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Grantr
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biggrin.gif posted on 11-10-2015 at 16:41
ETN success


I made a batch of ETN following the 2006 notes from Quicksilver. I used pure Erythritol, clean shot drain opener and fertilizer grade AN. The acid is red in color and the ETN turned out white.

I ground up the E and AN with a morter and pestal to fairly fine power. I did not dry the AN I just ground up the prills with a blender then milled it.

I measured out the 110 ml of sulfuric and added to a 250ml beaker in an ice bath. The acid temp was 18 C when I started adding AN. White fumes rolled out when the acid was added. The fumes were very acrid. I assume this is nitric acid. I added the AN a little to fast at first and the temp rose to 25C. I waited and kept stirring and the temp went back below 20C. It took a little while to add all of the AN.

After all of the AN was added I let the temp go down to 15C before adding the E. Too my surprise adding the E did not cause a rise in temp. I started with very small amount and continued until the 20 grams were all added.

After all of the E was added, the mix had become thick like light syrup. It had the color of egg custard and similar consistency. Blowing on the mix gave off white fumes. I stirred it frequently during the hour rest time. The temp never rose. I even removed it from the ice bath one time due to it getting down to around 12C.

After the hour was up I slowly dumped the mix into 400 ml of water. Not slow enough. The temp rose to 45C. I should have used ice water. I used ice in the mix to cool it down some and then I poured it through a paper towel filter. The Acid in the water was still too strong and discolored and ate a hole in the towel. I doubled up on my towels and was able to filter the 2nd time. I then again dumped the ETN in another beaker of fresh water to cut the acidity down some more and filtered again and uses baking soda solution in a spray bottle to neutralize the ETN.

Once neutralized, I spread the ETN out on wax paper to dry. That took too long so I scooped up some and rolled it up in a paper towel to dry it. That worked well. The ETN was still a little damp but it worked.

Hammer test gave a nice pop. I took some larger quantities and pressed them tightly by hand and rolled the pressed mass of ETN up in Aluminum foil. I put the foil pack on a open flame of coleman fuel burning in a tuna can. About 2 mins after sitting in the fire there was a loud crack like a high powered rifle. Small amounts of the stuff are quite impressive. The size of the pressed ball was only the size of a jelly bean. I would compare the noise to a 308 rifle.

I did notice the ETN would only pop to fizz when it was loosely poured into the foil. When the ETN was pressed as hard as i could by hand into the foil then wrapped up It would produce the very sharp bang when heated in the fire.

Overall I had a great success. I did not weight the final product however it made a lot more powder than the E I put into it. I did not recrystallize since I am not storing it. Under a 100X microscope, I do not see any needle shaped crystals. They seem to be more flat shaped.

My biggest problem was trying to filter the product. I used heavy blue shop towels which work well when the acid is not too strong. Do you guys have any tips for a better way to do the initial filtering? I had though about adding baking soda to the water prior to pouring it over the paper towel.

What method do you guys used to dry the product and how long does the method take?
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Hawkguy
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[*] posted on 11-10-2015 at 17:00


Congrats, good work. Try recrystallizing the ETN to see if you can get better needles. Otherwise maybe you might have a lower nitrate?
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OneEyedPyro
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[*] posted on 11-10-2015 at 19:52


Nice, ETN was my first and remains my favorite HE.

Drying times will vary depending on humidity, temperature, the consistancy of the ETN, how much is there, how well you wring it out, what it's sitting on etc etc, it could take overnight or over a week. I like to wring it out in a coffee filter then break the lumps of ETN up and spread it out before placing a second filter over the top and using paper towels on both sides to squeeze out whatever remaining water I can.

For a filtering setup I like to take a round plastic food container 4.5" in diameter by 2" tall and poke it it full of holes with a hot screw driver or something similar, these will fit a coffee filter perfectly and are nice because you can make a bunch of them if you have to filter a large quantity of liquid. You're just going to have to use more water when diluting your acid, this will eliminate the heat problem and stop it from eating your filters but you will of course have more water to filter off.



Even if you don't intend to store your ETN you really should recrystallize it since it decomposes very quickly and can behave differently when crude.
All you have to do is put an alcohol of a fairly high strength (80%+) in a jar and place it in a pot of simmering water, wait until the solvent begins to boil then slowly add your ETN with lots of stirring to make sure it doesn't settle on the bottom, now dump the solution into 10x or more the volume of cold distilled water while rapidly stirring. You can optionally add a couple % urea and baking soda in the water for extra stabilization.
With this method you will see a very minimal loss of product and get an acceptable level of purity, isopropyl alcohol works just fine if you don't have access to methanol or high proof ethanol.

[Edited on 12-10-2015 by OneEyedPyro]
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Grantr
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[*] posted on 12-10-2015 at 04:35


Hawkguy,
I think it is ETN. It is powerful. The product has no smell to it and feels kind of like baby powder. It does have a unique smell when it goes off.

OneEyedPyro,

All of those alcohols boil over the melting temp of ETN. ETN melts at 61c. Does that seem to be a bit hot to recrystallize?

Will diesel exhaust fluid Urea work?
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hissingnoise
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[*] posted on 12-10-2015 at 05:18


Quote:
All of those alcohols boil over the melting temp of ETN. ETN melts at 61c. Does that seem to be a bit hot to recrystallize?

The hot, melted material will have much increased sensitiveness ─ so use sufficient ethanol to dissolve @ ~50°C or cooler?

And you might benefit from reading this thread?
http://www.sciencemadness.org/talk/viewthread.php?tid=22554#...

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OneEyedPyro
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[*] posted on 12-10-2015 at 05:42


Any lower nitrates would have dissolved upon crashing so it could only be ETN.

As long as you add your ETN slowly enough and stir as not to allow the ETN to pool at the bottom of the container it won't be an issue, the temp will drop as you add the ETN anyway. I have noticed you get little clumps of ETN upon crashing if you have it too hot and pour it in too quickly, I find it's best to stir the urea/baking soda solution so that it's swirling then slowly pour in the ETN solution in a circle opposite the flow of the water (if that makes any sense) this helps to keep the ETN from clumping upon recrystallization.
Of course there's no reason you couldn't do it at 50C if it makes you feel any better :P, I don't feel it makes much practical difference in the end but safety first, I was just sharing my personal method that has worked for me.

I've always used urea from instant cold packs, it's cheap and quite pure. I'm not really sure what exhaust fluid urea is.

[Edited on 12-10-2015 by OneEyedPyro]
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Grantr
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[*] posted on 12-10-2015 at 09:25


Hissingnoise,

I read that thread a few weeks ago. That is why I am concerned with the temp of boiling alcohol.

OneEyePyro,

What does the urea exactly due chemically to the ETN to stabilize it? How does that work?
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[*] posted on 12-10-2015 at 10:02




Quote:

What does the urea exactly due chemically to the ETN to stabilize it?


Urea is basic in sol. but who doesn't have sodium bicarbonate . . . ?

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Joeychemist
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[*] posted on 12-10-2015 at 15:05


The idea of using urea as a stabilizing agent has been well documented, Urea reacts with nitrous acid to form nitrogen and carbon dioxide. A better choice would be diphenylamine as it will show a blue color in the presence of the acids.
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[*] posted on 12-10-2015 at 18:31


There's a big difference between the method I suggested and what Yamoto did. He directly heated a non pyrex container containing a solution of methanol nearly saturated with ETN which then broke and caught fire, it had absolutely nothing to do with the temp at which he carried out the recrystallization and not to bash him but he was practically asking for it.
Simply using a double boiler setup would have prevented it from ever happening.

I'm not sure why people seem to think ETN turns into nitrogen triiodide once it melts but my testing indicates that ETN at 65C is measurably less impact sensitive than NG.

[Edited on 13-10-2015 by OneEyedPyro]
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Grantr
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[*] posted on 13-10-2015 at 05:19


I was able to scrape up a nice pile of ETN off of my wax paper after the residue had dried. I did the hammer test with great success. Loud pops that removed some material from my vice!

I proceeded to roll up the rest into aluminum foil and put it in the fire. All I got was a woof! I tried agin with a much smaller amount and got the same result. That sucked.:(

The problem was I was not able to compact the ETN into the foil when it was completely dry. So all I wound up with was loose powder in the foil.

Dry ETN feels somewhat like cornstarch and leaves my finger with a white residue. Somewhat slick feeling powder that will not compress without solid confinement

Anyway the successful tests involved wet ETN that was prepared by rolling it up in a paper towel to ring out the excess moisture. That leave a slightly damp product that was easy to press into a hard mound on the flat piece of foil. The foil was simply warped around the mass and tossed into the fire and then boom!

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OneEyedPyro
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[*] posted on 13-10-2015 at 23:12


Pure ETN should take a few firm whacks to set off especicially when in a fine powder.

In my experience acid impurities often cause ETN to deflagrate rather than DDT, you should have recrystallized it :P

Just out of curiosity roughly how much did you yield?
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[*] posted on 14-10-2015 at 16:05


I am not sure how much it made. It was a pile of it about twice as large as the E I mixed into the acid. I was surprised by the amount of it as i didn't expect that much to come out.

I still have some very small amounts of residue around on the wax paper and it is still white, doesn't smell and pops with a firm hammer blow. How long does this last without recrystallizing? So far 3 days.

Does the ETN need to be completely dry before recrystallization?

Before I make it again I will get some denatured alcohol to recrystallize the next batch. The Klean Strip brand is 45-50% Methanol. Jasco is 52 to 55 % methanol.

I noticed these have very small percentages of other chemicals in them so are they fine to use? I have seen reference to denatured being used.
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[*] posted on 15-10-2015 at 00:17


It may appear white at a glance but when compared to a piece of paper I bet it will look an off white/cream color, it should look glittery virgin white when recrystallized. It will likely also look reddish when you melt it instead of clear

How long it lasts will depends on on the individual batch and how well you washed it, if kept in a sealed ziplock baggy it will slowly inflate due to decomposition gasses and you'll be able to smell the NO₂.

It doesn't need to be dry to recrystallize it but the more water there is the less that will dissolve per amount of solvent so it's good to get it as dry as possible.

I'm sure Kleanstrip denatured alcohol will work fine although the type of recrystallization I suggested works with many solvents, having trace amounts of denatonium benzoate isn't going to hurt anything. I've used 91% isopropyl alcohol many times.
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hissingnoise
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[*] posted on 15-10-2015 at 02:52


Quote:
It will likely also look reddish when you melt it instead of clear.

The red colour is evolved NO2 and it means the ETN is in a very dangerous condition ─ pushing your luck in this way will likely lead to "lifechanging", (or worse?) consequences . . . ?

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[*] posted on 15-10-2015 at 04:04


My point exactly although melting less than 100mg on a piece of Al foil isn't likely to do much more than ring your ears if it does detonate.
Recrystallizing your ETN is (in my opinion) an absolutely essential step no matter how soon you intend to use it, that's what I'm trying to stress here.
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[*] posted on 26-10-2015 at 05:57


I had another successful batch of ETN following the same method as before. I did make a few changes I cooled the acid in an ice bath prior to adding the AN. It wound up getting to 10c. This helped speed up the process some. I also used a small fan to disperse the acid vapors. I did not smell it so that worked well.

My biggest issue is filtering the product. I spent way to much time trying the do this using the beakers. 2 plus hours. Yea! Well it was a learning process and I think I came out ahead.

My solution is using a plastic 5 gallon bucket with 4 gallons of water! I have 125ml of nearly pure mixed acids so dumping that into 15,141 ml of water makes the entire solution have less than 1% acid concentration. This gives some advantages, One I can wash out my beakers very well in the water to get all of the ETN out and two I can use my bare hands without getting burned. Baking soda could be added to the wash water to neutralize the raw product as well.

Most of the ETN sinks to the bottom. I did have some floating that would not settle. Hammer test did set it off so I am not sure why a very small amount floats. The amount floating in 4 gallons was not worth the effort to filter it off.

I did drill holes in a plastic food container and used a coffee filter to filter the ETN. That worked well as the filter did not fall apart. I am thinkg of using a cheese cloth next time so I can squeeze out the excess water to speed of the drying times.
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hissingnoise
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[*] posted on 26-10-2015 at 09:00


'Time for a pack of whatman, what?

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Grantr
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[*] posted on 26-10-2015 at 10:04


The coffee filter actually drains quick. I need to drill larger holes in my food container. Whatman filters might drain faster? A vacuum filter would help dry it faster.
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[*] posted on 26-10-2015 at 18:08




Attached is a pic of the results of my recrystallization after I let the alcohol/ETN solution cool to 15C in the freezer. I poured it through a coffee filter. I think the yield looks decent.

I used denatured Alcohol to recrystallize. I heated the alcohol to 55C in a water bath on a hot plate. I stirred it with a wood spoon.

Can the old alcohol be used again for a new recrystallization?

I started with 200 ml and wound up using 800 ml. The 200 would not dissolve all of the clumps. The alcohol took on a yellow tint as it dissolved the ETN. The mix stayed cloudy while warm but I did not see anything settling on the bottom of the beaker.

Does 800 ml seem like too much to dissolve an estimated 40 grams of ETN?

20151026_215855.jpeg - 902kB

[Edited on 27-10-2015 by Grantr]

[Edited on 27-10-2015 by Grantr]
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[*] posted on 28-10-2015 at 14:43


It looks like my dry recrystallized yield is going to be only 20 grams.
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