golfpro
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Poor performing ETN
Hi,
So I have made 3 batches of ETN in all of my life. I yeild about 10 grams on average, which that's alright, I don't need stockpiles of it. My first
batch I detonated about 2-3 grams by heatshock, the detonator was a thin bit to be heatshocked about .1g on top of some packed 2-3 grams ETN. I
actually detonated this on the backside of a curb in the street. It was fairly loud, but not much louder than the standard aerial fireworks you go buy
at the stands. Well, I made another batch, but it was only 6 gram yeild, it was a slightly different procedure, I let it nitrate for longer, BTW, all
times it is recrystalized from Denatured alchohol, which is 90% ETHANOL. I had 6 grams of those shavings, I decided I wanted more so I did another
synth. and got approx. 12 grams, this was recrystalized from pure Ethanol like the other times, only I then recrystalized it all by first disolving it
in warm ethanol, then dumping this in cold water for more of a powder material, but still dense, won't blow away
Well, I can get about .3 grams pack it in some Al foil and hammer this and not even get ringing ears and without ear plugs,. I'll try detonating
around 5 grams of it later on, but I didn't know if it is possible I have a mix of ETN and unnitrated Erythritol? So basically an impure product
maybe? It is rather unimpressive
I can give my procedure in a brief description:
120ml 93% Sulfuric (Drain Opener) I add 60 grams recrystalizd and dry AN powdered, this is completely disolved, This goes in the freezer and cools to
20*, I add about .5-1 gram of Erythritol at a time and stir a LOT I add 20 grams Erythritol (Truvia Sugar) Takes about 30 minutes, I let this sit at
room temp for 45 minutes then dump this "pudding" into cold 500ml water, it instantly precipitates, I stir very hard to dry and disolve any unwated
stuff, and then filter, rinse 4 times, dump into sodium Bicarb water until no more reaction of the sodium bicarbonate. I filter the neutralized stuff,
and let it dry for a little bit as I prepare 150ml Denatured Alcohol, heat this with boiling water bath (away from flame) and disolve all of the
product, cool in the freezer to precipitate it all out, and then filter these shavings, My ETN is almost pure white when finished, it has a slightly
sweet smell for some reason, but that may be just me.
Like I said, I would comfortably hammer a little less than a teaspoon (approx .2 grams) without ear plugs and be just fine
Maybe my expectations are too high? I'll do one test when I can use my silver Acetylide DS cap, with 5 grams or so packed, maybe take video.
Any Ideas? I can't imagine that the powdered erythritol would precipitate out in the water along with the ETN and then not disolve?
[Edited on 25-7-2013 by golfpro]
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Hockeydemon
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I don't think your expectations are too high. I am skidish about igniting 2 rice sized flakes of the stuff wrapped up in tin foil because it haha. It
startles me every time. It definitely makes my ears ring too.
I would guess it is your materials, and not your method. If you can get your hands on 'Rooto professional drain cleaner' (Ace Hardware carries it
here) it is a little over 18M (97%) sulfuric acid, and is very clean looking. I've never used AN powder as I make nitric acid, but I would guess this
is probably another pitfall as I really followed almost the same method. The only exception is I didn't bother recrystallizing because I don't want to
keep the stuff at all.
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Bot0nist
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Ammonium nitrate works well for a salt acid nitration of ethyritol. If you are in the states you can order tech hrade sulfuric acid from onlime with
no problems. Rooto brand is really good though.
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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golfpro
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I'll maybe try Rooto as a last resort, so it is possible that what I have isn't pure ETN? Even if it was recrystalized?
If that's the case, I'll just stick a cap in all 16 grams I have now and get rid of it, maybe that will be a nice noise, it's hammer sensitive and
deflagrates smoothly. However, when it's hit with a hammer, some powder remains on the hammer, like there is some inert contamination, I don't know
how in the world that's possible. .
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Bot0nist
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I doubt it. When i do impact tests some is always left behind undetonated.. 16 grams will make a noise alright...
U.T.F.S.E. and learn the joys of autodidacticism!
Don't judge each day only by the harvest you reap, but also by the seeds you sow.
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energetic.material
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Could your AN possibly have impurities? Not positive but i think instant cold packs may have some anti-caking agent that is difficult to filter out. I
know that in order to get a more pure product you can dissolve it in water, filter, than evaporate or reheat in the oven. The anti-cake is usually
yellowish if this helps.
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golfpro
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My AN is from cold packs, it is disolved completely in water, filtered the filmy, anticaking stuff, and then boiled down to about half of it's volume
and then the water is allowed to evaporate in a warm oven, the end product is white.
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Fantasma4500
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for how long and where did you dry the etn
also the 0.3g was it confined very well or not very well confined
also how and where do you dry the etn?
10g from 120 mL H2SO4 doesnt actually sound like a good yield really.. 120 mL H2SO4 in only 500 mL water, doesnt that heat up alot, creating sudden
run off?
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plante1999
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I believe truvia sugar is some sort of leaf extract, that is what sound most problematic to me.
I never asked for this.
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watson.fawkes
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The product
Truvia is a glycoside extract from the stevia leaf, which has very concentrated sweetness, so it uses erythritol as a carrier. I believe they're
co-crystallized. As plante1999 said, it's anything but pure erythritol. (Specifically, they use the rebaudioside fraction of the stevia glycosides,
but not the steviosides, which are the ones linked to adverse health effects.)
Now there are artificial sweetener products that are just erythritol (and others that are just xylitol), but you'll have to locate an appropriate
brand name available to you.
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golfpro
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I wonder if the reason for my poor yeilds is my lower conc Sulfuric acid (93%) or if it's that my erythritol isn't very pure?
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plante1999
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Erythritol for god sake. Can't you read? 93% H2SO4 is well enough.
I never asked for this.
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watson.fawkes
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Oh, I'm sure he can read just fine. What he can't do is to take your word as unfailing
authority.
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golfpro
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The main ingrediant is still erythritol in the Truvia brand, I couldn't imagine it could be much different than the erythritol sugar from other fancy
brands, which I do not have access too.
I also didn't know plante1999 if you were saying the impure erythritol was causing lower yeilds or lower purity of ETN lowering the performance, 5
grams handpressed slightly still took a chunk of cement out of the sidewalk.
Specify what you are saying plante1999.
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