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Author: Subject: pearlescent ETN?
Thanatops1s
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[*] posted on 17-8-2013 at 16:02
pearlescent ETN?


So I synthesized a few grams of ETN last night and recrystallized today. This is the second time I've done it and ever more so than last time, the crystals are very pearlescent and shiny with very small but visible needly crystals. Everyone elses I've seen looks to be more a flat white. So I'm wondering if there's anything wrong with mine? Unfortunately my only camera is my phone so this is the best pic I can offer.

etn.jpg - 273kB
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NeonPulse
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[*] posted on 17-8-2013 at 17:27


In the past mine ended up looking the same as this, actually it was my 1st Etn synth. I thought it was because I used cold ethanol to recrystallize it with.different solvents will give various crystal formations.the plate like forms are my favourite as you can pack them fairly dense. I don't think they're a problem like that, but I guess if it bothers you you can always recryst it again.as long as its neutral and has the correct melting point temp as well as the hammer and foil burn tests do well, I think its fine.



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CaliusOptimus
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[*] posted on 17-8-2013 at 17:44


Just a friendly heads up... that ETN is rather impure and won't be storage stable. Recrystallized from denat EtOH or other? ETN made with a nitrate salt tends to be that yellow color, but made with WFNA is very white after one recryst.
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Thanatops1s
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[*] posted on 17-8-2013 at 17:53


Quote: Originally posted by CaliusOptimus  
ETN made with a nitrate salt tends to be that yellow color, but made with WFNA is very white after one recryst.


Yes, it was made from ammonium nitrate & sulfuric. However my distillation apparatus will be ready to go soon, just waiting on another ring stand and some clamps. Soon after I will distill some WFNA.

Recrystallization was done with 99% isopropyl. It was what I had on hand so I thought I'd give it a shot since I figured re-recrystallizing is always an option if the results were unsatisfactory. I was going to grab some denatured EtOH tomorrow or Monday. I have to say though, part of that is the lighting. It's not nearly as yellow in person. Compared to the last time, it's amazingly light and fluffy as well. It very much reminds me of the lightest fluffiest snow you can imagine. Now that it is fully dried too, average crystal size appears to be about 1-1.5mm little needles.

I'll be going to a friends who has a bunch of land in a couple days to test a gram or two, only made 6.

[Edited on 18-8-2013 by Thanatops1s]
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golfpro
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[*] posted on 17-8-2013 at 20:34


Calius that would be incorrect

My ETN is pure white, like snow after recrystalization, no slight hint of yellow and I use nitrate salt, I use pure ammonium nitrate.

But a full solution of ETN in ethanol is dark yellow.


ETN is not storage stable? What about in a sealed container completely dry, neutral and recrystalized clean in total darkness sitting at 65*F? 2 Months?
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[*] posted on 18-8-2013 at 01:08


Quote:
What about in a sealed container completely dry, neutral and recrystalized clean in total darkness sitting at 65*F? 2 Months?

Impure ETN is not stable and should not be stored for any length of time!




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golfpro
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[*] posted on 18-8-2013 at 05:44


Pure, Pulverescant...
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Rosco Bodine
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[*] posted on 18-8-2013 at 06:08


Pure and stabilized it is probably good for 6 years even under less than ideal conditions outdoors. Refrigerated it could probably last 3 to 10 times that long.
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Thanatops1s
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[*] posted on 18-8-2013 at 08:43


Well I did another recrystallization and it has the same texture, but is completely white now.

While the alcohol was still hot, I noticed some insoluble matter so I filtered it; then it was totally clear with a slight yellow tint. I crashed it into a bunch of cold water with a little NaHCO3 just in case there was any acid that made it through my first neutralization and washes(there didn't appear to be any). Immediately a big bright white cloud precipitated. It's filtering now.

After filtering and a final wash, it's drying now and it seems like the needles are no more as well. I'll take a pic when it's dry to see what you guys think.

Here it is now, not totally dry though, and any hint of color here is just the picture, it's white as can be.
[Edited on 18-8-2013 by Thanatops1s]

2013-08-18_14-52-35_482.jpg - 245kB

[Edited on 18-8-2013 by Thanatops1s]
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golfpro
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[*] posted on 18-8-2013 at 09:08


I have melted the ETN in the ethanol by accidentally letting the ethanol get too warm, could this be dangerous if the liquid ETN settles on the bottom while it's stirring? Is it of any use to melt ETN in ethanol? I guess the ethanol couldn't dissolve any more ETN...
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Thanatops1s
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[*] posted on 18-8-2013 at 10:48


Quote: Originally posted by golfpro  
I guess the ethanol couldn't dissolve any more ETN...

Others can probably tell you for sure, but if you just didn't use enough EtOH to dissolve it all, I don't see why you can't just slowly add more until it's all dissolved.
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[*] posted on 18-8-2013 at 19:31


Because I was out and the beaker wasn't big enough.

Someone in my other thread which got closed told me a cast booster can be made very similar to pentolite (TNT/PETN) whatever ratio that may be but substitute ETN in that mix?? TNT has a higher melting point than ETN so this would seem like it could become a problem, just as much as dealing with melting ETN and pouring it or whatnot in it's most sensitive state.

I'm not worried about the synth of ETN or the recryst anymore, I have plenty ETN now, plus it's a huge pain for what it's worth to make, and only fun the first time.
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