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Author: Subject: ETN synthesis issue
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[*] posted on 24-10-2013 at 06:59


Stirring with a glass rod is not the safest manipulation for a sensitive nitroester

It does not stirr very effeciently with these glass rods anyway, but I never found something better - there are spoons made from PTFE, but they cost a fortune.

Have you guys ever found something else that resists the nitration mix and stirrs better? I mean something ordinary people have at home?
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underground
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[*] posted on 24-10-2013 at 09:35


Does anybody know any ETN plasticized formula, i was thinking something about ETN/NM/FLOUR. Will that work ? Or ETN/WAX/VASELINE...
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[*] posted on 24-10-2013 at 14:53


Okay, plenty of these replies are going off track. Underground, do you know that you can make your own threads for the questions you're asking?

Anyway... I've seen people stir their ETN mix using a kitchen mixer, so if glass rods are considered rolling the dice, then I don't want to know what that would be considered.

Would anyone happen to know if letting the bisulfate settle and harden at the bottom of the beaker has an adverse effect on the process? Or should the bisulfate be constantly agitated and broken up? Since the potassium bisulfate chunks i've experienced are too hard to break up into smaller pieces, I let them be while exclusively stirring the liquid portion of the mix. Could this have been the reason for my failed experiment?
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golfpro
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[*] posted on 24-10-2013 at 15:58


stirring with a glass rod is annoying and takes a lot of effort. I am also looking for a replacement. Maybe a regular plastic spoon?

underground, you just have to play around with mixes. I tried a rubber resin w/ solvents in a 90/10 ratio of ETN/plasticizer/binder and got good results. What's tricky is plasticizing large amounts at a time.
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Pyrotrons
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[*] posted on 24-10-2013 at 17:39


On the glass stir bars - duly noted. I have PTFE rod that will turn into a small bar tonight for stirring. This will replace those sharp hard things that "detonate" at hypersonic velocities when broken inside my ETN/Acid slurries :o

Rosco - Fear not the reaper.

Chill - looking forward to a response to your questions.

golfpro - I would advise against using "regular plastic spoons" in contact with high-concentration Nitric Acid. Look up "chemical compatibility" of different plastic types with Conc. Nitric Acid.
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Rosco Bodine
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[*] posted on 24-10-2013 at 18:47


Thinking about the properties of the reaction mixture being stirred the ideal material would be a length of teflon rod ....and an improvised substitute that possibly could work though I have never tried it would be a wooden dowel which has been soaked to saturation in molten paraffin.

Nitroester molecules are temperamental little beasties and you really don't want to piss them off by knocking them around between rock hard surfaces, because the potential reaction there could just ruin your whole day in a way that could even make it your last one in this world. Now what good is a learning experience if the student is no longer around, except perhaps as an object lesson for others who are tasked to gather up any pieces of the recently departed. It is highly presumptuos to approach a nitration carelessly with the idea that if you don't get it right this time there will be a next time, because there may not be a next time if you haven't given thought to what you are doing and that thinking has been correct or fortune has favored you for guessing right. Things can still go wrong that are the proverbial fly in the ointment and beyond your control. Some risk analysis is a good thing here with a prudent implementation of countermeasures that is mindful of the nature of the thing being done, which is serious and not trivial.
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Pyrotrons
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[*] posted on 24-10-2013 at 19:11


Thank you Rosco for everything shared. It is absolutely true that I will never again use glass rods for this.

Chill and I share a common issue - large amounts of Ammonium Bisulfate precipitating out of our mixed acids, possibly correlating with failed syntheses. What would be your recommendations on how to eliminate or deal with this problem?
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