More Stable AP? No Way!

[tacmatricx]

Mde a batch of AP about four months ago, Standard procedure with crappy 3% H2O2... Not a great Yield, The difference to all the other methods however was that we icebathed it with salted ice to mix and then we stored it overnight at 1 deg C... The next morning we had the standard top cake and lower precipitate but this stuff was almost insoluble in water? (small amount of Ice appeared at the top as well 0.5 deg C maybee?)

We dried it in a dark container constantly changing the paper towels it was sitting on and when we were sure it was dry, we took a 1/4 teaspoon and with earmuffs on struck it with a hammer lightly... and again and again progressivly harder until we heard the loud report. the pound would've drawn blood from a finger we had to hit it so hard! We thought it was dead at first until it went!

The same amount however would explode furiously on a toilet tissue with the slightest hint of a flame without blackening the paper. It was four months ago and I still have some in a cool dry place stored in a film canister. It only seems to be affected by sunlight or ulraviolet light.

The canister we made it in had pencil tip sized xtals on the sides that would not dissolve even with repeated soakings in tap water... I wouldn't dare scrape it! but how do I dissolve the bastard?!?! Acetone also has no effect.

Could be a new method for assuring no Di AP and only Tri AP is made?

I live in the caribbean with 80-90% humidity if this would make a difference?

I Would be Very interested in batches made in other climates!

Thanks.

[Hang-Man]

I live in Canada, and let my AP rxn run outside in sub zero temps. I get the same thing you do; stable as hell, only goes off when I want it too. The only way I can get it to explode on shock is if I really pound the hell out of it with a hammer on a hard surface, ie anvil. And I have to hit it, not just around it. I use 33% H2O2 unlike you, and humidity around here is pretty much zero (hard to keep water in the air when the air is -33 C)

I don't know why some peoples is kick-ass stable and others explodes if you look at it wrong. Don't worry about scraping it off the glass, if its wet at all its fine. or take a red-hot stick to it.

[Desmikes]

Hang Man, NI3-NH3 and such would probably explode if you hit "around them". Unless you can swing at supersonic speed, why would AP explode from indirect contact with the hammer?
Does anyone have any solid data (multiple drop tests with various surfaces yielding consistent results) on whether or not it makes a significant difference if your AP is acidic or is made up of large crystals, or if it has impurities such as sand or additional oxidizers like KMnO4, KNO3? I suppose it would be difficult to attribute effects of oxidizers to sensitizing/desensitizing because you have particle sizes coming into play. It would also be useful to know how very acidic AP would behave when mixed with things of this nature.

[Skean Dhu]

yea, I made some not too long ago(before the thaw) and its been happy living in an open-top container that used to hold cooking herbs. Its easily 2 months old and shows now definative signs of sublimation that some of my other batches have shown.

[tacmatricx]

[QUOTE=Desmikes] Does anyone have any solid data (multiple drop tests with various surfaces yielding consistent results) on whether or not it makes a significant difference if your AP is acidic or is made up of large crystals, or if it has impurities such as sand or additional oxidizers like KMnO4, KNO3?

I agree with the drop tests Desmikes but the purpose of this post is the apparent stability of AP synthesized over hours at near zero Deg C temperatures, Drop tests can vary depending on the crystal size, acidity, salt impurities etc.

The AP I made was 1/4 size of a grain of salt and bright white in appearance. They were washed repeatedly with distilled water and verified to be neutral with litmus paper when still damp.

Other batches of AP I made without extended cooling, sublimed more easily with a noticeable loss after a week in an open container was much more unstable to storage temperature with seemingly random detonation under certain conditions.

This I believe is due to the creation of more Di-Acetone Peroxide instead of Tri-Acetone Peroxide making batches more unstable.

Extended cooling seems to produce a stable product that can be easily stored more than six months without loosing even 30% of your batch! Much more stable to shock and temperature (higher temperatures increase sublimation) without any loss of VoD.

I would greatly appreciate more results of this method and any data collected. I will begin building a drop rig to test AP synthesis with varying cooling temperatures and durations.

Results to follow

[Boomer]

I had no loss due to sublimation either, not even after one year at room temperature. Maybe only the dimeric form sublimes that fast?

The only thing I noticed is a slightly larger crystal size after long storage, but dissolving in acetone and pouring in water gives a product with the consistency of a new batch!

I mix the batch at -20C and keep it in the freezer at that temp for 48 hours. But I do NOT have to pound THAT hard! A 1/2 pound hammer on a steel anvil detonates it if dropped (from its own weight only) approx. 15-20 cm, this is 1/3 of what NG needs. At least this sensitivity is quite constant with batches and age.

[tacmatricx]

Hey Boomer, Love the Renew the batch method, Its almost a fountain of life for AP :) To get my batch to go off I really do have to smack it, It could be the 90% humidity down here.

Question... When I make my batches at near zero deg C I notice ice forming at the top... At -20 for 48 hours does your whole mix freeze? I always figured that would slow the reaction to a halt and keeping it at near zero would just slow it down enough to make sure the trimer is all that forms?

I am heading down to the lab this weekend (Wife Permitting) :p to make up some more and hopefully get a few detailed pics of the creation process and some vids of me smacking it with a hammer (SMALL amounts! as always but this time THICK EARMUFFS I don't intend on going deaf again) Thanks for the Help!

[Hang-Man]

When I make my batches at near zero deg C I notice ice forming at the top... At -20 for 48 hours does your whole mix freeze?
I let my batches run for about 5 hrs, not 48. Depending on the container, acid, and time, I sometimes end up with a frozen slurry of AP, its like a cake. turns back into slurry with a little water though.

I chill all my reactants before use, and I get AP forming in between 30-60 seconds, so the cold dosn't seem slow the reaction down. I do dump all 50 ml of fumeing HCl in at once though.