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Author: Subject: HMTD smells like ammonia
crazyboy
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[*] posted on 8-3-2008 at 09:57
HMTD smells like ammonia


Well I just synthed some HMTD (mostly to test my magnetic stirrer) and I decided to smell it AP has a unique smell so I was curious about this peroxide. I thought it would smell fishy like my hexamine but it smells fairly strongly of ammonia. Is this normal? Is it because I didn't neutralize it enough? Is it even safe?



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vulture
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[*] posted on 8-3-2008 at 17:09


Quote:

Well I just synthed some HMTD (mostly to test my magnetic stirrer) and I decided to smell it AP has a unique smell so I was curious about this peroxide.


Can I put this on my wall please? Because this must have been the most memorable excuse for making HMTD I've ever heard. If you want to test your magnetic stirrer, make a friggin salt solution.

Look at the chemical structure of hexamine & HMTD and then wonder again why it might smell like ammonia.




One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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crazyboy
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[*] posted on 8-3-2008 at 18:19


No I was going to make a primary and I chose HMTD over silver acetylide so that I could use my magnetic stirrer in an actual synth for the first time to see how my homemade stirrer bar would hold up to concentrated H2O2 and very cold temps for an extended period of time. And sorry for not looking I forgot the diamine part of HMTD was referring its double ammonia complex. Anyway the smell is gone now I let it soak in bicarb soln. then purified with acetone and washed it.



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Rosco Bodine
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[*] posted on 8-3-2008 at 18:48


Two ammonias are the byproduct of the reaction between hexamine and H2O2 which produces one mole of HMTD .
Usually what you would do is add just sufficient acid like
HCl or HNO3 or acetic acid to the cold mixture so that the byproduct of two ammonias is neutralized as the reaction proceeds . Using hexamine dinitrate as the precursor instead of hexamine , the neutralization equivalent is already included in the precursor .

Why would you wash HMTD with sodium bicarbonate ?
To neutralize ammonia you would use a dilute acid like acetic acid ....not a mild base like sodium bicarbonate .
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[*] posted on 10-3-2008 at 07:10


The bicarb wash is hard to kill, probably comes from the AP synths that spread the myth about peroxides being more sensitive in an acidic environment.
Ever wonder why Merck puts *acids* into their H2O2 as a *stabilizer* ???

And while we're here, one of the stupid cookbooks tells the kids to add an oxidizer to their TATP to improve the power. Now guess what oxidizer they recommend? Permanganate, a powerfull *decomposition* catalyst for peroxides!

I made a test with approx. 20mg each of HMTD and KMnO4, intimately dry-mixed on a piece of paper with the tip of a knife. Surprisingly it did not spontaneously detonate (which a 500mg batch unfortunately did some years ago), but already during the mixing it started to stink, and turned to fishy non-explosive shit within hours.

Oh and finally, TATP is not too sensitive to handle, but too sensitive to handle in bulk when dry. Other primaries are worse in some respect or some other, just think of LA. A dripping wet chunk in paper towels will not detonate on pressing, but for pressing it nearly-dry in a vise (my method) I do strongly recommend to stay in the milligram range. And that's not 500mg unless there is additional protection.

Hell, with enough water you can put it through a blender. Do that with non-dextrinated lead azide. But once dry, it can go off when you pour it from a folded paper, just from the little friction between crystals and paper, most likely via static.

If you don't believe me, do a test. Finish-dry <50mg on a sheet of paper on the oven plate at 80C for 10 minutes, let it cool, then rub with a knife tip like a coke user to get a fine powder. You won't be able to shove it back together to a line, as it clings to the paper and even jumps into the air to attach itself to the knife blade, simply from static. Go figure!
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Rosco Bodine
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[*] posted on 8-9-2017 at 16:38


Quote: Originally posted by Rosco Bodine  
Two ammonias are the byproduct of the reaction between hexamine and H2O2 which produces one mole of HMTD .
Usually what you would do is add just sufficient acid like
HCl or HNO3 or acetic acid to the cold mixture so that the byproduct of two ammonias is neutralized as the reaction proceeds . Using hexamine dinitrate as the precursor instead of hexamine , the neutralization equivalent is already included in the precursor .

Why would you wash HMTD with sodium bicarbonate ?
To neutralize ammonia you would use a dilute acid like acetic acid ....not a mild base like sodium bicarbonate .


I have recently ended a 15 years long term -10C cold storage test on a sample of HMTD which showed no sign of decomposition after 15 years storage at -10C. The sample was made by simply dissolving hexamine dinitrate in ice cold 27% hydrogen peroxide, and keeping in the cold for several days until no further precipitation occurred, rinsing with cold distilled water on the filter and air drying, stored in a LDPE container in a freezer. There was no fishy odor from decomposition or color change and the sample appeared perfectly preserved after 15 years storage. At ordinary temperature HMTD gradually decomposes, but kept in the cold it appears to be very stable.

A 50/50 mixture of coprecipitated MEKP/AP (liquid) was stored long term at a much warmer but still slightly cool temperature for 13 years and showed no sign of decomposition.

No "neutralization" scheme using any base was used for either sample which seem to be storage stable anyway.

http://www.sciencemadness.org/talk/viewthread.php?tid=20&...

[Edited on 9/9/2017 by Rosco Bodine]
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