Sciencemadness Discussion Board

nitroglycerin

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Vikascoder - 11-6-2012 at 03:41

I am storing 5 ml of nitro glycerin mixed with 1 gram of ammonium nitrate 3 grams of fuller earth lots of saw dust is this safe . It has been kept at 35 to 40'c from the last week . Is it safe

Hennig Brand - 13-6-2012 at 11:58

There is a lot of myth and legend surrounding nitroglycerin. There have been some terrible accidents during the manufacture and use of nitroglycerin, however, that being said nitroglycerin's sensitivity is most often hugely exaggerated. There are some circumstances where NG will be more sensitive, like at elevated temperatures or if the liquid has frozen NG in it or other gritty particles like sand. Some contaminants or decomposition products can apparently make NG more sensitive as well. Normally NG takes a fairly solid snap with a hammer to make it pop, which is much, much more insensitive than anything I was led to believe before I had any personal experience with it.

I am not suggesting that one should become careless or overconfident, but if the NG is absorbed in something it is very insensitive. Even if it was to go into rapid decomposition because of improper purification/acid neutralization, with the small quantity involved (5mL), any kind of explosive event would be very unlikely.

Why are you storing it at 35-40C? Sunlight is much worse than heat (unless excessive heat), but still, storage stability will be better at lower temperatures. Also, like I said above explosive sensitivity is higher at elevated temperatures.

ksj_6808 - 6-7-2012 at 23:28

Here are some tips that i've found while making nitroglycerin. First off, yes you can use vegetable glycerin, it's the same thing as the high dollar glycerin. I've made several batches with 95% fuming nitric and also 70% nitric, they both work great, except you wont get as high as yield with the 70. As for the sulfuric, i've used both 98% from dudadiesel and rooto drain cleaner from ace hardware and they both work fine except the nitro tends to take on a more pale yellow color when the drain cleaner is used, but from my experience, it's not any more sensitive. Another thing, have a good idea of how to carry the synthesis out, don't get into a hurry,
I was nitrating 400g of glycerin in about 6L of acid, i'm fairly experienced in the synthesis but those big batches are a lot easier to run away than the little ones, needless to say i wasted over a pound of nitro and about 6L of acid, It didn't run away but the temp just started jumping up too fast, got in too much of a hurry, won't try that again!!

Okay, another point to make, do not go off volume when deciding how much acid to glycerin you will need when ramping up the quantity of the batch, always go by weight.

Don't crash the whole batch into water as it will get very hot and the nitro could become unstable, instead use a pipette to draw the nitro off the top of the acids and drop it into a beaker of ice water, just take your time.

Allright, this is something i had a problem with, the neutrilization. What i'd do is wash wash wash with bicarb and wash with water and let it sit overnight, yet when i removed the nitro from the water it would have a ph of 1. Well figured that out, wash once with water, next slowly drop it into a bicarb solution and swirl it around and let it sit for about an hour, do the bicarb thing twice, next do one water wash, then seperate the nitro and dissolve it completely into acetone, then crash into water and do 2 more water washes, now you have nitro with no acid left trapped in it and it also seems to be more stable with that tiny bit of acetone dissolved in it.

Lastly, dehydrating the nitro...I havent found it to be anymore unstable dehydrated than hydrated. Put your nitro in a small beaker or plastic cup, now find some type of jar or something that's air tight and cover the bottom of it with salt, just regular table salt, put quite a bit in there, now just set the beaker of nitro on top of it, seal the lid and let it set for about 24 hrs, now you have high quality anydrous nitroglycerin. The nitro should have a slight smell of acetone, this is good, as it should be a little more stable. Wack it with a hammer to test the stability. Now just store it at room temperature and you should be good, I've never stored nitro but for about a week but i wouldn't store it too long, i usually use it within a week. Just make sure it's neutral or close to it. :D

Ral123 - 7-7-2012 at 02:25

I don't know is it because of the quantities, why industrial nitro is supposed to be pale yellow with 10 washes and mine is just fine with like 2. I take the crude egdn/ng, dump in distilled water and swirl well, then again but with soda solution or ammonia. Then final 1-2 washes with distilled water (if it's egdn I'm not afraid to shake hard), leave in open container for a while and it becomes crystal clear, odorless for ng. Ksj_6808 how did you stirr and cool your huge batch?

ksj_6808 - 14-7-2012 at 01:07

I used a huge flower vase, probably about 15L. And a 5 gallon pickle bucket with a shit load of ice and water. I put all the acid together in the vase and then set it in the pickle bucket, then put the lid on and put it in the deep freeze. Then i used a turkey baster to add the glycerol, about 10-20mL at a time. The vase full of acid looked like something you would see in a nightmare!!lol. But i wobbled the vase around to stir it. I may try it again in the future, but i think im gonna work up slowly toward it, right now im a champ at nitrating 70g but that's all my 1L beaker will hold. Truth is, it was a couple nights before the 4th of july and i was in a big hurry to get it done and it was 4am when i was almost done. Didn't take any longer really than a small 70g batch, but the temps definately a little more unpredictable though. All i can say is 85g of nitro makes one hell of a bang and has incredible power!!:D BTW i think i found a very easy shaped charge, take a coke can, cut it in half, fill it up with nitro, thats what i did in the image, im pretty sure it made a decent shaped charge!!

A.png - 899kBB.png - 970kBC.png - 1MB

Ral123 - 15-7-2012 at 08:46

From 1l batch you expect 50ml?? Man, I distill nitric from KNO3/H2SO4 and it's totally worth it. You get yield almost as you're spend acids. To "wobble the vase around to stir it" is totally unacceptable for that kind of operation, specially in these quantities. Third, that nifty iron piece is nothing to what you would expect from a nice shaped charge with blasting jelly.
http://www.youtube.com/watch?v=nyM1Y0OjfzQ
btw ng is not suitable for use in liquid form, egdn is better.

Kalium - 16-7-2012 at 01:34

Quote: Originally posted by ksj_6808  
Here are some tips that i've found while making nitroglycerin. First off, yes you can use vegetable glycerin, it's the same thing as the high dollar glycerin. I've made several batches with 95% fuming nitric and also 70% nitric, they both work great, except you wont get as high as yield with the 70. As for the sulfuric, i've used both 98% from dudadiesel and rooto drain cleaner from ace hardware and they both work fine except the nitro tends to take on a more pale yellow color when the drain cleaner is used, but from my experience, it's not any more sensitive. Another thing, have a good idea of how to carry the synthesis out, don't get into a hurry,
I was nitrating 400g of glycerin in about 6L of acid, i'm fairly experienced in the synthesis but those big batches are a lot easier to run away than the little ones, needless to say i wasted over a pound of nitro and about 6L of acid, It didn't run away but the temp just started jumping up too fast, got in too much of a hurry, won't try that again!!

Okay, another point to make, do not go off volume when deciding how much acid to glycerin you will need when ramping up the quantity of the batch, always go by weight.

Don't crash the whole batch into water as it will get very hot and the nitro could become unstable, instead use a pipette to draw the nitro off the top of the acids and drop it into a beaker of ice water, just take your time.

Allright, this is something i had a problem with, the neutrilization. What i'd do is wash wash wash with bicarb and wash with water and let it sit overnight, yet when i removed the nitro from the water it would have a ph of 1. Well figured that out, wash once with water, next slowly drop it into a bicarb solution and swirl it around and let it sit for about an hour, do the bicarb thing twice, next do one water wash, then seperate the nitro and dissolve it completely into acetone, then crash into water and do 2 more water washes, now you have nitro with no acid left trapped in it and it also seems to be more stable with that tiny bit of acetone dissolved in it.

Lastly, dehydrating the nitro...I havent found it to be anymore unstable dehydrated than hydrated. Put your nitro in a small beaker or plastic cup, now find some type of jar or something that's air tight and cover the bottom of it with salt, just regular table salt, put quite a bit in there, now just set the beaker of nitro on top of it, seal the lid and let it set for about 24 hrs, now you have high quality anydrous nitroglycerin. The nitro should have a slight smell of acetone, this is good, as it should be a little more stable. Wack it with a hammer to test the stability. Now just store it at room temperature and you should be good, I've never stored nitro but for about a week but i wouldn't store it too long, i usually use it within a week. Just make sure it's neutral or close to it. :D

That's a lot of NG! I'm guessing it will be used with diatomaceous earth to make traditional dynamite, right?

SherlockHolmes - 29-7-2012 at 09:13

Hi guys. Here's my way of getting nitroglycerin:
This is materials

[img]http://prikachi.com/images.php?images/836/5071836N.jpg[/img]

mix 220m 600m nitric acid and sulfuric acid at ice bath and begin to slowly add 100 ml glycerol



in the middle of the process



Finally pour in 3 liters of water and there it yields




[img]http://prikachi.com/images.php?images/889/5071889A.jpg[/img]

I tested the resulting nitroglycerin on 7 mm iron plate, here's the result:
http://www.youtube.com/watch?v=B5dcGkIwQKQ
Nitroglycerine has a low sensitivity to initiation of EGDN and very strong starter wants to detonate properly and I used an explosive-based pyroxylin as a booster :) Excuse me if I have misspellings or typos but English is not my native language. thank you.

ksj_6808 - 5-8-2012 at 23:13

I've found nitro to be the best explosive for the home experementer simply because it is the easiest to make, the chemicals are easy to get and it is very brisient and powerful, and you can use it for so many things such as gels, dynamites, use it as a plastecizer and a lot of other things.



[Edited on 6-8-2012 by ksj_6808]

ksj_6808 - 5-8-2012 at 23:26

Quote: Originally posted by Ral123  
From 1l batch you expect 50ml?? Man, I distill nitric from KNO3/H2SO4 and it's totally worth it. You get yield almost as you're spend acids. To "wobble the vase around to stir it" is totally unacceptable for that kind of operation, specially in these quantities. Third, that nifty iron piece is nothing to what you would expect from a nice shaped charge with blasting jelly.
http://www.youtube.com/watch?v=nyM1Y0OjfzQ
btw ng is not suitable for use in liquid form, egdn is better.



I watched your video, nice job!! Yeah i don't think you entirely understood what i was saying, first off may i correct the term "wobble" to "Swirl" and yes it's totally acceptable and cools the mixture off better than stirring it in my experience, it's just easier i've done it for about a year with beakers no problem at all. And shaped charge, i know i probably said that but it was 80g nitro in the bottom half of a coke can and the metal was laying on a shale road, it went through it so you cant guage by the picture how much it would have done to a thicker piece. Oh and using a fuse with a HE is "Unacceptable", get updated and use a wireless detonation system. And i said the yield would be a little over a lb on that big batch, where do you get 50mL and i don't go by volume either. You don't get as good of yield as using the 95% nitric because it's 70%, and if you know where to buy the 70 cheap, it's much easier and cheaper to make. Well anyways im not trying to start an argument just backing up what i said. Anyways congrats on the EDGN, i haven't made that one yet

ksj_6808 - 5-8-2012 at 23:31

Quote: Originally posted by Ral123  
From 1l batch you expect 50ml?? Man, I distill nitric from KNO3/H2SO4 and it's totally worth it. You get yield almost as you're spend acids. To "wobble the vase around to stir it" is totally unacceptable for that kind of operation, specially in these quantities. Third, that nifty iron piece is nothing to what you would expect from a nice shaped charge with blasting jelly.
http://www.youtube.com/watch?v=nyM1Y0OjfzQ
btw ng is not suitable for use in liquid form, egdn is better.


NG is not suitable in pure form in large quantities, however you can dissolve some acetone in it, about 5% by weight i suppose, all i know is the more acetone you add the harder it is to detonate, I can barely set the ng off with a big hammer with 1% dissolved in it so it's safe enough as long as you have acetone dissolved in it.

Ral123 - 6-8-2012 at 07:53

So ng isn't good for small charges because of critical diameter and low order detonation possibility and not good for large charges because of sensitivity. No such worries with egdn. Let me tell you something more. I had a batch of 50ml with witch I did a test. I had like 7ml egdn left. It was just washed, I'm not sure if it was neutralised at all, just well washed with tap water. It showed no change for more then 6 months. It was crystal clear, sitting near a window with other glassware. I did ng, I washed with distilled water, neutralised with ammonia excess, washed again multiple times. It was clear like water, but after like a month it had a brown-green layer. So talking about stability in liquid form egdn rules. For dynamites and stuff ng is the way. I admit I use it for my etn/ng/nc composition. I washed my last ng with tap water. It's little less yellow then my fuming nitric acid :D Just threw in fridge and hope the crap doesn't decompose for the next few months.

ksj_6808 - 6-8-2012 at 13:55

Ya EDGN im sure is alot better to use all around, and im sure it keeps alot better, ill probably try some here in a week or so, and yes ive noticed the same thing with ng, it tends to take on a yellowish color after a few days, the way i use it is ill usually make about 85g and it is very powerful every time and i dont store it for more than a week, havent really tried any bigger and did a 20g charge back in the day. Im assuming you get higher yields with edgn because of the 2 nitro groups. Anyways good luck!!

Ral123 - 6-8-2012 at 19:44

NG better for all around purpose. EGDN best in liquid form. And yes, you get more product for your acid with egdn.

killswitch - 15-8-2012 at 15:16

Quote: Originally posted by ksj_6808  
NG is not suitable in pure form in large quantities, however you can dissolve some acetone in it, about 5% by weight i suppose, all i know is the more acetone you add the harder it is to detonate, I can barely set the ng off with a big hammer with 1% dissolved in it so it's safe enough as long as you have acetone dissolved in it.


When I've finished neutralizing my batches, I dissolve it in nitromethane rather than acetone. The best I've tested is a mix of 1 mL NM per 8 mL NG. Add 1 mL of ethylene diamine per 10 mL of NG/NM mixture immediately prior to use for added kick.

I've often wondered if liquid bases like ethylene diamine could be used to quickly neutralize NG. But I've never had the balls to try it.

Ral123 - 15-8-2012 at 19:49

How do you add kick by reducing the energy of a mixture? And at ratio near 1:1 ethylene diamine/nm.

ksj_6808 - 16-8-2012 at 14:39

As far as i know to add a kick to it would be to add some aluminum powder, as far as a stablizing agent, i dont know if NM would work, i would guess that it dissolves nitro but dont know if it would stablize it, the NM is an explosive however very much of it would surely lower the vod, however if your talking 1%, it shouldnt do more than simply stablize it and the power reduction should be minute. If you were wanting to do a large charge, say several kilos, either make it into dynamite or use TNT instead.

Ral123 - 14-1-2013 at 13:49

This article suggests that mixture of NG and cocaine gives more powerful effect then cocaine itself. What effect do you think NG will have with weed? May be ETN/cocaine or a bong with MeNO3 in the water?
http://en.wikipedia.org/wiki/Brown-brown

SherlockHolmes - 20-3-2013 at 09:30

Today I made a test with 140ml nitroglycerin on 30 mm hardened steel disc. I put 5 grams. pyroxylin booster because I'm not sure that will raise 7500 m / s in glass jar only with lead azide blasting cap. Synthesis made ​​with 600 ml. Sulfuric acid, 600 g. Ammonium nitrate and 150 ml glycerol. Lot I tried to do the video. Hope you like it: http://www.youtube.com/watch?v=sKwknfZCLE8

Ral123 - 20-3-2013 at 12:10

The best pure NG test ever. That nitro looks brisant like EGDN. Nice yields also.

SherlockHolmes - 20-3-2013 at 13:49

Normal. Nitroglycerin is like egdn. egdn is a little more powerful than nitroglycerin but the difference is almost unnoticeable. This booster that I was able to lift 7800 m/s. Greater speed can be raised only with metal body and 80g of picric acid booster :)

Ral123 - 20-3-2013 at 14:02

I dream explosives weren't illegal, so I can make universal purpose 65g picric acid boosters in 28mm copper pipes with cap in the one end. It will be a classic, that may last long for my grand children.

Peroksit - 22-3-2013 at 02:09

I' have a question of NG separete (I'm use teflon tap sparatory funnel)

separatory funnel tap is can be compressed of ng and may be exploding NG ? what are you recommend to separate of NG ?

SherlockHolmes - 22-3-2013 at 02:24

This is not ethyl perchlorate: D nitroglycerin will explode in a separatory funnel. One of the possible procedures for separating the yield of nitroglycerin with separatory funnel. If so easy detonate NG, now no one would risk it synthesizes.

Peroksit - 22-3-2013 at 02:48

Quote: Originally posted by SherlockHolmes  
This is not ethyl perchlorate: D nitroglycerin will explode in a separatory funnel. One of the possible procedures for separating the yield of nitroglycerin with separatory funnel. If so easy detonate NG, now no one would risk it synthesizes.

I'm not fully understand :S separate with separatory funnel of NG do explode ? did not explode :D or possible risk is nitration of NG ?




[Edited on 22-3-2013 by gamez34]

[Edited on 22-3-2013 by gamez34]

SherlockHolmes - 22-3-2013 at 03:42

Risk nitration always. If the temperature passes 30 degrees will explode. And I mean that nitro will not explode in a separatory funnel.

Peroksit - 22-3-2013 at 04:08

Quote: Originally posted by SherlockHolmes  
Risk nitration always. If the temperature passes 30 degrees will explode. And I mean that nitro will not explode in a separatory funnel.

Ok Thanks I'm understand

Ral123 - 22-3-2013 at 05:36

SherlockHolmes, did you find a piece of the steel with stamped text from the bottom of the glass vessel?
For safety, not that I have much experience with NG, I'd suggest adding some acetone to the NG and then wash, add to separatory funnel, mix with acetone and wash again. Take the NG again, let the water and acetone evaporate for a few days. You'll have predictable PH neutral NG, that can be stored safely from months in cold, dark place. Label you bottle with warnings, you never know when it may have do be handled by someone else.

SherlockHolmes - 22-3-2013 at 08:35

If I found it, I would show it. This Acetone Why? Even then dissolved in acetone mixed with other compounds will not disappear. Here's a good way to neutralize and clear: Raw NG derived from the nitration mixture I put it in a container with larger triple volume 2% solution of sodium bicarbonate, or better yet, potassium carbonate. Gently heat up the water bath to 35 to 40 * C and stir vigorously 5-6 minutes with a wooden stick, being careful not to overdo - NG has the ability to form stable emulsions if overdone with stirring. Wait half an hour or more to settle exude it and put into a water layer of 24 to 48 hours. If it is clear, change the water and let to rest one more time.

Ral123 - 22-3-2013 at 08:45

Have you tried it's PH or storage stability. I washed a batch of NG several times with distilled water, ammonia and bicarbonate. It was still a little acidic. It took 3 weeks before it got brown-green layer, stored at warm, sunny place, but not under much direct sunlight or heat.

SherlockHolmes - 22-3-2013 at 08:55

With proper cleaning can be stored and more than a year.

dasgoose21 - 22-3-2013 at 09:27

Quote: Originally posted by SherlockHolmes  
With proper cleaning can be stored and more than a year.


This is not always nessecarily the case, although he did hint at a good point. If you use dark amber glass bottles and store the nitro in a cool dark place, then it will decompose slower than if placed in a sunny place in a clear bottle. You could also keep it more stable by adding a desensitizing agent such as dinitrotoluene, but this will also make your final product much harder to detonate.

I Like Dots - 10-4-2013 at 16:40

Hey guys, first post. Yesterday I tried my hand at this.
6ml Sulfuric Acid
4gm ammonium nitrate
1ml Glycerine.
Everything went fine, I got almost 1ml of NG.


Today I tried to scale it up 10x. Again, everything fine (except for a rather large amount of NO2 when I added the nitrate).

After the reaction I poured it into ice water, and removed what I thought was the Glycerin layer. Washed with cold water one more time.
I left this mixture to settle out and came back in a hour to find this:


The top layer is water, then there is a clear layer, then a brown layer. The brown layer later settled on top of the clear layer. There are also bubbles forming, and froth on top.

I have yet to neutralize the NG solution. Both brown, and clear liquids are oily, only brown burns. Im guesing dinitrate and trinitrate? Or some ammonia compound from the dissolved NH4NO3.

Has anybody done this before that experienced this? thanks.

Trotsky - 12-4-2013 at 01:18

It looks more pink than brown.

Did the solution ever get warm? The color and the bubbles sound like it may have partially runaway and the result is a lot of dissolved NOx gasses being released.

Alternatively, as was discussed in my thread entitled nitration bath turned colors, you could have impurities in your reagents. What was the source of your AN? I have used Walgreen's brand cold packs and crushed them down to a fine powder. However, I did not wash my AN. After washing my AN, it was easier to dissolve into the H2SO4 and it did not turn this pink/red/brown color. Unfortunately it was harder to get it to a real fine powder. I'm not using a ball mill, though, I'm just using an improvised mortar and pestle.

There was very little or no coloration present in small nitration baths, but larger ones, the size you've got, were just about identical in color to your image there. However, my solution was more opaque almost. This was due to whatever anti-clumping agent they used with their prills.

What about the purity of the glycerin?

If I were you I would separate the two and then treat them both the same, clean them up properly, and see how things are. The clear could just be unreacted glycerin perhaps, but that'd be quite a bit of unreacted material if your had the ratios correct. If it's due to an impurity or dissolved nitrogen oxides it should go away with time, cleaning it up with remove the coloration, but I'd still work with them separately.

When you say the clear layer won't burn, do you mean that it doesn't deflagrate or that it is non-flammable? Even unreacted glycerin will burn, according to Wikipedia some use crude glycerin as a heat source. If it's non-flammable, is it possible that you have an NG/Water emulsion? I have heard that NG will form a stable emulsion with water if it's mixed too strongly. Given that you haven't neutralized it yet, I suspect that this isn't the case, but if possible what's the solution then? Perhaps adding ethanol to dissolve the NG then salt it out, remove ethanol layer and evaporate the solvent? That should work pretty well, I think.

I Like Dots - 12-4-2013 at 08:50

Thank you for your thoughtful reply!

It was kept between 6-10 C in a ice/salt/water bath chilled in the freezer.
Glycerine was 99.5% anhydrous.
Ammonia nitrate was from a cold pack from CVS.
Sulfuric acid is 96% drain cleaner with a slight red/range tint.
When I added the nitrate to the acid, it turned a reddish color and was opaque.

The clear layer was non-flammable, even when a torch was applied (NO2 vapors were observed). This leads me to think that it was unreacted glycerine that absorbed some water when I washed it.

The brown layer was NG .

Ok, now I think I know what happened. I rinsed it well, but there was a small amount of acid remaining in the NG, which started nitrating the glycerine when I removed it from the ice water I rinsed it in. The remnants of Nitric acid started to react with the Glycerine as it was warming to room temperature.


So my goof was not neutralizing it sooner. Next time I will allow the glycerine to sit in the cool nitrating bath for longer, then immediately neutralize it after washing.

Hennig Brand - 3-8-2013 at 04:37

Thought this might be of interest. This is what 200 g of ammonia dynamite with only 10% NG can do to over 35 tonnes of granite rock when placed in a borehole drilled just past the center of the rock and stemmed with crushed rock. About 15 tonnes of the rock pieces have already been hauled away. What is left is about 20 tonnes.

35 Tonne Granite.JPG - 423kB

Notice the Canadian 5 dollar bill placed on the rock for scale. The rock is more than 7 feet tall.


[Edited on 3-8-2013 by Hennig Brand]

Peroksit - 19-12-2013 at 09:28

I would like to ask a question
The ng can freeze in nitration acid when it is between 0C-5C ? The low temp occurs a problem ?

Edit :
I have found answer of my question


[Edited on 19-12-2013 by Peroksit]

pic.png - 188kB

Hennig Brand - 26-1-2014 at 19:07

During nitroglycerine production the bottle neck for me, and I am sure for others, has been the residual acid neutralization step at the end. It can be a righteous pain in the ass to neutralize the acidity, especially if the quantity of nitroglycerine is substantial.

The problem again is that in the absence of agitation the NG simply sits on the bottom of the vessel and only the surface is exposed to the bicarb solution. Also, if the bicarb solution is not circulated, the concentration of bicarb in the reaction zone (next to the NG) can become lowered which also reduces the efficiency of the process. Another point is that the acids in the NG are, of course, very soluble in the aqueous solution and agitation helps wash the NG and transfer the acid to the aqueous bicarb solution.

I was using a small centrifugal pump for a while to agitate the NG and circulate the bicarb solution, but I wanted something better. I was a little nervous of the NG being sucked into the pump and encountering friction. I decided I wanted to build a machine to swirl or shake a flask in much the same way as a person would do by hand. At first I was considering building a shaker, but after reading the webpage below I realized that a rocker was probably the right machine for the job.

http://www.stuart-equipment.com/category.asp?dsl=120&

A pdf of the text from the webpage is also attached below.

A dc motor and gear train was salvaged from an old printer. Some scraps of wood and a bit of packing foam were also used. I spent about 2 hours on this, and no money, so a much more professional and reliable machine could easily be built. It does work very well, however, even if it is just a first crude attempt.

The motor is rated for 24 V dc, but I found that it was much too fast at that voltage even with the gear reduction. I found an old 16 V switching power supply which seems to give about the right speed. The 16 V power supply still rocks the flask fairly aggressively (about one cycle in 0.7-0.8 seconds), but doesn't splash water everywhere. One picture of the stationary machine and two stills from a video of the machine in motion are included below.

With warm bicarb solution, I believe this machine could do a lot of neutralizing in 10 minutes.


Attachment: Laboratory Shakers and Rockers.pdf (115kB)
This file has been downloaded 379 times

Rocker.jpg - 416kB Rocker In Motion 1.jpg - 106kB Rocker In Motion 2.jpg - 107kB


[Edited on 27-1-2014 by Hennig Brand]

Ral123 - 27-1-2014 at 07:50

I'm not sure if NG purification can be done well without solvents.

Motherload - 27-1-2014 at 08:24

I used to mix in acetone about half the volume of nitro glycerine.
10 ml crude NG + 5 ml of Acetone and then swirl with bicarbonate soln.
Was always too afraid of pure NG.

Hennig Brand - 27-1-2014 at 12:33

Quote: Originally posted by Ral123  
I'm not sure if NG purification can be done well without solvents.


It most definitely can. I had a fluid ounce stored for 3 years or so, which was treated with just aqueous bicarb solution, and it was still perfectly clear (not even any yellow tint). It did of course take days of sitting in bicarb solution with occasional swirling to get it to that point.

Depending on the acetone used it might actually add contaminants, and the method will result in at least a small amount of product loss. I do like the acetone method concept, but I still prefer the aqueous bicarb method over it.

With warm aqueous bicarb solution and good agitation residual acidity can be neutralized quite effectively and quite quickly.

roXefeller - 27-1-2014 at 16:37

I'm so glad other people use the coffee table for prototyping also. What is your method to agitate while nitrating? And do you ever store in a binary state or do you mix the binary/tertiaries prior to use. I'm worried about weep if I rolled up a dynamite for later use.

Hennig Brand - 27-1-2014 at 17:31

When I first started, during nitration, I used to stir with a glass laboratory thermometer very carefully (trying not to hit the sides or bottom of the vessel). I quickly decided that swirling would be a lot safer and from then on I tried to use vessels that allowed easy swirling. I usually store the pure liquid. I try not to store large amounts and am very careful about it. The pure liquid is much more versatile among other things.

Edit: Rocker/Neutralizer update

I made 8 mL or so of NG just to test the rocker/neutralizer machine. What I found was that the 24 V motor had to be run at an even lower voltage than 16 V or else the NG blob stayed more or less stationary even though the flask and water were moving vigorously. This is because NG is very viscous (resists flow) in comparison to water. I have found that at about 12 V, or 1 cycle per second of the rocker platform the NG blob rolls around quite well. Slightly slower than this may even be better. Another thing that could be done in order to place a larger proportion of the gravitational force on the NG blob in parallel with the bottom of the flask, and increase blob motion, would be to increase the range of motion of the rocker so that it was tipping the flask over farther.


[Edited on 28-1-2014 by Hennig Brand]

Hennig Brand - 8-2-2014 at 06:30

Here are a couple of pictures of the rocker machine with better lighting. A couple of small adjustments have been made. The platform was raised above the axle more and higher pieces of high density packing foam were fastened to the top of the platform. The foam is quite elastic and the pieces were installed so that the flask fits very snugly in the surround made by them.

Something that wasn't obvious from the earlier pictures, and can be seen in the second picture below, are the two wooden blocks which were installed below the platform to prevent the platform and flask from flipping right over in the event of a mechanical failure. An old computer power supply, seen in the first picture, is used to supply 12V dc to the 24V electric motor.

Rocker Machine.jpg - 371kB Platform Underview.jpg - 398kB

[Edited on 8-2-2014 by Hennig Brand]

Ral123 - 8-2-2014 at 06:51

What does the litmus show after the procedure, if only bicarbonate and distilled water is used?

Hennig Brand - 8-2-2014 at 07:08

When tested, pH paper shows that the water above the NG is always slightly alkaline, due to unreacted bicarb. Never tried to directly test NG with pH paper. My testing methods may not be the best. One thing I look for is the presence of CO2 gas bubbles rising from, or on or in, the NG. If a little shake of the NG in bicarb solution shakes free any CO2 bubbles or causes any to become evident on the surface of the NG I conclude that the bicarb is still doing its job of neutralizing acidity. If with a bit of shaking no CO2 bubbles are evident, and the aqueous solution above is still alkaline of course, then I conclude the acidity is pretty much neutralized. As I have said, my methods may not be the best, but I have stored NG samples for years with either no or very little signs of decomposition.

The_Davster - 8-2-2014 at 10:36

Aquarium bubbler.

dilute bicarb wash alternating with water wash, each agitated by a bubbler.

3-4 washes of each, each allowed to go overnight, and then dried it in a desiccator. Was stable for 3 or more years staying pH neutral and perfectly colorless. Tasted the same before and after too :D

Motherload - 8-2-2014 at 11:03

How long did your boner last after tasting it :D ?

Hennig Brand - 8-2-2014 at 11:52

I really like explosives, but so far I haven't mixed explosives and sex. You guys are really into this. :D

The aquarium air bubbler idea sounds good. I have avoided air agitation for the nitration process just because of nitric stripping and moisture addition issues. I guess the air could be dried. For neutralizing residual acidity, it's probably a pretty good process.

The_Davster - 8-2-2014 at 12:11

Quote: Originally posted by Motherload  
How long did your boner last after tasting it :D ?


Hard to tell, I already had one before I tasted it...

Quote: Originally posted by Hennig Brand  


The aquarium air bubbler idea sounds good. I have avoided air agitation for the nitration process just because of nitric stripping and moisture addition issues. I guess the air could be dried. For neutralizing residual acidity, it's probably a pretty good process.


What moisture addition issues? you are either washing with aq. bicarb or water. Why would you care about dry air when it is under water?

[Edited on 8-2-14 by The_Davster]

roXefeller - 8-2-2014 at 12:12

The use of ED drugs is a contraindication for the administration of NG or nitrates. So if you are already getting black market viagra, don't go dosing on NG for added effect.

Hennig Brand - 8-2-2014 at 12:18

Quote: Originally posted by The_Davster  

What moisture addition issues? you are either washing with aq. bicarb or water. Why would you care about dry air when it is under water?
[Edited on 8-2-14 by The_Davster]


I was referring to using air to agitate the nitration mixture in that case, not the bicarb solution. A lot of old texts describe using compressed air to agitate NG nitration mixtures.

[Edited on 8-2-2014 by Hennig Brand]

Peroksit - 10-2-2014 at 23:54

Hennig Brand what do you use for mixing of nitration acid ? mechanic mixer or hand mixing or air ?

Hennig Brand - 12-2-2014 at 17:39

Quote: Originally posted by Hennig Brand  
When I first started, during nitration, I used to stir with a glass laboratory thermometer very carefully (trying not to hit the sides or bottom of the vessel). I quickly decided that swirling would be a lot safer and from then on I tried to use vessels that allowed easy swirling.


The rocker would work, but some sort of three dimensional rocker or swirling type machine would probably be better. The rocker I built works in only two dimensions. I was also thinking of a small overhead stirrer, with a teflon or teflon coated paddle rod. One could easily be built, with a shield and maybe a small (loosely stuffed) stuffing box to keep acid vapors from destroying the electric stirrer motor. A dc motor would make stirrer speed control easy. The top part below the neck (funnel shaped) of some plastic bottles could easily function as the shield and the neck and screw cap could easily be converted into the stuffing box. A little cotton or flax with some wax or grease (Vaseline maybe) worked in could be used as packing for the stuffing box. This would keep the acid vapors from getting at the motor and electrical connections and still allow the stirring rod to turn mostly unimpeded. Most support for the stirring rod would need to come from some sort of bearing between the stuffing box and the motor. A simple sleeve bearing would probably be fine for this low speed and low duty application. A makeshift sleeve bearing could be made from a bit of metal tubing or even a smooth hole through a bit of hardwood (well lubricated) would probably suffice.

A stuffing box is a very old and ingenious way of sealing a rotating shaft. It serves as a barrier preventing leakage of liquids and/or gases.

[Edited on 13-2-2014 by Hennig Brand]

Hennig Brand - 27-7-2014 at 11:02

I used 230mL of the nitric acid that was made with the home made distillation apparatus to nitrate some glycerine. The following link should take you to where production of the nitric acid was discussed.
http://www.sciencemadness.org/talk/viewthread.php?tid=15676&...

A round, glass coffee pot was used to perform the nitration. About 230mL of nitric acid which titrated as 82% was used. About 460mL of sulfuric acid which titrated as 91% was used. About 115mL of glycerine was used. The flask/coffee pot with mixed acid had a plastic wrap cover put over it. The plastic cover is in my opinion a wonderful addition, because it keeps water out and the unpleasant vapors in. A liquid medication 10mL syringe was used to add the glycerine. A small hole was poked in the plastic wrap cover so that the plastic tip of the syringe could be put through and the glycerine could be added. About 2-3mL of glycerine was added at a time followed by a few swirls. During swirling one hand was supporting the flask from underneath (temperature sensor and support) and one hand was on the handle. A few times during the addition the flask started to warm up above room temperature so it was placed in a large bowl of ice and water and swirling continued which quickly brought the temperature back down. The addition of the 115mL of glycerine took about an hour. A piece of plastic wrap, without a hole, was then placed over the coffee pot and the flask left to sit in the dark at room temperature for about an hour and a half. The NG was removed using a separatory funnel and the nitration mixture recovered and put back in the dark. The next morning another crop of NG (about 20-25mL) was removed from the acid mixture.

The nitroglycerine was washed twice in water and then left in 4-5% sodium bicarbonate solution for several days with occasional swirling. Yield was a bit better than 1mL NG per mL of glycerine. I was also thinking that a rocker/washer vessel should have a corrugated bottom, which should facilitate washing much better than a flat bottom (see posts above).

A bit of 10% NG, starch, ammonia dynamite was made and used on a green maple stump. The tree was healthy and cut just days before the blast. About a 300g charge was used. A blasting cap, with 1g of ETN, 0.1g of undextrinated lead azide and a bit of basic lead picrate, was used for initiation and was fired electrically. The charge was placed in a 1 3/4" inch hole that was bored below ground level into the stump with a hand auger. Boring was difficult and the hole ended up being slightly off center. It is difficult to see from the pictures taken, but half of the stump below the ground was blown away and the rest is damaged because the stump can be wiggled easily by hand. Before the blast an available farm tractor couldn't budge the stump, but now a tractor or a set of come alongs should be able to remove it easily. A larger quantity of explosive was not used, and another blast was not considered because of the proximity to a house. It was quite risky as it was. Several other stumps were removed completely the same afternoon, in safer locations farther from structures and vehicles.

Plastic Wrap Cover.jpg - 205kB NG on Surface of Mixed Acid.jpg - 346kB NG Yield.jpg - 424kB Charge in Place and Tamped.jpg - 484kB Moments after Detonation.jpg - 491kB Damage.jpg - 523kB


[Edited on 28-7-2014 by Hennig Brand]

Turner - 27-7-2014 at 16:02

That is very close to a house!!

What did your neighbors have to say of the 300 grams of HE exploding right there?

Hennig Brand - 27-7-2014 at 17:48

Well, it wasn't my neighbors, but even so it was a very rural location (farm land, etc). The owner is a friend and understood and accepted the risk. Blasting stumps is not loud like an air blast above ground, for a similar weight and type of explosive. Actually, usually when I blast a stump it is more of a big thump kind of sound rather than a bang (not hard on the ears at all). The exception would be if a stump, or other target, was severely overcharged (too much explosive). Then you can experience a significant air blast. The earth, wood, etc, normally do a very good job of deadening the sound from an explosion, especially if the blaster isn't being wasteful of explosives.

Bert - 27-7-2014 at 19:34

Did you stem the bore hole? That is, tamp sand, dirt or clay into any empty space over the charge-

NeonPulse - 27-7-2014 at 19:50

Pretty close there. I wouldn't personally have let 300g off so close to my house though,but if the owner understood the risk and was still willing then why not? Great to see a practical use for the NG. Seems to have done what NG does best! Good pictures and story to go along with it too.:)

Hennig Brand - 28-7-2014 at 06:12

Quote: Originally posted by Bert  
Did you stem the bore hole? That is, tamp sand, dirt or clay into any empty space over the charge-


Yes indeed, crushed rock was used to fill the borehole over the charge and then a wheelbarrow load of very wet, heavy earth from a nearby stream bank was packed in over that whole side of the stump (over the bore hole). I learned a while back that crushed rock makes excellent stemming when rock blasting. It tends to bridge or lock together in the hole and makes a very solid blockage. It may not work quite as well in a wood hole though, I don't know. Very wet and heavy sandy earth with high clay content was chosen as tamping material (it also happened to be close). It is mostly the high water content which makes that tamping material so effective.

As stumps go it was a fairly tough target. Green maple is pretty tough stuff. The dynamite used was a very low velocity type as well.

@NeonPulse
Thanks, I hesitate to post things of this nature, but for the most part I think I was being responsible. Of course, the professionals would probably never consider blasting anything that close to a house, especially in modern times. Insurance is the big thing nowadays.


[Edited on 28-7-2014 by Hennig Brand]

Hennig Brand - 30-7-2014 at 13:57

I realize that the results of that last blast didn't look all that impressive, so I took some pictures of another blast that should be a little more interesting. The first picture is of the last stump with a Pepsi can beside it for scale.

This stump was very large, but it was cut at least a few years ago and was softwood not hardwood to begin with. This charge was of the same type but slightly heavier, at 350g, than what was used for the stump from the last post (ca. 300g). The same materials and quantities were used for the detonator.

Stump from last post.jpg - 485kB 350g charge & cap.jpg - 437kB Capped charge.jpg - 460kB Hole ready.jpg - 518kB Charge in place.jpg - 516kB Tamped with mud.jpg - 519kB Moments after detonation.jpg - 507kB After smoke cleared.jpg - 532kB


[Edited on 30-7-2014 by Hennig Brand]

Bert - 30-7-2014 at 20:45

I can't fault the performance-

I'd suggest that a charge placed in a shaft augered into the earth next to, and angled under the stump to loosen the earth and allow a tractor or 4WD truck to snatch the stump out with a log chain would be easier than trying to drill the stump itself below ground level? Such drilling is quite awkward, and the inevitable dulling of auger bits by sand & etc. from the soil slows the process even more.

An ammonia dynamite of less than 15-20% nitroglycerin content is essentially an ammonium nitrate explosive with an active sensitizer... For such uses, my taste would be to use a very thin jelly of around 98% NG:2% NC, and as dense a fuel/absorbent as possible to allow a somewhat plastic and more easily rammed to fit bore composition. Naoum in "Nitroglycerin and Nitroglycerin Explosives" suggests rye flour as a suitably dense absorbent/fuel for such very low NG variants of ammonia gelignite. Plus, you can make a nice pumpernickel with any leftover rye flour?

For close in to valuable structure blasts, blasting mats are the thing. These may be approximated by placeing disposeable scraps of plywood over the backfill/tamping materials, and then covering the blast zone and over laying plywood with burlap potato sacks filled with sand. You want the gasses to be able to escape fairly easily once they break the surface, without offering up any large, hard, dense objects that could fly beyond your safety perimeter.

Safe & efficient stump blasting is an art, and "reading" both the soil & the stump is a vital skill to be learned. I'm barely a beginner.

Hennig Brand - 31-7-2014 at 04:04

You have some good points there. It isn't really clear from the above pictures, but that maple stump is more than half cut off below ground level now and the half remaining appears to be severely crushed, because the stump can be wiggled by hand now. I think a tractor could now pull it out easily. Just to clarify, we were careful to dig down on that side of the maple stump and remove the earth before drilling into the stump. It was just wood (not rock or earth) that was drilled, which was a bit lucky. The hole was drilled down at an angle as well, probably around 30-40 degrees from horizontal. It didn't occur to me to take pictures until after the charge was placed, which is a bit of a shame. What I have noticed is that very often hardwoods can be very difficult to dig under and make a hole large enough and in the right place (center of stump) for the charge. I blasted a large green elm stump a couple of months ago and after about an hour of picking away with a large crowbar and a garden trowel I did manage to get a small hole under it, but the charge was made to fit the hole not the other way around. Big soft wood stumps on the other hand, like the last blast posted about, have a much less complicated root system, and generally no tap root, and it is usually very easy to dig a hole underneath and place the charge.

The explosive type was chosen because it stretched the supply of NG, not because it was necessarily the best explosive for the job. I sometimes go as low as 7-8% NG even, which is still cap sensitive, but yes, it really isn't dynamite and is called nitroglycerin powder IIRC.

I like the improvised blasting mat idea. I made do by being very careful of charge placement and charge size, etc, but blasting mats would have been a good idea.

I am still a beginner too. I think I have 20-25 stumps under my belt and about 20-25 boulders as well. Now that I have a bit of experience I should probably hit the books again. The bit of experience should make absorbing the theory easier now.


[Edited on 31-7-2014 by Hennig Brand]

Jimbo Jones - 31-7-2014 at 08:17

Ordinary flour is superior to starch in terms of absorption, so there is no need to gel the nitroglycerin. Just dry the flour in oven before use, mix it with the AN and then add the nitroglycerin. Heavy duty nylon bag is OK for this purpose. It allow you to form the mixture in the shape of stick and actually tape it to real stick, which is handy when it’s come the time to put the charge in the bore hole. I have made excellent ammonium dynamites with 15 % NG and even better with EGDN and flour.

Always bore the holes in the earth deep beneath the roots and close to the center of the stump. These will allow you to use more explosives because the earth will confine the blast where it’s needed and will act as natural tamping material. Putting the charge near the roots will shatter the wood instead to “remove it”. Consider them as a week spot.




[Edited on 31-7-2014 by Jimbo Jones]

Hennig Brand - 31-7-2014 at 09:24

According to "anval.net" corn starch has the highest bulk density of the three fuels/absorbents mentioned. Attached is a pdf of the bulk density table where the figures came from. I suppose bulk density can vary as well. With only 10% NG, the ammonium nitrate & starch mixture still basically looks and feels dry. Once you get up around 30 to 40% NG it is nice to add a little nitrocellulose though.

Corn Starch: 689 kg/m^3
Rye Flour: 673 kg/m^3
Wheat Flour: 673 kg/m^3

I have found that by using cardboard or wooden forms that waxed paper tubes can be quickly and easily rolled. This allows me to make the charges or sticks just under the diameter of the borehole in the case of rocks and stumps that have been drilled. It is best if the charge fits snuggly in the borehole. The powdered explosive is simply spooned into the tube in increments and then tamped with a wooden dowel (I actually used a large drill bit the other day (the shaft end) because a dowel wasn't close by).


Attachment: Bulk Density Table.pdf (255kB)
This file has been downloaded 649 times


[Edited on 1-8-2014 by Hennig Brand]

Jimbo Jones - 31-7-2014 at 12:28

Yes, indeed, you are right. When I made my tests I judged by the look and the feel of the mixtures and have not search for any further information. With 15 % my mixtures also looks barely wet. Sorry for the confusion.

Try the flour version if you wish and have the time & NG to do it. After all it’s all about the funny things.

Hennig Brand - 31-7-2014 at 17:33

Flour probably works just fine, maybe even better than starch I don't know. I imagine the result would be pretty similar though. Here is a link to an interesting site which gives descriptions of what looks like most of the available techniques for removing stumps. Blasting was one of the methods mentioned, but it was obvious that they didn't plan on very many people being able to use that method.

http://www.dumbstump.com/Decisions-Decisions

Bert - 31-7-2014 at 22:53

With such a low amount of liquid nitroglycerin, curious as to the use of a LIQUID fuel to get the mix with ammonium nitrate back to a "putty" consistency that would be easy to cartridge and later to tamp out the cartridges so as to contact the walls of a bore hole- I've seen these types of extremely dry appearing low NG mixes, they are either powdery or chunky when handled. I like something closer to modeling clay.

Say, real turpentine in sufficient quantity to make an OB mix. Or diesel fuel cetane booster additive. Or other liquid dual purpose sensitizer/fuels, ideally ones that won't interfere with forming gelatin...

It's late at night, perhaps do a search in the morning.

(Edit)

Yup! Reinventing the wheel again...

http://www.google.com/patents/US3450584


Quote:

United States Patent US. Cl. 149-50 16 Claims ABSTRACT OF THE DISCLOSURE A gelatinized dynamite in which the nitroglycerin content is reduced to about 8 to 16% by weight by blending a gel of polyvinyl butyral resin in a solvent, such as caster oil, dibutyl phthalate or dioctyl phthalate, and polyoxyethylene stearate, with a known constituent, such as nitroglycerin or nitrocellulose, and which nevertheless has excellent detonation ability plasticity and extrudability The present invention relates to gelatinized dynamites in which the content of nitroglycerin (or a mixture of the same with nitroglycol, which will hereinafter be referred to as nitroglycerin for simplicity) is reduced to about 8 to 16% by weight and which nevertheless have an excellent detonation ability and are sufiiciently shapable into cartridge by conventional extruder type or rollentype cartridging machine, and a process for the production thereof. The plasticity and extrudability of conventional gelatin dynamites depended upon the amount of nitro gel consisting of nitroglycerin and nitrocotton, and the minimum amount of the nitro gel, which provides for extruding of the resultant gelatin dynamites, has been about 30% by weight. However, there has been a desire for reducing the amount of nitroglycerin blended in gelatin dynamites to a minimum, due to the facts that it is expensive and that nitroglycol admixed in nitroglycerin is poisonous for human body. Recently, an auxiliary plasticizer, such as aromatic nitro compound, surface active agent or synthetic resin, have been used for the purpose of reducing the amount of nitroglycerin to below the aforementioned minimum limit, but even in this case an amount of nitroglycerin as much as 18% by weight is the practical minimum limit. The amount below the said limit results in drastic deterioration of the plasticity and extrudability of dynamites. Even if the product dynamite is shapable, it tends to be hardened with the passage of time, with the result that the detonation ability thereof is deteriorated, making the dynamite unserviceable for practical applications. The use of such auxiliary plasticizer in a large amount to avoid such undesirable effect, however, will cause various drawbacks. That is, the use of an aromatic nitro compound in a large amount will result in lowering the sensitivity of explosive and also in separation of and exuding a liquid substance, whereas the use of a surface active agent in a large amount will render the explosive excessively soft, so that the explosive cannot retain its shape and therefore handling of the explosive, during production, storage and use, becomes inconvenient. On the other hand, when a synthetic resin is used in an excessively large amount, the detonation property of the explosive is extremely deteriorated and the capability of sympathetic detonation of the explosive is lowered remarkably. Due to the foregoing reasons, only the use of auxiliary plasticizer in a large amount has not been very much effective in reducing the amount of nitroglycerin. The object of the present invention is to provide a gelatinized dynamite in which the amount of nitroglycerin is reduced to about 8 to 16% by weight by blending a gel of polyvinyl butyral resin in such a solvent as castor oil, dibutyl phthalate (hereinafter referred to as DBP) or dioctyl phthalate (hereinafter referred to as DOP), and poyloxyethylene stearate, a non-ionic surface active agent, with a conventional constituent, such as nitroglycerin or nitrocellulose, and which nevertheless has a good detonation ability, plasticity and extrudability stands up satisfactory in long storage.


[Edited on 1-8-2014 by Bert]

Hennig Brand - 1-8-2014 at 02:50

Good find. I see more now the significance of what you are talking about. That would be an improvement. Starch and flour do have the advantage of being easily accessible to pretty much everyone though. I suppose there could be some commonly available liquid fuels/sensitizers that could work well.

Yeah, what I need is a good auger for drilling under stumps, through earth and roots, etc. The hand auger we used was really designed for wood working.


[Edited on 1-8-2014 by Hennig Brand]

Rosco Bodine - 2-8-2014 at 09:34

Just making a note that there are several cheaper easier to make ammonia dynamite compositions that have good heaving power that would make them suitable for stump blasting and breaking up earth, where there isn't much need for the shattering of rock that would require higher velocity explosives. Also urea nitrate is in this category of explosive intermediate between ANFO and nitroglycerin sensitized ammonia dynamite. Some of the double salt / adduct dry granular composiitions of ammonium nitrate sensitized by hexamine or glycine, or nitronaphthalene sensitized ammonium nitrate could be applicable also to such uses which is generally earth moving, ditching, clearing beaver dams, soft rock blasting, cratering ground for drainage or making an instant waterhole with larger charges, loosening ground for excavation for holding tanks, preparation for drilling or digging water wells, clearing tough spots for laying pipe or installing junction boxes, ect. Even reactive target mixes like tannerite would work for these kind of low-medium velocity blasting chores that are less demanding than hard rock blasting. Low water content "formite" type or "Tovex" type water gels and emulsions that are cap sensitive could also be good choices as cheaper alternatives to a nitroglycerin sensitized ammonia dynamite.

Hennig Brand - 2-8-2014 at 15:27

I have tried using urea nitrate for stumping several times in the past couple of years and the results were generally pretty poor. I experienced low order detonations with low power for the most part and even incomplete detonations sometimes. The material seems to often take a very substantial kick to get it into high gear and/or some extra confinement. Out of the 5 or 6 times I have attempted detonation only once have I had a result which was similar to low velocity dynamite. That time the material was dried very well (and carefully to avoid decomposition), and funneled into an old propane torch canister and left loose. Initiation was accomplished with a 2 or 3g PETN base charge (can't remember which since it was a few years ago). The urea nitrate charge in this instance was buried in the ground and I remember being impressed by how much earth it threw. I find the material very reluctant to go high order, especially if not perfectly dry. I would imagine a small booster charge would result in urea nitrate more reliably going high order. Urea nitrate sounds like a good material for larger charges, but I have found that nitroglycerin or nitroglycol dynamites are about the most reliable explosive materials there are, especially for small charges and small scale blasting.


[Edited on 3-8-2014 by Hennig Brand]

Rosco Bodine - 3-8-2014 at 09:55

Urea Nitrate is a good test material for detonators because if a detonator will cause high order detonation of urea nitrate, then it will likely also be good for any other energetic material that could reasonably be called cap sensitive.
Two grams of picric acid as a base charge will usually do the job on urea nitrate that is dry and loose crystals at only a slightly settled bulk density as would occur from gently tapping a plastic container to settle the contents. Dry and untamped urea nitrate should go high order if it detonates, and if it doesn't completely detonate then the detonator is inadequate and may have to be increased to 2.5-3 gram range......depending on the quality of the detonator it will high order detonate urea nitrate in that 2-3 gram range of base charge for picric acid, and this test is a good followup to plate testing of detonators, since urea nitrate is only barely cap sensitive and requires a strong cap, it provides a good proof test for a detonator. There is a kind of parallel about the technical difficulty of getting good output from a picric acid base charge and the difficulty for initiation of urea nitrate as a secondary main charge. So urea nitrate will function as a kind of "truth test" material by which you can polygraph your work and gauge its performance.

Safety & Pointers

deadpool - 8-8-2014 at 08:10

@ Henning Brand. First good job on your success; however, I have serious safety and lab concerns with your coffee pot! The top of the “pot” looks to be plastic, and I’m quite certain this would react to the nitro/sulfuric acids making a mess (how did you even get the acids out?). The picture of your mix acid/glycerin solution almost appears the same color as the plastic, which makes me wonder if this was due to plastic contamination or nitrogen dioxide in the nitric acid. Also please use a sealable container and not plastic wrap! The plastics wrap can react to nitric acid, not to mention just being in proximity to nitroglycerine can cause serious headaches, and a drop in blood pressure. Safety note worth mentioning: Do not use latex gloves they combust when in contact with nitric acid (seriously violent awesome to see), nitrile gloves are poor protection, vinyl is best. Here are some pointers to follow that might help, if you used a fuming acid solution, this will increase your yield because it will facilitate water as a leaving group from the glycerin during nitration. Have you considered nitrocellulose as binder? Keep in mind, this will be a high detonation velocity depending of the nitrogen content of the nitrocellulose. In cold climates, substitute the glycerin for ethyl glycol, end product has much lower freezing point.

[Edited on 8-8-2014 by deadpool]

roXefeller - 8-8-2014 at 17:46

Quote: Originally posted by Rosco Bodine  
Urea Nitrate is a good test material for detonators because if a detonator will cause high order detonation of urea nitrate, then it will likely also be good for any other energetic material that could reasonably be called cap sensitive.
Two grams of picric acid as a base charge will usually do the job on urea nitrate that is dry and loose crystals at only a slightly settled bulk density as would occur from gently tapping a plastic container to settle the contents. Dry and untamped urea nitrate should go high order if it detonates, and if it doesn't completely detonate then the detonator is inadequate and may have to be increased to 2.5-3 gram range......depending on the quality of the detonator it will high order detonate urea nitrate in that 2-3 gram range of base charge for picric acid, and this test is a good followup to plate testing of detonators, since urea nitrate is only barely cap sensitive and requires a strong cap, it provides a good proof test for a detonator. There is a kind of parallel about the technical difficulty of getting good output from a picric acid base charge and the difficulty for initiation of urea nitrate as a secondary main charge. So urea nitrate will function as a kind of "truth test" material by which you can polygraph your work and gauge its performance.


We should quote this difficulty in initiation the next time somebody tries to claim terrorist explosives are readily available from urine. Assuming someone is so short on resources that they turn to 'urine explosives' then a strong cap probably isn't going to be acquired.

Ral123 - 9-8-2014 at 10:14

UN has very low energy but I've heard it can be set off with 2g HMTD. Also I'm not sure if it's easy to tell when the UN is completely dry, but still hasn't lost HNO3. I believe UN+NG/EGDN can make cheap dynamite with decent brisance and density(may be densities that are too high for ammonium dynamite).

PHILOU Zrealone - 9-8-2014 at 11:43

Urea is a very weak base and so Urea Nitrate (UN) is mediumly acidic while Ammonia is a stronger base what makes Ammonium Nitrate (AN) less acidic.

Medium acid is no good for NG because UN hydrolyses back to HNO3 and NH2-CO-NH2 quite easily.
This will ruin the basic wash devoted to stabilise the NG!

Good advice...don't ever store your UN/NG or UN/EGDN dynamite or whatever nitric ester with UN.
You might get spontaneous runnaway, fire or detonation of your batch...just as uncorrectly washed nitrate ester would do.:(

[Edited on 9-8-2014 by PHILOU Zrealone]

Rosco Bodine - 9-8-2014 at 16:04

Quote: Originally posted by Ral123  
UN has very low energy but I've heard it can be set off with 2g HMTD. Also I'm not sure if it's easy to tell when the UN is completely dry, but still hasn't lost HNO3. I believe UN+NG/EGDN can make cheap dynamite with decent brisance and density(may be densities that are too high for ammonium dynamite).


Actually urea nitrate does not have very low energy but has good energy, and no it can't be set off with 2 grams of HMTD, and it is very easy to tell when it is dry, and it is stable and won't lose HNO3 at ordinary temperatures. There is a simplicity and economy that is an advantage for using urea nitrate alone. The difficulty encountered is that it is only barely cap sensitive to a very powerful detonator, however once it is detonated high order it works just fine.

Ral123 - 9-8-2014 at 21:43

Half a kilo charge on the surface barely made a crater to fit a shoe. Although it was heavily beaten with a ceramic rod and felt quite dense, it went off with 15g AP. You could find pieces of the plastic jar in the smoking crater. Yes somewhat dry ,pressed UN can be a cap test may be, but I don't see it as an accurate one.

Rosco Bodine - 10-8-2014 at 03:06

Quote: Originally posted by Ral123  
Half a kilo charge on the surface barely made a crater to fit a shoe. Although it was heavily beaten with a ceramic rod and felt quite dense, it went off with 15g AP. You could find pieces of the plastic jar in the smoking crater. Yes somewhat dry ,pressed UN can be a cap test may be, but I don't see it as an accurate one.


I won't argue with your tests, methods, or opinions. There is plenty of good information published already. Used alone or in OB compositions, this material has proven to be a quite good mining explosive having plenty of velocity and heaving energy for the purpose, regardless of your tests or opinions to the contrary.

Some urea nitrate / ammonium nitrate / urea compositions are nearly as brisant as TNT and have greater total energy, but can be difficult to detonate, and 15 grams of AP does not a special engineers #16 detonator make.

[Edited on 10-8-2014 by Rosco Bodine]

Ral123 - 10-8-2014 at 04:32

I don't give UN more then R.E. 0.8, specific energy less then ANFO and whopping 4700m/s velocity. Once BP was a good mining explosive also.
TNT is something completely different. For example it can be used for a shaped charge.

Hennig Brand - 10-8-2014 at 13:51

Quote: Originally posted by deadpool  
@ Henning Brand. First good job on your success; however, I have serious safety and lab concerns with your coffee pot! The top of the “pot” looks to be plastic, and I’m quite certain this would react to the nitro/sulfuric acids making a mess (how did you even get the acids out?). The picture of your mix acid/glycerin solution almost appears the same color as the plastic, which makes me wonder if this was due to plastic contamination or nitrogen dioxide in the nitric acid. Also please use a sealable container and not plastic wrap! The plastics wrap can react to nitric acid, not to mention just being in proximity to nitroglycerine can cause serious headaches, and a drop in blood pressure. Safety note worth mentioning: Do not use latex gloves they combust when in contact with nitric acid (seriously violent awesome to see), nitrile gloves are poor protection, vinyl is best. Here are some pointers to follow that might help, if you used a fuming acid solution, this will increase your yield because it will facilitate water as a leaving group from the glycerin during nitration. Have you considered nitrocellulose as binder? Keep in mind, this will be a high detonation velocity depending of the nitrogen content of the nitrocellulose. In cold climates, substitute the glycerin for ethyl glycol, end product has much lower freezing point.

[Edited on 8-8-2014 by deadpool]


No need to worry about me, I have been making that stuff for probably about a decade now; dozens of times. :) I have considered everything you have mentioned many times. The coffee pot does have an non-ideal material for its top, but it had a very nice shape for swirling and was about the right size for the job. The same type of coffee pot is available with a glass spout and handle attached on the outside with a steel band, but the one with the plastic spout in my possession came from a thrift shop for $1-2 dollars. The orange/red color comes from the dye, or whatever was in the commercial drain cleaner I used as the source of sulfuric acid. The acid was simply poured out of the coffee pot via the pour spout. I noticed slight discoloration in the plastic spout but nothing serious. You are right that more concentrated acids, with less water, would result in a higher yield of NG. I decided to use the lower concentrated acid anyway because it would produce enough for my purposes and the gain in yield didn't seem worth the extra time and energy required to re-distill the nitric acid and/or concentrate the sulfuric acid further. I have found plastic wrap and polyethylene bags to be suitable for covering the tops of vessels containing sulfuric and nitric acids (at least temporarily). Fuming nitric acid fumes degrade the surface of the plastic over time, but it never seemed to be a cause for serious concern.

Especially when done on a small scale, a NG synthesis does not require the same precision as analytical work does. Often times, especially in small scale syntheses, saved time is more valuable to the synthetic chemist than a higher yield.

Regarding urea nitrate, has it ever been used commercially? I know it has decent power and is cost effective, but I thought it had stability and/or compatibility issues that kept it from being used as a commercial explosive.


[Edited on 11-8-2014 by Hennig Brand]

PHILOU Zrealone - 11-8-2014 at 06:21

Ammonium nitrate has higher density than urea nitrate and than nitroglycerin.
So overal density of the mix AN/NG will be higher.
But AN and NG both display a positive OB...so maybe would it be good to add some high density fuel to increase power.

UN/NG mix would have a lower density than AN/NG mix. But UN has slightly negative OB what means there exist a Perfect OB mix between NG and UN to reach optimum energy release.

One step further would be the use of nitroguanidine/NG or nitrourea/NG perfect OB mix ;)
Or even better replacing NG by ETN, XPN, MHN in the mixes to reach better performances!

Vikascoder - 12-8-2014 at 08:46

Making urea nitrate is very cheap but for detonating it u will need a powerful detonator .
Recently I made a charge of 200gm urea nitrate mixed with charcoal and packed in steel pipe of length 6 inch and diameter 1 inch detonated by2 gm rdx and 1 gm mercury fulminate detonator . After detonation it made fair noise and nothing happened to ground but no pieces of steel pipe were seen don't know where they had gone

Rosco Bodine - 13-8-2014 at 18:10

Quote: Originally posted by Hennig Brand  
Regarding urea nitrate, has it ever been used commercially? I know it has decent power and is cost effective, but I thought it had stability and/or compatibility issues that kept it from being used as a commercial explosive.


Yes I believe it has been used commercially and is mentioned at least as a component in some patent compositions. The PATR article mentions that an OB mixture with KNO3 is regarded as one of the best blasting explosives. I'm sure if money is no object anything could be used for blasting, but where the economics are governing, the cheapest useful explosives for the job will be the winning bid for the contract.

Using a double salt of urea and sodium nitrate or a double salt of urea and calcium nitrate might provide an energetic fuel value that is needed for OB in a mixture as is proposed by franklyn, as an alternative to the urea peroxide.

http://www.sciencemadness.org/talk/viewthread.php?tid=16785&...

I think it likely any of these type OB mixtures are going to have higher performance than ANFO, smaller critical diameter, and higher velocity and brisance, and will be more sensitive. These compositions are sort of intermediate between ANFO and NG dynamites......but are cheaper than NG dynamites, and are similar to tovex type water gels or emulsions in power, but even cheaper.

There are some related posts that are worth considering

http://www.sciencemadness.org/talk/viewthread.php?tid=1778&a...

http://www.sciencemadness.org/talk/viewthread.php?tid=15019&...

I'm sure there is much more.

I recall Philou Zrealone describing OB mixtures of urea nitrate and ammonium nitrate as potentially useful, and there are ways of incorporating these materials in a foamed melt cast that is cap sensitive and may be more sensitive than granular urea nitrate used alone. But even just plain dry crystalline urea nitrate when detonated completely by a powerful detonator should have plenty of power sufficient for ordinary blasting uses.

[Edited on 14-8-2014 by Rosco Bodine]

Hennig Brand - 14-8-2014 at 05:26

Interesting, thanks for the links. I have tried some of the ammonium nitrate/urea nitrate mixtures. With the mixtures I made the two components were simply dry mixed. I found a few pictures from a couple of months back where about 1kg of urea nitrate was put in an empty aluminum oxygen tank for a small portable cutting/brazing torch and used on a stump. The aluminum tank was about the same size as a handheld propane plumbing torch tank. The UN was simply funnelled into the cylinder, and the cylinder was tapped on the table every so often to settle the charge. For initiation, a well pressed 3g ETN base charge was used. It looked like a complete detonation, but the power was extremely low in comparison to even the lowest velocity dynamite. At least the stump will be fairly easy to remove now, since the earth was cleared out from around the roots and the tap root was sheared off.

When I try urea nitrate again I will use a considerably more powerful initiating charge and see if that makes a difference. Attached are three of the post detonation smoke scenes just because they look nice.


1.jpg - 452kB 2.jpg - 437kB 3.jpg - 548kB 4.jpg - 546kB 5.jpg - 523kB 6.jpg - 492kB 7.jpg - 520kB 8.jpg - 512kB 9.jpg - 520kB


[Edited on 14-8-2014 by Hennig Brand]

Rosco Bodine - 14-8-2014 at 07:46

If you used a 3 gram ETN detonator then that is more than enough for urea nitrate. I don't know what is the issue that would cause low output. Even a Kg of black powder should have done the job there. PATR gives a ballistic mortar test value for urea nitrate at 92% of TNT .....so something wierd is occurring with these anomalously low outputs being reported. From the charge you used, I would have expected the stump to be tossed in pieces high into the air and nothing left but a smoking hole where it used to be.

Attachment: Urea pages from PATR Vol. 10.pdf (1.2MB)
This file has been downloaded 623 times

[Edited on 14-8-2014 by Rosco Bodine]

Attachment: FR585671A Urea Nitrate mixture for blasting.pdf (63kB)
This file has been downloaded 871 times


Hennig Brand - 14-8-2014 at 09:23

The urea nitrate may have had questionable purity, but I have had similar results other times as well. Without supplemental heating, it can be a long & tedious process to get urea nitrate really dry. If the heating is not done very carefully, decomposition can easily occur. I used one of those glass heating trays for keeping food warm at the table. A large clear glass casserole dish was set on top of the heating tray and is what held the UN to be dried. The heating tray is rated at 250 watts, which I found is more than enough to decompose the UN when used the way it was used. I was careful to discard the material that had obviously decomposed, but the charge was likely still of reduced purity as the result of contamination produced from decomposition. The density of these charges is also very low, but you are right, they should still function better than this.

How much decomposition and reduction in purity would it take to significantly drop the sensitivity of the charge? I am guessing not very much. How much moisture would it take to significantly drop the sensitivity? I am also guessing not that much. I did have that one positive test years ago, with what seemed like good performance, that I mentioned earlier. I remember air drying the UN with no supplemental heating for several days and using 2-3g of well pressed PETN to initiate the charge in a steel propane cylinder. The only part of the synthesis that I believe I could have screwing up was the drying of the product. I wick away as much moisture as possible before drying, with large cotton towels, but even so drying is a long and tedious process. I have seen old posts by Philou at the old E&W forum where a final wash with a more volatile solvent than water was used before drying. Sounds like an option but it would increase cost.

I have since put a light dimmer on the glass heating tray, so that the heat can be turned down. I imagine this should solve the excessive decomposition problem. Urea nitrate is definitely not thermally stable and must be dried carefully. I may give it another try.


[Edited on 14-8-2014 by Hennig Brand]

Rosco Bodine - 14-8-2014 at 16:36

I did not experience any "long and tedious" drying issue with urea nitrate. It isn't hygroscopic and dries easily to a mild cake of crystals but easily broken apart lumps that results in free flowing loose glittering crystals, about like table sugar. When filtering about a kilo of the material, I filter it through a cloth from an old pillow case or dress shirt draped in a one gallon funnel, and when it finishes gravity draining, gather the edges of the cloth and twist tightly the grapefruit sized ball of crystals to squeeze out as much liquid as possible, and then place the still tightly twisted ball onto a folded several thicknesses bath towel to wick out as much residual liquid as possible. Maybe let it sit there for an hour on the
blotter and the crystals are almost dry already, then break up the ball of crystals in a large glass oven tray . I heated my tray by using a cheap heating pad like is used for sore muscles, laid on a half inch thick stack of newspapers on a sheet of plywood. Set a fan to move fresh air across the crystals and they are bone dry in a few hours. Break up the cake of crystals with a a potato masher and they fall apart easily and completely to the point you don't have to screen them, but just dump the tray into a container. So far as comparing physical properties at mild temperatures with another common crystal, urea nitrate is a lot like potasium nitrate.

[Edited on 15-8-2014 by Rosco Bodine]

Dany - 15-8-2014 at 03:28

The reason why the charge of UN made by Henning did not yielded the expected results may lie in the density of the charge itself. The charge is essentially made of loose granule of UN so it's density is fairly low. Low density+low energy explosive (UN) make a low performance explosive charge. Another reason may lie in a partial detonation of the charge. Partial detonation were unreacted explosive can be found is seen in ammonium nitrate-salts explosive, quote from [1], pp. 66:

"In a classic paper, Miron, Watson and Hay, presented experimental evidence that large amounts of the ammonium salts remain in the explosive residue left from exploded ammonium salt-explosive mixtures used as commercial explosives in a 3.7 meter diameter steel sphere with the inside surface metallized with aluminum. Up to 50% of the ammonium nitrate was recovered from the explosion residues of granular, water-gel, and gelatinous explosives while no oil was recovered. Large percentages of sodium chloride, sodium nitrate, calcium carbonate and even nitrocellulose were recovered from some of the commercial explosives. Up to 96% of the aluminum was recovered in the residue of an aluminum containing water-gel explosive."

Reference:

[1] Charles L. Mader, Numerical Modeling of Explosives and Propellants, Third Edition, 2008.

Dany.


[Edited on 15-8-2014 by Dany]

Rosco Bodine - 15-8-2014 at 07:04

That paper seems like a commentary about inadequately boosted insensitive charges showing partial detonation.
When complete detonation occurs, residues are generally only detonation reaction products and there are not even trace residues of undetonated material. Many explosives including picric acid for example don't even leave microscopic traces of undetonated material, and with a dye it is easy enough to see in the absence of color in the test chamber washdown water.

It might seem like it would be the low density and that might cause some energy reduction but not the extent of reduction that occurred. The energy of UN is good even at a loosely poured bulk density which is the same or similar uncompressed charge as would generally be used in a bore hole into which is simply poured for example loose charges of prilled ANFO. There is some drop in velocity but most of the total bubble energy of the charge weight is still realized and for a heaving earth type of work the reduced velocity is actually a benefit. For something like stump blasting it is wanted to eject the stump from its socket in the earth more than it would be desired to shatter the stump to pieces.

[Edited on 15-8-2014 by Rosco Bodine]

Hennig Brand - 15-8-2014 at 08:07

I think lately I have been doing basically everything you suggested above in terms of drying procedure, but probably not years ago when it took several days to dry the UN. The only significant difference this time, from your procedure, was that I used a more powerful heat source which resulted in some decomposition of the UN next to the glass dish. In my limited experience UN will gladly go low order if given a choice and for high output it needs to be overdriven. There are many factors which could affect the sensitivity of a UN charge to initiation and the minimum initiator requirement to achieve high output.

Rosco Bodine - 15-8-2014 at 08:26

There is a possibility that ETN used as a base charge could have gone low order and that may have coupled with a low order detonation of the UN. I have only used picric acid base charge detonators, and PA does not low order detonate in my experience if it completely detonates it always goes high order. It could also occur that a PA base has a catalytic effect towards coupling with the UN and causing it to high order also. I'm not sure what is going on with your low order and low output from UN, but I'm sure that differs from my own observation of UN.
Looking at the link where Bert showed tannerite in a small column diameter in PVC loosely loaded .....it is easy to see there is still plenty of energy developed by a loose charge....so don't make too much of charge density versus blast effect except for the more local direct contact or jet effect of close contact of cutting charges. Those are more of a microclimate localized "point contact" effect for a charge than is the larger "bubble energy" kind of blast effect as comes into play for blasting charges.

[Edited on 15-8-2014 by Rosco Bodine]

Hennig Brand - 15-8-2014 at 13:03

I am inclined to believe most, if not all, explosives can detonate with a low output if not properly initiated. From old explosives texts and my own experiments, I know picric acid can definitely have diminished output if not driven hard enough. I always thought that ETN either went high order or not at all, but I did a couple of tests with ETN plastique in the last while which showed that these types of explosives can detonate with very different velocities depending on how they are initiated (at least in small charge size). Larger charges may self accelerate to the higher velocity, I don't know.

I think the problem me and many others are having with urea nitrate is thermal decomposition during the drying process. I found an interesting article which shows that urea nitrate can be easily thermally decomposed, especially in the presence of acidity. I imagine my urea nitrate was heavily contaminated with decomposition products.


Attachment: Decompositions of Urea and Guanidine Nitrates.pdf (211kB)
This file has been downloaded 1163 times


Here is an interesting table from the appendix of the report.

Catalytic Decomposition of Urea Nitrate.jpg - 34kB

I would have liked to have seen results for lower temperatures.


[Edited on 16-8-2014 by Hennig Brand]

Rosco Bodine - 15-8-2014 at 14:06

1 kg of UN should have tossed that stump the same distance as a pair of 1lb blocks of TNT. Why that did not happen I'm not really sure. You already know how difficult it is to get picric acid to detonate fully and it is a lot worse for trying to detonate TNT which is even harder to detonate......and urea nitrate has about the same sensitivity as TNT. So it could be that it isn't being overdriven enough to get it to go. You don't want the UN to be powdered but just plain crystals loosely poured and only gently settled, as the more densely it is packed the less sensitive it will become, and it is already difficult enough to detonate. However, so is TNT difficult to detonate, and a lot of other relatively insensitive explosives, which once they do get going have good energy.

Hennig Brand - 15-8-2014 at 21:28

I appreciate your insight. I am going to give UN another try in the next while. I really think it has been my impatience with drying that has been the biggest problem, but I will need to test that out to know for sure. 

Rosco Bodine - 16-8-2014 at 04:18

Here is a video of a UN loose charge in an open plastic bowl reportedly 700 g UN
as an example ......not my video but this would appear to be about right. I'm not sure what is the development concept of the particular booster mix and detonator, and it may have just been a trial and error kind of approach. I think a hot enough detonator should give similar results in a simpler configuration. A loose charge is as simple as it gets, pour it in a ziplock bag or an empty plastic pop bottle and shoot it. From the video you can see the blast effect for a loose charge is considerable, given the time delay for the falling debris, one piece of the tire was blown est. 500 feet or more straight up into the air. That same charge in the earth underneath a stump should I think have been plenty to do the job of convincing that stump to jump out of the ground. So a full 1 kg like you were using with confinement of an aluminum cylinder would seem to have been plenty.

https://www.youtube.com/watch?v=5SpTofaUY0I

<iframe sandbox width="640" height="360" src="//www.youtube.com/embed/5SpTofaUY0I?rel=0" frameborder="0" allowfullscreen></iframe>

Hennig Brand - 16-8-2014 at 05:32

That looks more like it. I am going to use a more powerful detonator/booster the next time I try it. I get so used to initiating dynamites, which can be initiated with the weakest caps, that it clouds judgment when it comes to these more insensitive materials I think. I need to learn to be more generous. :)

Rosco Bodine - 16-8-2014 at 06:38

Mud capping the charge, or wetting and packing the earth in the bore hole after charge placement could also help if the blast is escaping through the loose dirt and force is being lost mostly blowing around the target instead of against it. A fence post hole dirt auger would be handy for boring under a stump. Set the charge and then dump a bucket of mud atop the charge in the bore hole to mud cap it before firing.

z13123 - 20-9-2014 at 20:06

First time making NG I used:
2mL glycerin
8mL HNO3 distilled from KNO3 and H2SO4
12mL 98% H2SO4
washed many times with water, then baking soda, rinsed in NaCl solution after it was neutral, rinsed again with water, extracted, and did a flame test, it took a while for the water to boil out (I didn't dehydrate it) but it burned very very quickly with a poof and a blue flame appeared. I burned the rest of this solution because I felt it wasn't worth the effort to dehydrate it. I yielded around 3mL of NG.

Next, I went larger scale, with the same proportions and 25mL of glycerine. I yeilded around 40-45mL before dehydration. I have not yet finished dehydrating it. It was very cloudy and milky looking, but after sitting in a box with silica gel on the bottom of it for half a day, it looks clear, but with a slight yellow tinge still.

I was reading through the pages in this discussion and someone mentioned not using a stirring rod. I was using a glass stirring rod and was wondering if this was an issue and if it could detonate the NG while washing/mixing. Also, because I don't have a separation funnel (I know... I should get one), I used a syringe to suck out the NG, and squirted it out into water to wash it. I noticed while doing this, some of the NG (looked oily-like) floated to the top. Any ideas on how to prevent this/what it is? Also, any ideas on the best temperature to store it? Should I freeze it in my fridge or just keep in a room temperature place? Also, thoughts on using a black powder charge to detonate it? I don't have AP, PETN or any common blasting caps available.

NeonPulse - 20-9-2014 at 21:18

Um, I probably shouldn't spoon feed you here but this is pretty dangerous stuff here so ill help with an answer other than utfse.....Why did you make it without a means to detonate it?
Glass should be avoided as a hard clink on the beaker could be catastrophic. With 25mls it would likely kill you. Black powder was what they ward in the old days but it works, not well but it does, and you won't be making the most out of your NG.
since you made the nitric acid you should be able to devise a way to a primary. Use it up and avoid storing it as it doesn't keep well. Did you test with PH paper? It MUST be neutral or it is incredibly dangerous to store. There is stacks of info on this stuff all over the internet. It would be wise to research it some more before something bad happens. NP

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