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Author: Subject: ETN lower nitrates
Ral123
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[*] posted on 30-6-2012 at 05:17
ETN lower nitrates


Here's dmg pics from 5ml egdn http://imageshack.us/g/861/dsc00129tq.jpg/
here's a video with 5ml cast etn with little dnt/tnt
http://www.youtube.com/watch?v=kdDbO3L3Y0A
here's a video of 5ml etn powder with some egdn, to help with density
http://www.youtube.com/watch?v=LDZS7i8-pxE
Obviously something is wrong with my etn synth. I used a bit little H2SO4, it looked like the eritiritol particles didn't really dissolve. But I washed with water well. Then dried the product, then dissolved in hot methanol. I let it cool slowly and bout 1/3 of the initially dissolved product crystallized out in needle shape. Maybe I've got lower nitrates that don't dissolve in water well, I don't believe that etn really sucks that much.

[Edited on 30-6-2012 by Ral123]
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quicksilver
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[*] posted on 1-7-2012 at 10:10


I think you called it. ETN is very close to MHN in many ways and a well- nitrated 5mg sample should make a damn loud pop. Often initial materials are not up to lab level quality. Most all H2SO4 (from drain cleaner) is surplus that MANY different companies sell off to maintain profit / loss margins. Often it's from metal treatment facilities & contains more (and more) impurities.
Classical needle shape for upper nitration (in ETN) is platelet shape. Study the "November 20" patent. I have distilled HNO3 more often than simply used a mixed acid and found the problem to be lower levels of nitration (via time or acid quality) or impurities.



The patent is posted several times on the Forum or I'd post it again. Do a "Search" for "ETN, patent" & you should find it.

[Edited on 1-7-2012 by quicksilver]




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[*] posted on 2-7-2012 at 00:31


Hi,

just wash your etn with lots of warm water, it will remove the lower nitrates. If it's completely insoluble, you got the real stuff.

Needle shape is OK, I've got that too.

And I cant (how did you do it exactly?) recommend casting, besides from it's dangers it's harder to initiate. Better carefully press (not ram) it.


Quote:

I don't believe that etn really sucks that much.


I can only speak for etn without additives, and that stuff kicks ass.

[Edited on 2-7-2012 by dangerous amateur]
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Ral123
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[*] posted on 2-7-2012 at 03:02


I guess I'll use more sulfuric next time. Can HNO3 distilled with aluminium pipe have any issues btw? Strangely, the product is quite hammer sensitive, burns like it's about to blow if the quantity is more then few drops. I poured the methanol solution in twice the volume very weak ammonia water. It turned brown, I can't explain that. Why would you guys use non oxygen balanced ETN? DNT/TNT and ETN aren't miscible, would it dissolve RDX I wonder. Just pressed powders don't get near their maximum density I think, so I prefer either melt casts or adding a little egdn/ng.
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[*] posted on 2-7-2012 at 08:35


The significance and utility is often used in a train-mechanism. That the material energizes well from impact initiation indicates that it's most likely appropriate. There is a substantive difference between HE materials and flame set utilities.
Generally, darkened H2SO4 from anodizing or pickling does have to left over metal within it but if you're getting impact sensitive material then the adulterant may have limited impact. One of the greatest problems I could think of is the rise of friction via the adulterant itself.
Frankly, I would not continue with adulterated acid. Simple heating will drive the metal adulterant to a layer.




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Ral123
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[*] posted on 2-7-2012 at 11:09


If the product is the highest nitrate, I hope recrystalization will suffice to give high purity product. Do you know of any rdx-like products given from nitrolisys of hexamine?
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[*] posted on 2-7-2012 at 15:14


When you use the term "hexamine" I would take a leap and suggest and think you mean cyclic-nitramines. The use of nitrourea to synthesis DPT is perhaps the least complex but again you must have some glassware. Solex is not particularly difficult & from there - there are several HMX synthesis yet they also demand acute temperature control and many require phosphorus pentoxide. A simple nitramine could be Tetryl. But the precursor (dimethylamine) is generally not too expensive and VERY easy to synthesize; it's just not too easy to find.
The demand for careful sulfonozation is very important (but Tetryl is a very easy to synthesize material). A "Search" will turn up both. But while urea nitrate has a very stable shelf life nitrourea is more demanding.

Many energetics are simple to synthesis but demand much more than a kitchen-labratory & should never be even conceived of in a rush toward completion. A proper distillation rig, digital Ph meter & scale should be as important as several lab text books in their utility & value.



[Edited on 2-7-2012 by quicksilver]




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Ral123
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[*] posted on 2-7-2012 at 22:53


My point was, is there a chance that I get some unpredictable product from hexamine and nitric, like it happens with ETN? Can I expect that tetryl unlike tnt and can be made as easy as picric acid? Can you give a link to a useful HMX synth, I always wanted to make a little, but I don't have acetic anhydride.
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[*] posted on 27-7-2012 at 15:28


I now did some etn again. I used 50ml nitric, 100ml sulfuric and 30g ball milled eritritol. So far my product looks a bit like my last one. Is it possible that the ammonia I use to neutralise takes some nitrogroups? I've heard ammonia is too strong base from such neutralisations. Do you think impact testing would distinguish well the poorly nitrated one from the good one?
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[*] posted on 28-7-2012 at 06:08


Have you checked the melting point? Sharpness of melt at the correct temperature is at least one indicator of a fully nitrated product vs a mix of lower nitrates.

If in doubt about the ammonia, try good old bicarb.
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[*] posted on 29-7-2012 at 02:45


http://www.youtube.com/watch?v=Djpni2Lhehg&feature=youtu...
Here's the effect from the carefully nitrated etn batch. I'm wondering if it's more powerful then rdx-ng mixture.
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[*] posted on 9-3-2013 at 15:08


I did another batch ETN. I used erythritol/WFNA/H2SO4 1:3:6. I added erythritol first as granules and then as fine powder. At the end it was imperfect crystals/particles. I dried them and recrystalised from methanol. I got a large volume of very low density needle crystals. I filled Al pipe with them(hand pressed). Threw it in hot water(to melt it) and the volume decreased, like two times. The little pipe nicely gained quite a weight :D The test however makes ETN to appear not much more powerful then TNP.
http://youtu.be/Gxii54xvRPc?t=1m7s
http://youtu.be/E97QGKzjwAE?t=43s //the dent is similar in depth
Should I nitrate at higher temperatures-25 instead of 20? If I can't get the true product with excess of H2SO4 and WFNA, I wonder what product do the guys with KNO3/AN methods get. I'd say EGDN is somewhat more consistent in that regard.
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