Huge AP Crystals

[Energy84]

I hate posting new topics, but jesus christ, I almost shit myself this afternoon! I was cleaning up my room and found a jar that I had used for making some AP putty using DBSP. Well, it was this jar that I used to make the actual putty in and when I was done, I just scraped everything out then threw in some acetone to keep the leftovers nice and damp. There wasn't much left in there, about mabye 2 grams of my ap/dbsp putty which was caked to the sides.
Anyways, when I opened up the jar, I almost dropped the damn thing in amazement when I saw what was inside (good thing I didn't drop it). There were some HUGE crystals formed in there. They were about an inch long! Great big suckers. I took a few pics with my shitty little webcam to try and show you guys, but the resolution just isn't good enough. These things look like those crystals you can make in little kid chem kits...
<img src="http://www.chr1s.b0x.com/AP/BIG-crystals.gif" alt=" - " />
This is a view of the inside of the jar. (It is a half pint jar) Those big white spots are the crystals. Bad res, I know.

<img src="http://www.chr1s.b0x.com/AP/BIG-crystals1.gif" alt=" - " />
Here's another pic of the inside, this time you can see the crystals a little better in the center of the jar. Lots of glare :mad:

<img src="http://www.chr1s.b0x.com/AP/BIG-crystals2.gif" alt=" - " />
Another shot of them...

<img src="http://www.chr1s.b0x.com/AP/BIG-crystals3.gif" alt=" - " />
This is the jar. I filled it full of acetone and put the lid back on until I get the chance to go and dispose of it.

So what do you think? Has anybody else ever had big crystals like this form? This was only the third time I've made AP and I was amazed at how much better 35% H2O2 works compared to 3% :D
Scary thought. Is there any way to preserve this thing? I was thinking of a just keeping it in a glass jar and filling it full of acetone with no airpockets. It would probably be too dangerous though. If it were to crack, that would be the end. <img border="0" title="" alt="[Eek!]" src="eek.gif" />

[MrSamosa]

Hmm...if it were me, I wouldn't store AP or AP puddy more than a few days. I tend to be overly-paranoid with things I make. Then again, I have NO experience in making AP; just go by what everyone else says about it :D . I remember another topic where someone described a similar situation; although his huge crystals were a result of the actual synthesis, not from storage. Now, what I recommend to you: Take some fireplace tongs, use them to take that jar into your back yard, and throw rocks at it :) .

[kingspaz]

this is one of the reasons there is great differences in sensitivity of AP. its also a reason as to why it has caused many accidents. one big crstal in a sea of small ones isn't going to be noticed until it cracks <img border="0" title="" alt="[Wink]" src="wink.gif" />
also glass and fireplace tongs will be slippy so its likely to slip and smash. there isn't that much AP in there by the looks of it so wrap it in a pair of old jeans (nice thick material) and take it to a cliff and drop it! so long as its not left round for some kid to find.

[Energy84]

I think I'm just gonna take it out back and plink away at it with a .22
The stuff must be fairly stable though because even though it's no more than a week old, it's been sitting on top of my stereo speakers. 15" subs and I play 'em loud. Even with all that rattling, it hasn't gone off, so I'm somewhat comforted by that. I really should however quit my habit of using my speakers as tables... :rolleyes:

[ALENGOSVIG1]

Throw rocks at it? Yeah that would be fun. Then again i dont want a rock coming back at me like a bullet going through my head :)

But seriously, I wouldnt even want to touch it. But since you already picked it up and screwed off the lid, you should just place the jar ontop of a detonator.

You know the rest...

<small>[ August 07, 2002, 06:11 PM: Message edited by: ALENGOSVIG1 ]</small>

[PYRO500]

I can't believe what some people do with their AP. I see it put in a jar, stored for long pieriods of time, having a screw on lid on the top. and placed in an area where it could get physical shock!

I'd get rid of that jar the instant you can get it oustide as it's not getting any stabler and is possibly subject to tempeture shock and other forms of shock as is. I don't think it's a very good idea to just throw rocks at it as that means your close enough for human power to bring an object like a rock to the target. an explosive sure could bring a little glass shard to you.

[Rat Bastard]

ARG! broken images :mad:

[FragmentedSanity]

Lo there :)
Sounds like youve been lucky so far. The fact that it still had putty in the jar prolly saved your ass. Ive known the putty to be a little lesss sensitive to shock. But with crystals of that size... :(
your damn lucky crystals hadnt formed around the lid - typing with stumps can present quite a challange (so Ive heard).
Disposal by detonation depends on your location - if your in suburbia you probably want to muffle the sound as much as possible and contain the shrapnel, in which case you would be well served to dig a small hole in the ground put the jar in and cover the dirt back over - the use whatever kind of remote det technique you want. But you did say your intent was to shoot it with a .22 - so I have to assume you out of surbibia - and have a .22 wirth decent range/accuracy and a nice contained place to shoot it and something solid to hide behind - youd still be well served to wrap it in some old jeans as was suggested - even so Id personally rather do it below ground - below water is always fun and theres no real danger of shrapnel, but your device dosent sound stable enough for the construction required (I wouldnt want to be near it any more than necessary).
FS

[Energy84]

I know it was stupid. I just wasn't expecting anything to be left in there.
Yes I live in a nice quite rural area (it's Canada!) with lots of room to myself.
I feel like an idiot for neglecting what little AP I figured was left in the jar. But oh well, learn from your mistakes right? To bring it out I think I'm gonna be wearing full welding dress. Thick leather apron, jacket, gloves and a welding helmet. Then a bucket on the end of a hooked broomstick to haul it out with. 'Till then, I'm staying the fuck outta the way of that damn jar. <img border="0" title="" alt="[Eek!]" src="eek.gif" />

[da man]

I think it would be best to deal with it immediately, than leave it to get worste :rolleyes: Well, AP is soluable i acetone, which it would stop it from exploding, so perhaps you could take it out side, and with an extended tongs pour some acetone into it, this could be dangerous however. What is the jar made of, glass, plastic?
Either way, i would get the jar outdoors as soon as possible! You could even just leave it outside, where there is little danger. Then decide what to do with it, but just get it outside!! You haven't been sleeping in your room with that in there have you!?!

[Mick]

he said he found it in his room cleaning up, so we can assume that yes, he has been sleeping in his room with it.
he put acetone in the jar already to make AP Putty, which is what the AP was for in the first place - so obviously the jar won't melt if adds more acetone, this also means he knows that AP is soluble in acetone.
and he already said he was taking it outside.

wow, da man - 1 minute of reading, and everyone wouldn't have lost 30 seconds of there life reading your reply.

gotta love it.

energy84, i have had a similar thing happen with a batch of APP i made using ping pong balls(however my crystals were no where near as big as yours). i got rid of them by putting some acetone in an empty "spray 'n wipe" bottle and then spraying inside the jar till the AP was dissolved/wet, then i poured about an inch of acetone into the jar to dissolve it all. i figured if i pour acetone straight into the jar it may detonate(dunno why, but i got the image of it happening in my head, so i thought it best just to play it safe)
once i poured the acetone in, i flushed the acetone down the toilet.

short of flushing it, the other way is to strap a small detonator to it.

this is a weird happening with APP that i have noticed.
i have discovered with my APP that if i scrape my jar out then pour some more acetone in with the leftovers in the bottom. after about a week or so i will start to get some pretty big crystals forming out of the putty.
however, if i dissolve some straight AP in acetone then leave it for a week the crystals reform to a normal size.
anyone have any theories as to why this is?
(not really important, but its got me intrigued.)

[Anthony]

Presuming you didn't screw the lid back on the jar, take it outside fill the jar with water and pour it down the toilet or into a small hole in the ground.

[Energy84]

The last picture in the series is a picture of the jar (glass) completely flooded with acetone. The crystals however aren't being dissolved... They're still the same size as before. Also I wasn't too worried about having any recrystalization happening in the threads because it's a canning type jar, which means that there is a thick (5mm) rubber seal around the rim and I tightened it really good. There was actually a slight "whoosh" sound when I opened it up as the air pressure equalized. This batch that I made seems to be very stable considering that it is afterall AP. I'd estimate that there is at least a 5-10% sodium bicarb content to neutralise all acid traces (HCl was used).

Mick, I have observed the same behavior where AP is dissolved in acetone then recrystalised a week later and still having the same size crystals. The only difference that I've seen is that the crystals have a tendency to "cake" together. Not safe, but if you take small bits (pea sized) and break them up seperately from the rest of the batch you still end up with a nice product.

[Energy84]

I'm starting to wonder whether or not that was AP in there... I just went out back and shot the jar with my .22 and nothing happened. The jar just shattered and fell to the ground. No explosion, no fire, no nothing. There were still big pieces of glass laying around, the definiate smell of acetone, and some small black chunks of the leftover SP. I didn't see the crystals, but it was all in some long grass and I didn't really want to prod around looking for them.
But anyways, it's all over, without incident.

Edit - I just found more evidence supporting the whole, "Not AP crystals" theory. I had another jar laying around basically the same as the other except that there was no AP mixed with the DBSP. There were large crysals, same type as the others that I thought were AP, formed in the bottom.
Conclusion, there must be something dissolving out of the DBSP that's being recrystalised. Any idea what it is? I doubt it's NG or NC, but I have no experience with those explosives. Besides, they should have probably exploded when shot with the .22.

<small>[ August 09, 2002, 01:52 AM: Message edited by: Energy84 ]</small>

[Sam]

This relates back to my year 10 science work. In volcanoes, the rocks in the middle of it will be very very large, as the magma has cooled down very slowly, this gives it PLENTY of time to form into VERY large boulders, whereas the rocks on top of the volcanoes have cooled very quickly, as they are exposed to air, these form in MUCH smaller rocks, because they have very little time to form. f you make AP and you put LOTS of acid in it, it will form a lot faster, and in much smaller crystals. If you put bugger all acid in it, it will form over a longer time and in much larger crystals. Try to get your AP putty to dry faster, this may help.

[X-Wulf]

I've had a similar experience with straight AP. After leaving in a plastic container, with a loose lid (most definitely not air-tight), for a couple weeks, I noticed quite extensive recrystalisation. What's strange is that no crystals formed on the sides of the container, nor around the lid, but instead in amongst the normal AP powder, some even growing straight up.
These crystals are clear, gometrically shaped (though are still too small to determine exact shape), almost like large salt or sugar crystals. They're between 2 and 5 mm in length and about 1 mm in height.
They don't appear to be more sensitive than the AP they formed from (detonate from roughly the same hammer impact, and only on contact with open flame).
They appear to be increasing in number and size, but their sensitivity remains comparable to tricyclo AP. Unfortunately I do not have a digital camera, but will try to get hold of one to take some photos as soon as possible.
I have also noticed that a small sample of HMTD also appears to be recrystallising, but at a far reduced rate.

These samples are currently in a cupboard on the far side of the house, but I'm going to move them into a steel box later today. As the samples themselves are small (both under 5 g), the box should be able to contain any accidental detonation.

EDIT: spelling

<small>[ January 12, 2003, 05:00 AM: Message edited by: X-Wulf ]</small>

[Zach]

x wulf, do yourself a favor and get the fuck rid of that stuff. You cant use a digital camera when you're dead.

[X-Wulf]

Thanks for the concern Zach, but I'm well aware of the power of AP and hence the steel box and extremely small quantities.

A friend of mine provided a theory on how/why these crystals could be forming. It's not due to the vapourising and re-crystallising of the AP (hence the lack of increased sensitivity - more about this later) but instead due to the inherent water-of-crystallisation (w.o.c.) present in almost all crystalline structures (including AP I assume - correct me if I'm wrong on that). Hence, when two or more small crystals are very close together, their w.o.c.'s combine to a very small degree, allowing even smaller crystals to rearrange themselves, and thus extend the larger crystals. This continues in, what I'd assume to be, an exponential fashion.

WRT the sensitivity - selecting one of the smaller crystals, I managed to remove it from the container and test it outside. I placed it on a slab of concrete and struck it gently with my highly scientific impact testing device (aka - a standard hammer). To my surprise, the was simply crushed back into a white powder. When I struck this powder again, harder this time, it indeed detonated.

On another strange point, I have been unable to recrystallise AP out of an acetone solution. One reason may be Sam's idea of the solvent being removed too quickly. Any thoughts on this?

EDIT: didn't sound right

<small>[ January 13, 2003, 01:31 PM: Message edited by: X-Wulf ]</small>

[Keyser Soze]

If you are going to keep it in a steel box, i'd at least leave the lid off or the door open. Even in small quantaties, enclosed AP could probably send shards of steel at you if it went off.

[Energy84]

Are you sure that you're actually getting larger crystals and not just 'clumps' of AP? I remember last time I made the stuff It was really lumpy after drying. It was quite the nerve racking experience though breaking up the clumps :mad:

[THe_rEaL_dEaL]

Just a Quickie :cool:

Does AP still have explosive properties when disolved in acetone?

If so this could be usefull for relatively safer "longer"-term storage and eliminating friction sensitivity.

I wonder if it needs to be a saturated soulution to maintain explosive properties.

I assume, if my idea is correct, that a detonator would need to be used. No?

<small>[ January 14, 2003, 01:30 AM: Message edited by: THe_rEaL_dEaL ]</small>

[IPN]

No! Don’t store AP, use it immediately.

Other wise you just risk killing your self!

[X-Wulf]

Energy84 - they're definitely single crystals and not clumps

[Mic]

X-Wulf:
</font><blockquote><font size="1" face="Verdana, Arial, Helvetica">quote:</font><hr /><font size="2" face="Verdana, Arial, Helvetica"> To my surprise, the was simply crushed back into a white powder. </font><hr /></blockquote><font size="2" face="Verdana, Arial, Helvetica">You are talking about your big crystal of AP right ?
If yes, I think that it is just clumps of AP and not single big crystal.. or maybe I am wrong ?

[metafractal]

Real Deal: You are correct, that acetone will not detonate wet. From personal experience, even if it is only slightly damp, it is bareley self sustaining. Still so, while it has been said a hundred times I will say it again: With AP's ease of manafacture and instability, it should never be stored under any circumstances. With that said though, it brings me to my experience earlier today when I experimented with some AP made using 12% cream peroxide, available to me at higher concentration than the regular chemist-bought one atm. It was, surprisingly, quite a success. I seriously doubted that it would work well and didnt even bother neutralizing it or washing it well. I set it out to dry in the sun and came back about an hour later. It was slightly damp, but felt more plasticized than anything wet, so I concluded that it was probably some oils rather than liquids that would not dry off any time soon. I light it and it sputtered while I held a match to it. This proving, thought, that there was still some amount of AP in there I left it to dry for another few hours while I went to cut some bamboo to make a staff. I came back and it was completely dry. I did a quick flame test, and 'Schwish!', just like regular ap. I then proceeded to do a hammer test. This was where it earned its merit. First, I hit it with a softly. No detonation. I worked myself up until I was belting it quite hard. It had become a compressed, fine, powder by now, and still not detonated! I wasnt going to let this go in a hurry... I proceeded to get my sledgehammer from the shed. I belted it with mighty fury, pulverizing the bricks that I was doing it on into dust. But still, no AP det.! I held a match to it, and, sure engough, 'Pop!', it deflagrated giving a pleasing little fireball! As usual, a slight bit of confinement gave a deflagration-to-detonation-transition. God knows what caused this, a multitude of things fly through my head... Sorry for drifting a little away from the topic, but I thought it was of interest and worth bringing up.
As for X-Wulf's crystals turning into fine powder upon breaking without ignition, this is rather parculiar. If they are really single, large, crystals, this does not seem to make sense. One of the defining properties of a crystal is their sturdy geometric structure. Breaking this should easily release enough energy to detonate it.
(Or maybe you just had magic insensitive AP crystals like me! <img border="0" title="" alt="[Wink]" src="wink.gif" /> )

[rjche]

Metafractal, your experience with cream peroxide based AP may have discovered a way to make detonatable AP that is insensitive to friction and impact.

I suspect something in the cream coated the AP crystals similar to the way that dextrose is added to lead azide to calm down its extraordinary sensitivity to friction and thus allow it to be used commercially.

If you would be so kind as to share with us the ingredients listed on the cream peroxide bottle if there are any, and describe in detail exactly how much of what you used to make that batch of AP, we may be able to home in on a form of AP that is very safe to handle yet still an excellent initiator.

Many a valuable discovery came by someone who just did it a bit differently... Goodyear and rubber, Nylon, and a bunch of other miracle plastics.

Yet to be determined is whether such coated AP requires a bit more to have the same initiating power as the uncoated. Even if it required double that would be well worth having not to worry about lids blowing up when unscrewed, or when it was being pressed into BC.

Also it may be found that the coating reduces its volatility...and that would be icing on the cake. All coatings are not alike until proven so, that's why I would like to learn what exactly was in the cream peroxide you used. I have often thought about using the lead azide coating method by adding some dextrose to AP acetone solution and letting it crystalize out with dextrose coating it, but haven't had time to experiment much.

[shooter3]

Cream hardener is benzoyl peroxide(sp?). Could it be something other than AP?

<small>[ February 02, 2003, 04:00 PM: Message edited by: shooter3 ]</small>

[rjche]

Sure could if Benyzol peroxide (BP) was the cream peroxide he meant.

I misunderstood and thought he used a beauty parlor cream type hair bleach, which might be 12% rather than 6% because the cream buffered its corrosive nature, and kept it from running places not intended.

He may have achieved some combination of AP and BP, or a complex between the two, or other things. It would take some high powered analytical equipment to tell just what resulted. However we don't need to know exactly what he made if it performs well. Leave that to the theoretical types.

So, to rephrase the request, please test its initiation ability. If it can come up to #6 strength with a couple grams that would still be worth doing. The BP, if the type used to harden fiberglass and similar types of filled putty, is not all that expensive, and every auto store has tubes of it. If a useful primary that is very insensitive to friction and shock comes of his method, that would be much desired.

[metafractal]

It was definiteley Hydrogen Peroxide cream. The label read "Cream Peroxide. 40 Vol. Contains Hydrogen Peroxide 12%". I have seen Benzoyl Peroxide deflagrate and it is markedly different from Acetone Peroxide. For one, my substance burnt with no visible residue (i.e. no black smoke).
Unfortunateley I am away from my lab for a few days, and therefore am unable to give more information. But stay tuned! I keep a log of almost all the experiments or synthesi(sp?) that I do, and so can give a full account of method and materials. Then I will synthesize by exactly the same method and carry out some more civilized test, or at least as civilized as an ameteur chemist with limited equipment can be.
For now, I will tell you what I remember off hand:
The cream was white and had medium viscosity. I used one hundred percent Acetone. I used a large amount of HCl to catylize the reaction. The crystals were super fine, and did clump an awful lot. This, could be utilized while they were still wet, as a plasticizer.
I have since then used up that batch for an experimental incendary. It was a great success, but thats another story.
Anyway, full write up coming soon.

[rjche]

The fact it is listed as 40 volume suggests strongly that it is beauty parlor product with 12% strength to cut the waiting time on a bleach job in the chair into half or so. Time is money and all that.

The creame can be most anything that does not interfere with its bleaching action. The cream is probably desired to keep 12 strength stuff running down from the head and bleaching skin or other remote hairs.

That cream may be an oil based substance, and that could radically calm down AP physical sensitivity. Remember how they put Nitroglycerine into sawdust to calm it down to being safe for commercial shipping. Also some have calmed down AP physical sensitivity by making putty from rubber glue and other things.

The ap made with a final wash with weak corn syrup water seems to be quite calm and grinding it under a 3 lb hammer face on a steel anvil did not cause it to decompose.

That suggests it would be quite safe to handle, at least as safe as lead based compounds. I would be surprised if a crystal cracking could initiate it unless it was one mother of crystals.

Nice thing about any inert coating on the crystals is that would prevent the energy released from one crystal "going" being strong enough when it reached the closest one to make it "go", unless the crystals were really large, and a large crystal "went".

I trust the hammer grinding test on an anvil because that is really brutal grinding. The forces on the contact point are large. Grinding tends to allow time for the heat build up from compression and friction to dissipate before getting to initiation temps. A fast whack however lets things go wild instantly and that can set things off. A BB hitting some on an anvil would surely set it off, although the energy of a hammer falling a couple inches would be much greater.

If you could use the brisance test using 22 LR hulls that is a fairly good test. Mercury fulminate leaves about 15 particles of brass from a hull. The method is discussed in the optimizing apan thread. It tells rapidly whether a material is fast and sassy, or just pushy.

[NeoSanity420]

I've never used rubber cement to desensitize AP, but I have succesfully used super glue. The super glue was made of cyanoacrylate. I made a saturated mixture, then waited for it to dry, and when it did, I broke it up into hard chunks that detonated loudly even in very small amounts.

I usually seal my caps by putting a drop of superglue in the open end of the cap, then dip the end w/superglue into a pile or container of AP. It mixes with the superglue, and makes for a more efficient detonation of ANNM as well as 15:85 APAN. I only have to use a .31 or .36 or even .22 shells for the cap casing, and I almost always get complete detonations.

[Anthony]

"waited for it to dry, and when it did, I broke it up into hard chunks"

I urge you to rethink this practise!

[NeoSanity420]

Well, when it was drying, it usually didn't stay in one solid piece anyway, and the amount I worked with when I tried it the first time was about .5 g. After the small pile dried, I would just use tweezers to pick up a small piece that came off by itself.

I wouldn't think superglue would make the crystal structure sensitive in any way, because the AP never dissolved into it; the glue only bound the AP together. The confinement from the hard glue only gave it confinement on the outside and in between the crystals, and I found that the mixture desensitized the AP against shock.

I usually don't waste my time mixing it together anymore, because when I light a small piece, melted cyanoacrylate flies in all directions. I got a piece of melted glue on my hand and, or course, it gave me a small burn. Now, I just put a small drop into the end of my caps, then add a little loose AP to fill the cap to the end. I think it makes for a better detonation, especially if it is in a compound cap. I put it in between the primary and the base charge (letting it dry before the base is loaded), and I find it to be more reliable.

[Efraim_barkbit]

That was some strange crystals..
I think I will let the left over solution stand a couple of weeks next time I make AP, just to see if that happens to mee too :D

[FrankRizzo]

Do you use sodium bicarbonate to neutralize your product? If so, that looks a lot like crystalized bicarbonate on your stirring rod. Burn some in an OB propane or butane flame and tell us what color the flame is.

[fowkes.l]

Hi, im new on this forum but have been into explosives for years. I was wondering if any one recieved that report from metafractal on his experiment using cream peroxide in the making of AP?

His experiment intrigued me and I was wanting to try it for my self. If any one has any info on his experiment or synthesis could you please post reply or direct me in the correct path.
I have searched for his results but have been unable to find them.

[yt2095]

i`ve made a little det cap with a .22 shell casing, it`s not like the normal .22 casings i`ve seen before, it about half as long again.
anyway, i pressed in about half a gram (the tube was about 2/3 full). then placed a small amouny of flash 70/30 then my viscose fuse , packed that with tissue paper and put a few drops of super glue on the top to seal it.
reading through this thread, i`m begining to wonder if storing this cap (it`s been a week now) is actualy a wise thing to do. just making the thing was more than enough excitement for one day, but now i`m a little reluctant to even look at the thing!
can anyone put my mind at rest as for it`s stability over time?

cheers and beers :)

[Arthis]

There are many threads about storing AP... I would advise you not to store it for long as it may become shock sensitive. You sure don't want your cap to explode in your hands when you take it, right ?

[yt2095]

Arthis,

Agreed, and most certainly not. 10 fingers have served me well in the last near 4 decades! :)
i was under the impression that most ALL det caps were shock sensitive anyway to a greater or lesser degree. i expect tho, that with TATP the temperature difference between 1 site and another could certainly be a factor tho!
i`ve probably made a poor choice of primary for my det cap, as i wished to keep it for as and when i required it. Now i`m rethinking that i must let this sucker go ASAFP just incase the weather gets a bit cooler and i lose the contents of the drawer i keep it in :(
maybe i`m just paranoid? but unless it`s properly factory made, i have little confidence with compounds like this, esp when it has a DV of about 5.3 Km/s
i`ll heed your advice, and blow the sucker tonight when it`s quiet an there no1 around.

Thanx Arthis, me and my drawer contents owe you one :)

[kingspaz]

yt2095, if you want something storage stable then take a look at mercury fulminate, lead azide, DDNP or silver double salts. all these have reasonable initiating capability and are reasonably storage stable. they also offer a slight challenge to make compared to the peroxide explosives.

[metafractal]

Fowkes.l, sorry about that. Soon after I that post I ran into some trouble, and, in short, lost everything in my lab. I posted briefly about this in some other thread, a while ago. Therefore, I never did get a chance to carry out those tests. But I have some free time coming up, so if I can find that same hair peroxide again, I will post back about it. It was a no name brand, I have described the physical properties in a previous post.

[fowkes.l]

Thanks alot metafractal,

i did an experiment yesterday, I used a washing liquid sold in a 2 litre bottle called Napisan liquid stain remover, it contains 6% hydrogen peroxide as well as some other additives plus soaps (no ingredients listed- except HP). The liquid is gloggy and has a blue colour to it. I mixed 200ml with 150ml Acetone and then slowly added 50ml HCL acid. once I added the acetone the napisan lost its glogginess and formed a white layer on the bottom. It has now been two days and no AP has fomed. I will keep it an extra couple of days, if it doesn't work I'll throw it out.

I also did some tests with wet AP. It seems to me that it can't detonate while wet, from shock or flame. I placed a 7mm cubed pile on a metal sheet and attempted to detonate it with a small sledge hammer (obviously wearing glasses, leather gloves etc.). This was done 5 times and detonation was not achieved. I then placed 1 gram of moist AP in 22-250 rifle shell and ignited it with fuse. It produced a small pop and a little fireball came out drom shell.- no damage caused to shell. I then used 2 grams same thing occured. I proceded lighting larger amount up to 1.5 teaspoons with an extended alluminium pole with lighten stick on end. The AP was placed in empty match box container. It produces a large fireball up to 1.5 metres wide with a swoosh. This was tried 4 times using different amounts.
- no detonation
My AP has been sprayed with a spray bottle filled with water, The AP was damp and formed small lumps.

I also must say that i wore alot of safety gear - so please don't think im foolish

[fowkes.l]

has anyone else got an experiment that they have recently tried which they could share?

[yt2095]

as a matter of fact yes,

last night i thought i`de try alternative catalysts for TATP production

Nitric Acid works a charm.
Copper sulphate gives strange tiny flake like crystals that sink, unlike the TATP i`ve made before where most of it floats.
i`m not sure if it is even TATP yet, i`ll find out later tonight. these are just 2 of a series of experiments i wish to try using different catalysts.
i`ll post full results when i know more :)

[Efraim_barkbit]

:confused:


I have to tell you about some weird cristals in my last AP batch.
I made it with 30% H2O2 and pure acetone as usual. it was not a large batch,~1½ dl fluid when all was mixed. the ratio was 50/50 acetone/H2O2
the acid used was 62% nitric, even since I got adviced by Kingspaz in the thread "alternative AP chemicals" not to use it.

the synthesis was carried out the same way as I usually do, except I didnt keep the temp down as much. (maximum temp reached ~25 degrees C)

when I checked the batch the next day, it had some icelike "flakes" (like small, thin pices of ice)on parts of the surface. it was VERY thin (I had to try 3-4 times to get one up without breaking it). I took a pice of it, about 1x0,5 cm, and put it on the table and held my lighter to it.
when the flame touched it, it starded to melt, and formed a small drop before it ignited with a poof.
then I took another pice of the layer (same size, It was maybee to little to detonate?) and put it on a anvil and hit it with a hammer.
I hit it several times, harder and harder, but I couldnt make it detonate, it only crushed into smaller pieces

I also tested to ignite some of the, still wet, "normal" crystals, and they behaved exactly as the AP from my previous batches.

I have washed and neutralized it now, and some of it are drying, and when dry I will test impact sensitivity on that to.
I hope it will be as unsensitive as the "flakes", but probably not.
the rest of the flakes broke up in smaller pices when I put it in a filter and during the washing, so there are nothing of them left as "flakes"

maybee it was impuritys left in the reaction jar that caused it to behave like this, or possible side reactions from the nitric, as mentioned by Kingspaz.

is there anyone else that had their AP "flake" like this?

EDIT: added a ~

[knowledgehungry]

Nitric acid does react with Acetone to form nitroacetone:confused: not sure if it's called nitroacetone but ive made it a while ago, did no tests on it, i had runaway nitration so i dumped the whole bath. I wasn't trying to make anything i was trying to purify Nitric acid using the solvent method(DCM) but using Acetone instead... not the best idea.

[yt2095]

Interesting! :)

i`m intruiged now, tho i always mix my H2O2 and Acetone (pre chilled) 1`st then re-chill it.
the Nitric seemed to have given me a better yeild than either the H2SO4 or the HCL(aq).
and it behaved in the same way as normal TATP.
i neutralised it with Ammonia also, as my plan was to make APAN, and didn`t want to use/confuse the TATP reactions with other chems (chlorides,sulphates) etc...

the CuSO4 catalyst failed to work and the odd crystal precipitate was not explosive, rather a contaminant in the CuSO4 crystal i`de made years ago using a gell pack SLA battery.

this Acetone Nitrate sounds interesting tho, i`ll look into that :)

[Efraim_barkbit]

I have tested the impact sensitivity now, and compared it with some AP I had left from my last batch. It was no difference in impact sensitivity.
the only difference were that the old AP had much larger crystal size, due to less acid used.
the AP from the nitric batch is like flour, the other like small sugar crystals.


BTW, I found this when searchin google:
http://www.sciencemadness.org/talk/viewthread.php?tid=403&page=1#bottom

[yt2095]

Ooooops!

I tried an unusual syth yesterday Acetone + Ether (50/50) then the usual AP synth technique.
Well! here`s what to do if you want HUGE AP crystals in the normal time taken to make regular AP (though why anyone would want to beats me?) I only discovered this whilst trying to make Ether Peroxide.

the chems used:
http://www.yt2095.net/tests/chemused.jpg

the appearance when making:
http://www.yt2095.net/tests/4mmxtal.jpg

here you can just about see a 4mm AP crystal in the whute emulsified layer and the Ether floating ontop.

here are 2 crystals that I was crazy enough to extract from the dried mix.
http://www.yt2095.net/tests/appen.jpg

I`ve used an ordinary pen to show the size, there are bigger crystals than this in my mix!, but they seem all attatched so I`m not touching them.
I lit a small one this morning with a lighter, a rather loud *Crack* echoed through the place and it left a small dent on the metal tin I lit it on, of course NOW I have the task of getting rid of the 2 grams remaining???
I think maybe I`ll do a storage test with it somewhere in the open away from anything of value, see how long it takes to completely vanish, SLOWLY I hope!
also, I left the AP in a flask of strong bicarb for 10 hours, stiring every half hour, I didn`t want to take any more chances than I already had by letting this reaction get to completion in the 1`st place.

note, unless you have all safety precautions you need and some you don`t in place, I wouldn`t recomend ANYONE try this deliberately!

[vulture]

yt, Do you have a death wish? Ether peroxide is even bigger shit than AP! It's sensitivity is somewhere between AP and NI3 and that is BAD.

Whole labs have been evacuated for an old bottle of ether which had been stored for too long. A simple shock or opening the bottle could cause a vehement explosion which would then disperse hot ether vapour throug the air...:eek:

[yt2095]

I couldn`t agree more, and yes I`m fully aware of it`s properties.

the point being, some may not be, and since this forum`s about education. who better to do some of these things 1`st and take pictures. that someone that has the appropriate equipment/experience/and dare I say it Paranoia associated with handling hazardous substances such as this.
I also have the time and patients not to rush headlong into danger (as some of the kewls or teeny-bombers might and do)
I certainly understand your concern, and although I`m shameless in taking precautions and measures neccesary to living a long life, I feel that showing what NOT to do, is just as beneficial (within reason obviously)

the white emulsified layer is indeed a combination of TCAP and EP, it also serves well as an AP crystal "incubator" for wants of a better word. be sure that the 4mm crystal isn`t as large as they CAN get, but that was as large as I felt comforatble dealing with, plastic polyprop tweezers were used to extract from the 250ml bicarb soln. whilst wearing gun range goggles and kevlar motorbike gloves, it was also done with a blast sheild and a mirror to see with.

Maybe I should take some pics of the techniques I employ?

death wish no... nerves of steel no... healthy respect and an understanding of potential but unapparent dangers, you bet yer ass!

[yt2095]

sorry to double post (an edit wouldn`t reshow this to people that have already read the last one), but a thought just occured to me as to some of the numbers people use for PERCENT H2O2 when thay may mean O2 VOLS!

I`ve often seen "30%" H2O2 bought from a chemist, when in fact it`s 30Vols H2O2 and NOT percent at all! it would be only 9%!

on the last page (2 posts ago) I show the chems used to grow a huge(ish) AP crystal. the peroxide used is only 9% but 30 Vols is the 1`st thing to hit you when you read it!
I wonder now how many posts have this mistake incorporated into them?

[Anthony]

Yeah, we've had a few people get mixed up between the two over the years. Doesn't seem to happen so much nowadays, I think it's because of the higher average level of knowledge.

[Arthis]

When using 130 vol H2O2 you can be tricked... ;) [-> ~30-35 %]

[metafractal]

A while back, when I made AP with 50% H202, 100% acetone and ~35% HCl (I always dilute reactants now, but that was only soon after I got a hold of some 50% H202), the crystals came out very large, about 5mm long. The reaction did get hot a little hot, but nothing much to worry about. The reaction was left to sit in about 4*C for about 24 hours. I remember I used the proportions described by angelo in a post called "3% compared to 6% H2O2 -archive file", which I had bookmarked on the old forum and had been unable to get back (are the archives accessable on this new setup?). After neutralization, I found them to be of regular power and sensitivity (even though one would expect that a larger crystal size would make them more sensitive. Note that no formal test were done, this is just from memory of use.)