted that after dumping it into water you should give it atleast 15 or 20 mins for all the NG to seperate out.

Grrrr this thread is just the same shit over and over. Just heat all of your reactants prior to the nitration and you should not have a problem. They're all hygroscopic! Especially NH4NO3 and glycerin, but H2SO4 it also hygroscopic.

I only achive great yeailds when making NG if i use freshly distilled HNO3, and when i heat my glycerine and H2SO4 prior to the nitration. Especially the glycerine. Those cheap ass bottles from the grocery store are not airtight damnit.

[DNA]

I just made NG again with 68% nitric acid...when I concentrated my nitric there were quite some white fumes....I suppose that was the water evaporating I let 14ml evaporate till it was 5ml, and well no red fumes but that was b/c I heated it very slowely...and my intention was to only evaporate the water....anyway everything went fine...mixed h2so4+hno3 96% and 68% and well added the glycerine...and it kept being clear...now it has stand for 30 min at room temp and still it is clear...gonna leave it for 60 minutes...and well I put it in cold water after 60 minutes...0*C destilled water...and I hope the NG will show up then....
Anyone knows why my nitrating bath is still clear? :(

[knowledgehungry]

No, however i dont think that is a problem really, you might as well dump it into the ice cold water now, and then wait another 10-20 minutes to decant. 60 minutes seems excessive and actually might start to decompose the NG giving you less product.

[DNA]

Well it is still clear...completely clearless...and well I'm trying it again after dinner....and then I let my acids longer on the heatplate...to get more conc. acids...maybe that works...and well maybe this is important....the nitric acid was fuming white the whole time even in the fridge on the hot plate on room temp....it kept fuming....
And it was fuming white quite a lot on the heatplate...is this normal...now I'll concentrate it until red fumes appear....

[frogfot]

DNA, maby I misunderstood you, but you can't concentrate nitric acid by boiling it!! You will only concentrate content of water in it..

[DNA]

If you heat nitric acid...you will evaporate the water out.... :confused: like with sulfuric acid....just gently heat it...not boiling it...very gently heating it...at 100*C so the water will evaporate...because water boiling point=100*C and sulfuric acid boiling point is higher than water so you will boil off the water...
And the same with nitric acid
Water B-point=100*C
nitric acid B-point=120 at 60%....

Nitric acid content 60 % 80 % 100 %
Melting point (°C) -22 - 39 -42
Boiling point (°C) 120 117 86
Density, 20 °C (kg/m3) 1.367 1.452 1.513

[frogfot]

I was wrong about water evaporating. But still, as was mentioned lots of times 68% nitric acid will form an aseotrope with water, meaning both acid and water will evaporate. (Theres a reason why one can destill <68% without dehydrating agents)

Anyway, just to be on topic I thoat to post different yields with different concentrations of acids: :)

200 ml of pure glycerine (dencity of 1,26 g/ml)
544 ml concentrated sulfuric acid
333 ml fuming nitric acid
The yield is 269 ml (430 g) which is 87,2% from theoretical.

191 g 86,5% glycerine (dencity of 1,228 g/ml)
1300 concentrated sulfuric acid
750 ml 62% nitric acid (dencity of 1,38 g/ml)
The yield is 288 g which is 61,1% from theoretical.

20 ml pure glycerine
150 ml concentrated H2SO4
70 g dry NH4NO3
This will give a poor yield, not more than 52%

[DNA]

I tried NG again....another failure...4th time...
Now I'm conc. sulfuric and I'll vacuum distill it and add 16 gr NH4NO3 ....now I dried it in the oven for 4 hours at 105*C....

And then when I've got 5 ml conc. HNO3 I'll add that to 10 ml H2SO4 conc. 98% and try NG AGAIN 5th time....this should really work....

With the nitrating salt I used...well there was to much water in it....it did got cloudy but when in water (after 30 min at roomtemp) there was no NG at the bottom even after 45 min in 0*C old destilled water....

So now I'll try HNO3+H2SO4 again....
Because when I conc. HNO3 on the hot plate normally it won't give of red fumes and I can heat it so long that all the HNO3 is gone...it just evaporates completely....so that's why I'm gonna make HNO3 the way with H2SO4+NH4NO3 distilling....

[Microtek]

NG is one of the most simple explosives to make. When it doesn't work for you it must be due to some fundamental error in your procedure, so I suggest that you go over each of your reactants to make sure that they are what you think they are. For instance, establish your exact concentrations by some objective means, not just assuming that sulfuric acid must be 98% because you heated it until fumes appeared. I experimented a bit with concentrating H2SO4 by boiling and can tell you that if you heat aqueous sulfuric acid until a temperature of 175 C is reached ( atmospheric pressure ), concentration will be at least 90 % ( established by multiple titrations ) . It starts fuming very early, but that is just water vapour.
Glycerine can be concentrated by heating to 185 C in a similar manner. Note that the boiling point raises as the sample becomes more concentrated, so it will not be possible to have, for example, a sample of sulfuric acid at atmospheric pressure and 175 C that is less than 90 % concentrated.
It is unclear how you prepare your nitric acid. Do you heat commercial 60-70 % HNO3 alone or do you distil it using H2SO4 to break the azeotropic behaviour.

All in all, something that you are taking for granted is going wrong, or your procedure would work.

[DNA]

everything is going good for now....(like before) now it is sitting at roomtemp and I'm constantely stirring...now someone else is stirring for me :D I weighed it and looked at the volume and all and I calculated that I'm using 96% now....NH4NO3 has been in the oven for 6 hours...and glycerine...well it isn't necasary to conc. it but still I conc. it a bit...to get a bit better yields....will buy draincleaner soon....97% and well than it will be much easier....
Although I've got concentrated sulfuric now as well....and I conc. my nitric acid...(38%) just pour the liquid in beaker and heat it....
How should I do it to get it to 68%....(the azeotrope of nitric acid) mix it with conc. sulfuric acid?
and then heat it?

[Microtek]

When you heat 38 % HNO3, both water and nitric acid will evaporate. At first, mostly water will be removed, but as the concentration slowly rises, more and more nitric acid is evaporating with it until the concentration finally reaches ca 68 % when equal amounts of HNO3 and water evaporates. Therefore, once you reach this concentration ( after having lost much of the HNO3 to evaporation ), you cannot concentrate it any further by heating like this.
What to do instead is to mix ca 50 mL HNO3 60% with 50 mL H2SO4 96 % and distil the HNO3 off. The sulfuric acid traps the water which then won't evaporate along with the HNO3.
If you use less concentrated HNO3, more H2SO4 will be needed.
Having said this, note that you don't need HNO3 of more than 60-70 % concentration when making NG, as H2SO4 of high conc is used to trap water as in the HNO3 distillation.

I still suggest that you perform a titration of your HNO3 in order to establish a reasonably accurate concentration. You need a titrant of known concentration which can be made by dissolving a known amount of NaHCO3 ( sodium bicarbonate, used in the kitchen ) in water and see how much you need to add before it ceases to react with a known amount of acid.

[DNA]

I'll just buy the draincleaner....it's 97% sulfurica acid...and then mix that with a nitrating salt....
Doesn't matter if it gives bad yields I've got plenty sulfuric then 1 liter 97% for 4 eurp, and ammonium nitrate 4kg for 5 euro and I purify that....and glycerine 100ml for 2 euro....so :)

[spring]

Hello all. I decided to post this in here, so I would't make a new thread. I have attempted to make Nitroglycerin for my first time, and everything was perfect until I added 200mL of cold water to wash the NG. I decanted the water, and I ended up with this...solid blob of some material. Actually, there seems to be two of them floating around. Here are three pictures:

http://f1.pg.photos.yahoo.com/ph/stupidsiter/lst?.dir=/My+Photos&.src=ph&.order=&.view=t&.done=http%3a//f1.pg.photos.yahoo.com/

The first picture is of when I first added 200mL of water, the second picture is when I decanted the spent acids, and the third is a picture of when I added more water, and you can see the two blobs of a light brown material.

My measurements are as follows:

50mL H2SO4 ("Pure virgin sulfuric acid" drain cleaner :o )
35mL HNO3 (70%)
12mL Glycerin (99.5%)

Im sorry for going over the whole procedure as I know most of you heard this 100 times, but I chilled the HNO3 and the H2SO4 to approximately -2 degrees Celsius. I added the HNO3 to the H2SO4, and the temperature never climbed over 25 degrees Celsius during that addition. I let the acids cool to approximately 6 degrees Celsius, and I began to add the glycerin which was also chilled, in the refrigerator this time. I added the glycerin slowly, and the temp never rose over 13 degrees Celsius, and the glycerin addition was then complete. I waited 10 minutes while stirring the NG a few times while it was still in the icebath. At that time, the temp was varied from 5-9 degrees Celsius. I then poured the NG into 200mL of cold water. It was not distilled water...it was "Crystal Springs" water from the 5 gallon jug water dispensers (maybe irrelevant). At this point, it got warm quickly, and the temp climbed to around 25 degrees Celsius (picture one), and I put the beaker back into the ice bath to cool it down. I waited for about 10 minutes until the solution cooled to around 15 degrees Celsius, and I decanted the water (picture two) and I noticed some stuff that shouldn't be in there, as I thought. I added some more water, (picture three) and I really noticed the blobs this time. Does anyone know what this possibly could be? The (NG?) is at the bottom of the solution as in picture three, and it is a reddish-brown color, from my H2SO4, maybe. So, my NG (hopefully) is sitting in the NG/water solution until I can find out what is happening. I am sorry if I missed anything, and thanks for any help.

[Chemical_burn]

Hmm not a clue it may be impurities from the water.

On another note if i remember right 10min nitration time is a little long as your NG will start to decompose in your acids. I have noticed that other people have nitrated there NG for 10 or 15 mins have noticed very poor yields even when using cosintrated HNO3 and H2SO4.

OK thats my $.02

[nbk2000]

Looks like a blob of snot floating in your acid! :eek:

Whatever it is, it's not nitro, so flush that shit! And you've got some serious issues with impurities in your precursors because SOLIDS in your NG means something is seriously funky.

You didn't have anything in contact with rubber/plastic did you? Like using a rubber stopper while distilling your acid?

[spring]

Thanks, both of you for replying. NBK, the only thing I had come into contact with rubber is the syringe I used to add the glycerin. It was so viscous from chilling it, either a whole blob, or nothing would come out of the small beaker so I had to suck it up with a syringe and add the glycerin that way. I know nothing is wrong with my HNO3, but my drain cleaner (again, :o ) label reads: "Pure virgin sulfuric acid with 12 buffers". Im sorry I didn't add that before...I forgot. From my knowledge, a buffer is basically a substance that won't change the acidity when a base is added. This is interesting. I am angry that I did not make NG on my first time, but I am also sort of happy, because I kind of like solving issues with different chemical problems, but this one I can't figure out. Upon further inspection, the solid mass' look like dissolving nitrated cotton, which is also interesting. There are no blotches of NG laying at the bottom, just that ugly red/brown crap.

[nbk2000]

Sometimes syringes are lubricated with silicone oil. Did you use the syringe for anything else prior to the glycerin?

[spring]

Yes, I have used the syringe approximately five times before to add HCl to various substances. After the 10th time I use the syringe for HCl purposes, I discard it and open a new one. I still wash the syringe with soap and water after every use, though. Arrgh I am racking my brains out! Ok...I purchased 2.5 liters of the HNO3 in it's 70% concentration state, and I do not believe anything was added to the HNO3 to make this happen, not that I would know what could be added to make it do this.

I could always boil the sulfuric acid, but that would only increase the concentration, not have any effect on these "buffers", I believe. I have been thinking about the part when I added the acids/NG to the 200mL water and it raised the temperature that fast. In every instance that I read, it will do that, but if I did not put the beaker back into the icebath, the temperature of the solution would have raised to over 30 degrees Celsius. I am just trying to break down everything I did/used to try and understand what happened. Thanks again for trying to help me with this problem.

[nbk2000]

It might be one of the 12 buffers, which aren't listed, right? :(

Maybe you'll have to try a different brand of acid. See if that works.

[spring]

Yep, you got that right...none listed. I will try another brand of acid, and I will go from there. Thanks again! Now I can go to sleep :D .

[ShockWave]

I added the HNO3 to the H2SO4, and the temperature never climbed over 25 degrees Celsius during that addition.

I would add the H2SO4 to the HNO3, and keep the temp. below 10 degrees.
Maybe it has nothing to do with it, but it could not harm.

Good luck.

[vulture]

Unless you are using 100% HNO3, always add your H2SO4 to your HNO3. Why? Because HNO3 mostly contains up to 30% of water and adding water to sulfuric acid...

I still wash the syringe with soap and water after every use, though.

While soap is used for cleaning all over the world, it's not suitable for chemistry, because soap will always stick to glassware. Soap = contaminant and base when doing chemistry.

Rinse with distilled water, far superior.

[ShockWave]

Offtopic

I never use soap for chemistry but I always wash my glassware with soap, en wash it with water, is that a bad idea ? since you said that it sticks to glass ?

[blindreeper]

Havn't seen ShockWave for a while - it's a good thing :D
Anyway back to the glass. I soak my dirty glassware in NaOH over night then rise them with tap water (very clean in my part of oz). Next they go through the dishwasher and come out sparkling and with a final rinse of distilled water they are done.

[Microtek]

Even low concentrations of NaOH will slowly dissolve glassware, so you shouldn't use it to clean glassware that you use for precision measurements.

[blindreeper]

Well then I best not use NaOH any more. I have a plentiful supply of HCl so maybe a 10% solution would be better than NaOH? This is getting off topic sorry.

[0EZ0]

I remember having quite nasty experiences with NaOH and borosilicate glass. Some NaOH solution was heated in a 100ml beaker up to about 100C for close to an hour with occasional stirring. After that time the solution was left to cool and evapourate under an electric fan, I found that the beaker had become quite pitted with marks all through the point where the liquid had been in touch with the glass. The interesting thing was it seemed that the NaOH solution had significantly weakened the glass. It got to the point where using a glass stirring instrument to stir the solution hastened the pitting process considerably. It took very little stirring to cause severe frosting and pitting of the glass where the rod was in contact with the walls of the beaker.

As the experiment was apart of a school activity and the equipment wasn't mine, I didn't care too much for the reason of the pitting. Interesting to note that after one experiment, the new beaker had to be discarded.

I don't know if the same thing has happened to anyone else here. It may well be that it was just a manufacturing fault with that single beaker. Who knows...

Back on topic.

You really must be careful with the cleanliness of materials that are to come into contact with explosives sensitive to contaminants. Always make sure that you try to eliminate contaminants as much as possible when following any procedure. Where possible do as suggested and rinse glassware with distilled/purified water.

[ALENGOSVIG1]

I once did an experement where a beer bottle was filled with NaOH, and was heated for a couple hours over a fire. The next day, i went to pick up the bottle and the whole bottle just fell apart as i grabbed the neck of the bottle.

I dont really worry about etching my glassware with NaOH solutions though, because i rarely work with concentrated NaOH and i break my glassware before i severly damage it with chemicals.

Wow this is geting OT.

[DNA]

I made NG, with white fuming sulfuric acid, and NH4NO3 and I kept it between 10*C and 15*C,
Then after adding all the glycerine kept it for 40 min at 15*C-20*C and then decanted and decanted again and neutralized, and added salt solution after i sucked up the NG, but now it is very odd, my NG was yellow, and it got white and then well it crystalized on the sides of my beaker...

NG picture (http://www.fortunecity.com/millennium/river/25/4ce8e2b0.jpg)

and another picture

NG picture 2 (http://www.fortunecity.com/millennium/river/25/4c9a53c0.jpg)

[DNA]

Well since I can't edit my message, I make a new post my NG worked out well now, with the draincleaner and very good succes
Look here for the results of 2,5 ml NG
NG test 2,5ml (http://www.fortunecity.com/millennium/river/25/id97.htm)

[Sir Dudalot]

Those pictures are very nice. Makes the procedure much easier to follow. I dreamed about 9mL of nitroglycerin probably a month ago using Alengosvig1's proportions. I used 50mL 91% (didn't know it was 91 at the time, the bottle said concentrated and I recently recieved a scale and checked the density) H2SO4, 25mL 70% HNO3, and 13.5mL glycerin. It took 20-30 minutes to add all of the glycerine to the nitrating mixture. During the addition temperature was kept between 10-15*C. After that I let it rise to room temperature. Then I decanted and neutralized it completely. The next time I dreamed about it I used double those proportions and didn't let it rise to room temperature, instead I waited five minutes then decanted etc. This time the yield was about 22mL from 26 mL of glycerin. This yield is much better because less nitroglycerin dissolved back into the acids. I put the two yields together and converted them to "ammonia dynamite." NG/AN/corn starch 50/45/5. It made 66g of this mixture and I detonated it all with a 1.5g AP detonator. I was very pleased with the results. I only have one question really (maybe I should've just posted this instead of giving all the details first)...

Alengosvig1, on your site you say that you used 70% HNO3 but on the first post in this thread you say you used freshly distilled HNO3 (around 95%) so which one is a typo? I just want to know so that I can adjust my proportions accordingly.

[blindreeper]

His procedure on the site uses 70% but if you notice in the pics of the chemicals used it says "and freshly distilled nitric acid shown" He could have diluted it to 70% and was only using it for the picture? Or freshly distilled doesn't have to be 95%, you only get that if you first distill to around 70% (maximum of 68% but 70% is a nice round figure) and then further distill that with H2SO4. I think thats all right :confused:

I am not sure but I think there is a logical explaination for it :p

[chemoleo]

Hi,
I recently found an OTC source for diatomaceous earth, which happens to be a very good adsorbent for NG. In fact, the mixture was orignially called Gurdynamite (at least in German), and used commercially for a few decades (no more, of course). Although I found the mixing proportions for NG/DE on this site (75:25), noone commented on personal experiences with it. I heard it is safe to use, but apparently it sweats NG over a period of a few months, thus making prolonged storage unsafe. Anyone knows more? I.e. sensitivity to flame, to excessive heat (like thermite), shock (what initiators are required, amounts) etc etc? Also, what grade of DE is required, powder particle sizes vary apparently, from fine dust to grains. Any comments would be appreciated...
thx, chemoleo

[nbk2000]

Firstly, when mentioning an OTC source of something, it's customary to give some details so the rest of us can make use of it.

But I can already guess what your source is...pool filter aid...correct? ;)

The answers to all the rest of your questions are readily available if you...say it with me folks...USE THE FUCKING SEARCH ENGINE! :rolleyes:

Google is your friend, use it. :p

[Trinitrotoluene]

Today SWIM tried to detonate nitroglycerin, but it was a failed detonation 10ml of NG, containing a little bit of acetone was poured into some cottonballs, then loaded into a cardboard tubing 2.5" in length .75" diameter, 1/8" thick, one thing was different with the NG was abnormally thin, it's suposed to be viscus. A electrical christmaslight detonator was inserted in, which contained blackpowder as the igniter, and 1 gram of double salt. The charge buried 30cm deep. Then wires connected. A faint boom was heard, when it was dug up, the casing was found, and the soaked cotton.
One explination maybe still acetone dissolved?

[ALENGOSVIG1]

'Twas definately the acetone. NG isn't THAT sensitive as it is, and acetone greatly decreases it's sensitivity.

[Sir Dudalot]

My nitroglycerine surprised me with how well it flowed. I expected it to be a lot more viscous than it was. I was able to detonate it with a pen full of AP (about 1g). It wasn't greatly pressed, just hand pressed...but not even as hard as I could push because I don't want to tempt fate.

EDIT ON MY LAST POST (sorry, reread it again just now): I had one 6g charge detonated with a 1cm length of pen full of AP taped to the side of it and the other was 60g with the same size detonator inside the charge. I have a video of the 60g charge Here (http://www.angelfire.com/falcon/dudalot/videos.html)

[pdb]

Not only must you use NG without any solvent that would decrease it sensibility, but you must also use a strong detonator to ensure you get the high detonation regime (VOD 7,700m/s) iso the low one (2,000m/s). 1g AP is definitively not enough; you would need al least the double, well compressed to induce a sufficient shockwave, which I wound't try if I were you: too dangerous. Best would be to use PETN.

You can easily verify this by initiating two identical NG loads with respectively a 0.1g and a 1g AP initiator: you will get the same results on a lead witness plaque.

[Nevermore]

Originally posted by frogfot
Finished second batch using ammounts from my above post (with 62% HNO3). Though I changed it a bit, used 10ml 96% H2SO4/5ml 70% HNO3/1,2ml 86,5% glyc. Ammount of glycerine in first batch was dubbled (2,8ml). Total reaction times was approx. same (45min). The final product was colorless liquid.


I made a batch using my 55% HNO3, i used 20ml HNO3, 40 ml H2SO4 and 5 ml glycerine.
The nitration was performed in an ice bath, and the temp never exceeded 13C, it stayed around 10C most of the time. I let the mixture nitrate for 15 mins after finishing adding the glicerine and oily droplets started to form, then i dumped all in icy cold water and collected...less than 2ml of glycerine..I've never been able to get better yeld, the first trial was with 20ml HNO3 and 30 of H2SO4 but i got around one ml of NG.
I wonder what is the problem..
However my final product was a milky white liquid, it has been neutralized with sodium bicarbonate solution, then dried on a shallow dish, till it was a colorless oil. im still waiting till completely clear for trying to detonate it..

[0EZ0]

Too much water in your mixed acid. As has been pointed out previously, incomplete nitration of the glycerine is the result of low concentration reactants. I advise more reading/researching on your behalf before you attempt any other procedures. 55% HNO3 will just not do and you should have known that if you had taken the time to read through this thread and others on the same topic.

The milky white appearance is the water in the NG. There are various procedures posted on how to remove the water.

[Nevermore]

i already know that i've too much water in my acids, that's why i will switch to xNO3 method..
i just wrote my experience here, anyway, even using far excess sulfuric acid i don't get the hno3 enough concentrated to perform a decent nitration..
drying ng in a shallow dish works perfectly, at least, i am going to try the inexpensive xNO3 method and see what happens..

[Some Guy]

Living in such an isolated "faming community", I don't always have access to the necessary reactants. However, in this case, it might work to my advantage. I am able to get both pig and beef fat for free. In my great google search, I came across many how to make soap processes that explain how to render fat by boiling water and fat in a 50/50 ration until the fat has melted (around 4 hours) but they don't exactly explain how to extract glycerin. When the fat hardens in the fridge, will the glycerin have its own layer, or will it be mixed in with the tallow? Has anyone attempted this before? As a lover of KNO3 from urine, and ASA from willow bark, this method of obtaining gylcerin would be helpful. Also, a big thank you for starting the post. I was timid about NG at first, but now feel quite comfortable. Keep up the great work.

[Nevermore]

i don't think you can have two layers by freezing the fat, in fact glicerine has a rather high melting point, much higher than the fridge temp., the mixture is gonna be a white greasy mass, and you won't be able to separate anything..

[frogfot]

Glycerine from soap should be in a separate thread..
I did a little experiment on this using 30 g vegetable fat and got nothing, it seems like one should use at least 0,5 kg of fat to get decent yields.
In industry they precipitate soap by addition of NaCl, I've tested this, but this does not remove all soap. To get all glycerine out, filtered soap can then be redissolved in boiling water, reprecipitated and filtered again.
This requires some free time :)