Sciencemadness Discussion Board

Diphoronepentaperoxide (DPPP)

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WaveFront - 19-1-2005 at 13:19

The spoon was trought violently down, the front part destroyed the lighter and part of my nail (you can see it is bend in the opposite direction than the rear part that became more convex, received a severe hit with the metalic part of the lighter). So I suppose that the shock with the lighter changed the direction of the spoon to the left hand that was holding the spoon. I can not find other explanation.

Dodoman - 19-1-2005 at 14:35

Just finished my exams the other day and I finally have some time to do experiments and I did :D. And I have some interesting observations that I think could help us determine the optimum reaction conditions.

Here is a detailed description of what I did.

In a 500 ml RB flask, with 24 ground glass joint, 100 ml acetone was added to which 150 ml of 30% HCl was added and a Allihn condenser attached. The solution was refluxed at 80 c for two hours.

Observation: the liquid turned from pale yellow (at the beginning of the reflux) to dark cloudy opaque black color with orange tint towards the end of the two hours.

There was thin layer of transparent oil floating on top. The oil was very little not even forming a complete film that covers the whole surface. We know that this by product is not peroxidisable. So the assumption would be that two hours of reflux at 80 C is the optimum condition for the formation of the precursor.

The liquid's volume at the end of the reflux was 244 indicating that 6 ml acetone was lost.

I cooled the liquid overnight (the oily layer became more pronounced).
In a 600 ml beaker, placed in a salted ice/water bath, 100 ml of the opaque liquid was added and then peroxidised with 100 ml 30% of H2O2. The peroxide was added 3ml at a time and the temperature kept under 10 C.

The crystals was filtered.

Observation: the crystals have a white color with a very faint yellow color the filtrate had a yellow/green color. On scraping the acidic crystals with a tin spoon they turned yellow indicating a reaction taking place between the metal and crystals. So I think that the assumption that the peroxide is compatible with metal is wrong or at least not when acidic. Whoever the neutral crystals don't seem to show any reaction towards the spoon though.

The crystals was filtered with a Buchner funnel and had a fruity pleasant smell. The still damp crystals weighted 41 gm :(.

The crystals burn very fast with a yellow flame, a crackling sound and no smoke.

As I told Rosco before in a U2U message I intend to determine the composition of the black precorser by using thin layer chromatography. Any thoughts would be apreciated.

[Edited on 19-1-2005 by Dodoman]

Joeychemist - 19-1-2005 at 14:47

The crystals crackle when burned because they are not dry. This stuff is quite the “bitch” to dry.
There may have been a reaction between the un-reacted precursor and the spoon and not the DPPP itself.

Dodoman - 19-1-2005 at 15:46

Quote:
Originally posted by Joeychemist
There may have been a reaction between the un-reacted precursor and the spoon and not the DPPP itself.


Just did a quick test to find out. I placed a few drops of the precursor on the handle of the spoon and nothing hapened.

If you want I could probably borow a camera from a friend and post a few picture of the spoon. It have a pale white layer from where the crystals were.

Joeychemist - 19-1-2005 at 15:50

Sure if you like, but I belive you.;) I knew the washed crystals reacted with copper and brass but I did not think that they would react with a spoon,(which is stanless steel right?)

Dodoman - 19-1-2005 at 16:14

Quote:
Originally posted by Joeychemist
Sure if you like, but I belive you.;) I knew the washed crystals reacted with copper and brass but I did not think that they would react with a spoon,(which is stanless steel right?)


No it is tin.

Can anyone please recommend a solvent for use in TLC. I asked Rosco and he recommended a few but i want to hear other openions first before I do any further expiraments.

The plan is to determin the components and try to separate them and analyse each separetly using NMR and IR among other methods.


[Edited on 20-1-2005 by Dodoman]

Some thoughts and some preliminary tests

Rosco Bodine - 19-1-2005 at 17:16

Dodoman :

I have been looking at the precursor preparation too because I believe it is a key factor .
My focus has been on the sealed bottle method because of simplicity in assuring no
loss of acetone . I have found that heating and excess HCl to acetone increases the production of the insoluble upper layer of oily material . An experiment has been underway to allow the formation of the precursor to occur very slowly at room temperature in a sealed bottle . I placed a carefully measured 100 ml acetone and 95 ml HCl 31.45% into the bottle and sealed it . After self reacting for 30 minutes I gently heated the bottle
at about 60 C in warm water for about an hour until it had the appearance of orange soda pop , and then discontinued the heating and set the bottle aside at room temperature .
72 hours later the color is very dark "black cherry red" or "blackberry red" and almost completely opaque to light , orange red in thin layers when swirled against the inside of the bottle , and having only a very slight isolated oily trace on the surface , not a continuous sheet of oily layer . The very slow reaction is something observed easily by sitting the bottle on a window sill . I am going to let the reaction continue slowly to see just how dark the mixture will become before any significant amount of oily precipitate is produced . I believe that adding extra HCl to the chilled precursor immediately before the peroxidation increases the yield . I also believe that somewhat more H2O2 than is specified by the patent is appropriate for the reaction . The mixture definitely lightens in color when allowed to stand for several hours and results in a purer product .

One idea which I intend to make the source of an experiment is to use the amount of peroxide required by theory to form the DPPP , and then to filter the DPPP crystals from the reaction mixture without dilution , saving the clear filtered and supposedly spent peroxidation mixture . Then to that freezing cold supposedly "spent" reaction mixture will be added an additional quantity of acetone , equal to the amount of acetone first used to originally form the precursor . The mixture will be kept in the freezer for three days to observe for any precipitation of AP , which should form from any unused peroxide which may be present in significant quantity . If a substantial amount of AP is recovered by this strategy , say in an amount perhaps 1/2 or more of the original DPPP amount , then DPPP will be immediately proven to be something else entirely , or to have formed by an entirely different reaction than the "pentachlorophorone" intermediate .

The reports about extraordinary brisance in milligram amounts do not square at all with my own tests so far with the molten material . Surely in larger quantities such behavior might be observed , but not in the range of a few milligrams . And so far the few tests that I have done indicate that the self accelleration is not even close to that of something like lead azide in small diameters and weights of charge , actually even lower than basic lead picrate for low order detonation . I am stepping up the diameter of the charge in small increments to find that smallest diameter where a moderately compressed pellet of twice its diameter in length will undergo DDT to low order in a tube open at one end . So far I am up to just under 1/8" diameter and am not getting any detonations yet for AP , DPPP , or HMTD tested side by side . Experience has shown me that finding that diameter where the material goes low order can be increased by 50% and a high order detonation will occur for a good initiating explosive . For a practical application , generally the low order minimum DDT diameter would be doubled to secure reliability for an initiator desired to always DDT in high order fashion . I can't give any citation on this , it is just something I have observed to be a practical rule of thumb .

What these small diameter tests are telling me so far is that DPPP is not an unequivocal primary which will high order detonate unconfined in amounts in the range of a few *tens* of milligrams . Now that doesn't necessarily mean DPPP is no good for an initiator , because HMTD is not small diameter effective either , but HMTD does get where it needs to be in output intensity at a reasonably small diameter and charge weight , actually surpassing lead styphnate in that regard where it achieves a "critical mass" to *high order* detonate with moderate confinement , and deliver sufficient impulse to make it usable as an initiator in a cap sized charge . DPPP could prove to be comparable with HMTD , or it may not . I have more tests to do before reaching the charge diameter which demonstrates DDT in an open ended tube scenario .

[Edited on 20-1-2005 by Rosco Bodine]

Instead of relying on reports

Matsumoto_Hideki - 19-1-2005 at 17:28

I know from first had that DPPP detonates in much much smaller quantities than AP and is WAY WAY more powerful. All you have to do is download from this form the Test.pdf and read it. .

BTW instead of relying on others' tests go try detonating some yourself.

Hey rosco I am not exggerating about the spoon as I will post pic shortly as my camera is on lone for a few hrs. no hole was blown through it though the spoon, DPPP seemed to propel the bowl downwards so that the bowl almost touched the end in kind of like a narrow U shape. Yes the amount was in the 1-3 milligram range
Give it a shot and let the DPPP melt ... You will be amazed just how much validity my post has.
Don't try and start that "you are BSing" shit all over again.

[Edited on 20-1-2005 by Matsumoto_Hideki]

Neutralisation of the black stuff

chemoleo - 19-1-2005 at 17:35

Hmm, I am not sure how far you will get with the TLC.
Solvents - you need something inert, but by the looks of it, the dark solution is rather reactive (see below). You can't use alcohols, ketones or anything like that. Even water may not be a good idea.

On anohter note, I did some tests recently, with various proportions of acetone vs 37% HCl, all being incubated at 65 deg C for 90 minutes.
Interestingly, the proportions 26.6 ml Acetone, and 13.3 ml HCl gave the darkest colour after the shortest amount of time, NOT the 1:1 mixture. I tested, 4:1, 2:1, 1:1, 0.5:1, 0.25:1 proportions of acetone vs HCl. Further, a huge excess of HCl only made the solution faintly lemmon yellow. A 4x EXCESS of acetone still resulted in a fairly dark solution, about as much as the 1:1 mixture!

Even more interesting, did someone actually try to neutralise this solution?
Well, I did (using the darkest, i.e. the 2:1 solution), once with NaOH and once with Na2CO3.
With NaOH, the solution first produced a precipitate, which redissolved once more NaOH was added (I analysed it later, it rapidly dissolved in H2O. Probably it is NaCl, which redissolves once more water/NaOH is added). Furthermore, an insoluble oil appeared, which rose to the top, i.e. 4 ml of solution produced about 0.5 ml of a dark oil. This oil is truly insoluble in water. With 4 ml conc NaOH and 4 ml black solution, the colour changed to a nice orange, with 1/2 ml of oil.
Interestingly, with Na2CO3, I got faint bubbling, but by far not as much as I expected. First I thought no bubbling occurred at all, so little it was. Yet the colour changed to bright lemmon yellow (8 ml total again), and deposited a small amount of brightly yellow oil - which seemed to have some fluorescent quality to it.
Water dilution with the same amounts just yieled a darkly orange solution, with no oil (or extremely little).

Also, did anyone notice that the black solution does NOT smell of HCl at all, even though 37% (which is strongest) was employed?

Well what can we conclude from this?

1) I am pretty convinced all the HCl has reacted with the acetone, which becomes pretty evident with the neutralisation experiment. The dark colour is clearly a result of polychlorination - as even carbonate is enough to decolour the mix. That's why I also think the TLC will not be easy - there may be many chlorinated species.

2) I would have thought that neutralisation should have produced phorone, which is insoluble (do correct me if I am wrong) in water? No precipitation however.

3) Also, I really can't imagine there is free acetone left after the experiment (cooking with HCl). It didn't smell like it at all, and after carbonate/base addition, the smell of acetone did not reappear. And my nose is pretty good :)


Altogether I have a little more faith now that this is possibly not AP after all. A condensation back to AP, from a highly polychlorinated conjugated material seems very unlikely to me, as the neutralisation still produced a yellow solution with an insoluble oil - which wouldn't happen if the polychlorination was reversible.

What I might test is
1) Whether a 1:1 dilution of black stuff and water, with H2O2 still produces a precipitate. I have the impression that the concentrated solution is chemically different from the solution diluted with water (the colour change seems too great)
2) whether the neutralised stuff (either with NaOH/Na2CO3) produces a precipitate with H2O2,
3) whether the neutralised stuff brought back to the original volume (boiling) produces a precipitate with H2O2
4) whether the neutralised stuff produces a precipitate with HCl (return to the dark colour? dissolution of the oil), when H2O2 is added?

Essentially I'd like to find out whether only the polychlorinated stuff produces a precipate. If the neutralised stuff produces a precipitate with H2O2, then, maybe after all, we got a large amount of acetone back again.

I got pictures, which I may post later. Am most intrigued by the oil though - essentially representing 30% of the total acetone initially employed. Quite a good yield with so many other things being produced!

Rosco Bodine - 19-1-2005 at 17:52

Systematic tests are being done in a way which has allowed me to have accurate and factual data derived directly from my own tests , information in which I have always placed more confidence in the validity of that information , for having obtained it directly from my own work , than in simply trusting what I read or even see pictured in photographs . What you say works for you is just great , but now I have to see for myself what works for me . When I do an analysis I tend to be careful and systematic and thorough so that I can have confidence in the validity of the findings , and learn what I want to know which usually goes beyond simply accepting what someone else tells me , while leaving many questions . It is a methodology of thoroughness I got from spending way too much time in the lab at way too early an age :D

LIGHTEN UP ROSCO!

Matsumoto_Hideki - 19-1-2005 at 18:04

Well, i guess you really haven't fully melted this stuff when it is totally dry? I got the scare of my life as I stated earlier. It is nice for one to be anal about everything but, as I said I shit you not DPPP in molten state produces a detonation and detonates downwards, this is why it tends to warp objects downwards that it detontes on. **************************I Never claimed that DPPP was nuclear LOL. GEez lighten up..

Edit by Chemoleo:
NO FIGHTING PLEASE, to everyone. There is no point. Accept that someone else wants to verify claims, and accept that exaggerations (such as 1-3 mg) are mercilessly exposed :)
Fight on U2U, in real life, whatever, but not here. It dilutes the thread with unnecessary crap.


[Edited on 20-1-2005 by chemoleo]

I melted 100 mg DPPP , pffftttt , no detonation

Rosco Bodine - 19-1-2005 at 18:15

I melted one tenth gram of DPPP in a stainless steel tablespoon clamped to a ringstand heated with a candle placed below . Half of it evaporated while melting . I plunged a glowing splint into the melt and it popped gently like a paper roll cap being set afire .

I repeated the test only without using the glowing splint , and the material puffed off quietly with no detonation after it reached flashpoint .

So now what , 1-3 milligrams detonates with vigor , but a hundred milligrams doesn't do shit ?

Rosco Bodine - 19-1-2005 at 19:03

Quote:
Originally posted by chemoleo
On anohter note, I did some tests recently, with various proportions of acetone vs 37% HCl, all being incubated at 65 deg C for 90 minutes.
Interestingly, the proportions 26.6 ml Acetone, and 13.3 ml HCl gave the darkest colour after the shortest amount of time, NOT the 1:1 mixture. I tested, 4:1, 2:1, 1:1, 0.5:1, 0.25:1 proportions of acetone vs HCl. Further, a huge excess of HCl only made the solution faintly lemmon yellow. A 4x EXCESS of acetone still resulted in a fairly dark solution, about as much as the 1:1 mixture!

Using half the HCl to first form a monohydrochloride derivative of phorone was something I mentioned early in the discussion of the possible reactions many pages back in the thread here , but I forgot about it till you mentioned it . Sometimes a reaction can have an unfavorable equilibrium towards the endproduct , and if two groups are to be introduced , then it may be more favorable to introduce the first group and let that go to completion , and then introduce the second group . This can be a workaround which results in a higher yield of the intended endproduct by having its two groups introduced one at a time ,
if the strategy applies to the equilibrium conditions . So to put it another way , adding half the HCl and letting the reaction go as far as it will go at a reasonable rate , before adding the second half of the HCl , and then letting the reaction complete , may possibly result in a higher ultimate yield of the dihydrochloride than adding all the HCl in one portion .
Quote:

Even more interesting, did someone actually try to neutralise this solution?
With the 1:1 solution , you should get some phorone precipitate .
I haven't tried it but that's the way it would likely go .
Quote:

Also, did anyone notice that the black solution does NOT smell of HCl at all, even though 37% (which is strongest) was employed?

Well what can we conclude from this?

1) I am pretty convinced all the HCl has reacted with the acetone, which becomes pretty evident with the neutralisation experiment. The dark colour is clearly a result of polychlorination
Agreed , probably some polymerization and then the polymer is condensed with HCl . Some alternate possible compounds which I have considered possible products are propylene chlorohydrin , and chloroethyl methyl ether , perhaps chloroacetone as well although I am uncertain of this .
Quote:

2) I would have thought that neutralisation should have produced phorone, which is insoluble (do correct me if I am wrong) in water? No precipitation however.
Did you try boiling it a bit ?
Quote:

3) Also, I really can't imagine there is free acetone left after the experiment (cooking with HCl). It didn't smell like it at all, and after carbonate/base addition, the smell of acetone did not reappear. And my nose is pretty good :)


Altogether I have a little more faith now that this is possibly not AP after all. A condensation back to AP, from a highly polychlorinated conjugated material seems very unlikely to me, as the neutralisation still produced a yellow solution with an insoluble oil - which wouldn't happen if the polychlorination was reversible.

What I might test is
1) Whether a 1:1 dilution of black stuff and water, with H2O2 still produces a precipitate. I have the impression that the concentrated solution is chemically different from the solution diluted with water (the colour change seems too great)
The reverse order of addition during peroxidation , adding the precursor to the peroxide very cold , results in even more yield of product than
the usual order of addition .

Blaster's Spoon

FrankRizzo - 19-1-2005 at 21:38

http://www.sciencemadness.org/talk/viewthread.php?action=att...

On review, this one may have been faked by shooting with a gun.

::

Pyroz - 19-1-2005 at 22:02

pt1. I like the idea about adding 1/2 HCL ---to acetone then adding heat and then adding more acid--- its seems to make sense to me-- I shall try that Rosco. Good suggestion.
---------------
pt2. Rosco, in order for DPPP to detonate in open air you have to gradually heat it--- then it pools as a liquid and becomes a unified compressed material and then --- with a little more heat you should get a sharp "bang". At least this is what I have experienced. To enhance the explosive properties maybe put 200mg in between 2 spoons (lay one ontop of another) and then heat gradually.
You will get a decent sized explosion!
---------------------
pt3. Chemoleo: that bright yellow oily layer from the reaction between acetone and HCL has been confermed as a Mestyl byproduct* its actually a very good sign and means that the dark liquid is a phorone-isomer. So I think we are all on the right track here.

you wrote (Chemoleo)"Altogether I have a little more faith now that this is possibly not AP after all. A condensation back to AP, from a highly polychlorinated conjugated material seems very unlikely to me, as the neutralisation still produced a yellow solution with an insoluble oil - which wouldn't happen if the polychlorination was reversible.
hehe, I'm satisfied... hands down. No convincing here. The only issue left to solve is the materials exact VoD/output power in joules during a detonation.

[Edited on 20-1-2005 by Pyroz]

DPPP minimum DDT diameter 5.5 mm

Rosco Bodine - 20-1-2005 at 14:09

That's what I'm getting from my tests .

What I have been doing is drilling holes in a hardwood block , so that the depth
of the hole is a bit over twice the diameter , then filling the holes to the surface with both the loose powder lightly tapped to settle it into the holes , and also subsequently testing a compressed charge in the same hole filled to the surface . The charges are ignited and the results observed . The size and depth of the holes is increased by drilling with the next size drill bit , until the point is reached where a low order detonation occurs . At 5.5 mm diameter , the charge of loose crystals detonates for DPPP made by either order of addition for the peroxidation , and also for loose crystals of AP . Compressed charges
of all three sample materials only burn , but the loose crystals DDT low order . HMTD only burns loose or compressed at this diameter . At this threshold diameter for DDT and minimum critical mass , the AP is actually showing greater brisance , even though that absolutely does not necessarily have any bearing on what will occur at larger diameters with larger charges , since it is already known that the HMTD will catch up and pass the AP as the charges are incrementally increased into the range where high order detonations occur . The DPPP is expected to behave in a similar fashion . Typically what these incremental increase tests will reveal is there is a certain quantity at which a sudden disproportionate increase in energy is developed , a sort of "critical mass" where a transition to high order detonation occurs . It is necessary to determine approximately what that amount is , in order to know what is the useful range of weights and diameters that are efficient minimums with regards to a particular material .

Your DPPP is NOT dry ! DANGER !!!

Matsumoto_Hideki - 20-1-2005 at 15:04

Boy oh boy you are in for a MAJOR scare !
I woulden't even consider 100mg in a spoon and heating it unless you want spoon shrapnel in your forhead. YOU are going to kill yourself!

Dry your DPPP out using 100% isopropylene .... Then when it has dried out completely ...then over a low flame, in a spoon let it completly melt then lower your spoon into the flame. It will detonate with a terrific detonation. As I said the small amount I did was in 1-3mg range and detonated with enough force to bend the spoon into a U shape. This aint a joke.
If you want to try bigger amounts I would be EXTREAMLY CAREFUL!
If this experiment is done on a hot plate you may try 10mg put turning on the plate from a remote location (10ft back)

Rosco Bodine - 20-1-2005 at 15:15

Actually my DPPP is quite dry .
And only in your dreams would .001 to .003 grams DPPP do the sort of damage you are describing . Try that story somewhere else okay , it isn't getting any mileage here .

Propylene is a gas like ethylene is a gas .

So , by "iso"propylene exactly what are you talking about ? Are you meaning isopropanol , the alcohol also known as
2-propanol ?

chemoleo - 20-1-2005 at 16:00

Aside from the obvious exaggeration (matsumo - weigh for once 1 mg. A single tiny crystal weighs about as much), did you actually recrystallise it from 100% ethanol, IPA or acetone? Just wondering. Cus it may make a difference, judging from prev. experiences with diff. peroxides.

Pyroz - 20-1-2005 at 16:39

I use 100% pure isopropyl alcohol for filtering--- sodium carbonate for neutralisation. And it seems to work rather well. The end product is super dry and nearly scentless.

Hideki, enough with the stories! Pls post relievent and accurate material* thank you.

PainKilla - 20-1-2005 at 17:26

Um, yea Hideki, I don't think you are telling the truth at all. Even ethyl perchlorate (which is IMO one of the most powerful explosives known to man) doesn't cause as much damage you are descrbiing and thorugh blaster's wonderful tests, its obvious he uses more than "1-3 mg."

No need to exaggerate it's power or anything, we are working together trying to make something. No one cares whether it is good or not, it is after all mad science and it is interesting. I don't understand why you need to add validity to yourself when noone cares.

Pyroz - 20-1-2005 at 18:35

tried the spoon test and I put 0.5 grams into a stainless steel spoon and then placed another ontop, compressing the powder. The spoon was then heated to 350C, gradually ouside on an electric hotplate. After several minutes I heard a loud bang and I found the one of the spoons on the grass-- the other spoon was no where to be found--- humm,
---the hotplate hadn't reached full temperature when the explosion occured.
Here a pict of the spoon i found. It isn't much damage, but the explosive force bent the spoon and warped the bowl slightly--- i wonder what the other spoon will look like?

found the other spoon and its really mangled** the bowl has completely inverted itself and the handle has been bent in a U shape ---I'll send the pict tommorow guys.. thanks

[Edited on 21-1-2005 by Pyroz]

100_2643.jpg - 101kB

Never mind... You guys are not reading the posts

Matsumoto_Hideki - 20-1-2005 at 22:37

I have Isoproplyene alcohol (Isopropanol) yes..
I never said the amount is dead on since I cannot measure small amounts of anything I did say 1-3mg range as I compaired this to a weight of a 1mg loratadine tablet used for alergies. Maybe it is more like 6 or so ???? I dunno, It was extreamly small the amount.
No my test wasn't scentific in terms of the weight.
However I seemed to have gotten the DPPP to melt at 160c and then to , only to detonate monents later. The detonation bent the spoon back into a U shape
ie) the handle portion and other than that there was not much damage. I don't know were rosco gets the "major damage" claim from.

BTW: NOT LIKE YOU READ ANYTHING I POSTED HERE
I am giving up on this forum since I have had it with the arrogant anal crap I have to take from some people here!!! :mad:

Mickhael - 21-1-2005 at 00:06

Just from reading how supposedly difficult DPPP is to dry, is it possible its a bit hydroscopic? And how do you filter/remove the water with isopropyl alcohol? I'm not quite clear on the method of that...

Whats left of my batch (20g or so) has been sitting in a paper cup for a couple weeks now, and is broken into little chunks, its turning whiter and whiter on the main surfaces, with a film of yellow on a few outer edges, like its getting purer from the evaperation of the contaminents? Also for the first time today when looking at it, in the same light as i always have...I noticed a sparkle quality appear to the white crystals...

[Edited on 21-1-2005 by Mickhael]

Pyroz - 21-1-2005 at 00:23

DPPP appears to be somewhat hydroscopic. That much is clear. I used Isopropyl alcohol to further elliminate any impurities after I neutrallised left over acid. The use of 100% isopropyl alcohol in general can act as a kind of medium through which evapouration occurs rapidly as it is extremely volitile--- 100% pure Isopropyl alcohol takes the moisture right out of your skin on contact with it!

So, it does work...

[Edited on 21-1-2005 by Pyroz]

Microtek - 21-1-2005 at 03:21

Quote:
Originally posted by Matsumoto_Hideki
I never said the amount is dead on since I cannot measure small amounts of anything I did say 1-3mg range as I compaired this to a weight of a 1mg loratadine tablet used for alergies :mad:



That might explain the apparant discrepancy; if you are saying that 1-3 tablets containing 1 mg of loratadine each weigh the same as the amount of DPPP you are using, then you will have much, much more than 1-3 mg of DPPP.
The tablets obviously contain large amounts of fillers and other ingredients as it is simply not practical to handle pills of the 1 mg size; they would be about one cubic millimeter in size.
100-300 mg for one pill is a more probable figure assuming a quite small pill.

hummm...

Pyroz - 21-1-2005 at 07:35

---I just tried forming a micro tablet sized amount into a compressed chunk and the smallest I could form was 150mg. Even at 150mg the material still was very explosive--- maybe this is what happened with hideki's test? DPPP material density is quite high due to its molecular structure--

Rosco Bodine - 21-1-2005 at 09:04

The small compressed samples which I have ignited have only burned rapidly ,
even in chunks 5.5 mm X ~ 12 mm contained in a cylindrical cavity drilled in a block of hardwood . However at that dimension , the loose crystals low order detonate when ignited . Now the response to impact is certainly there for a smaller amount , perhaps even for a single crystal , but that is an entirely different parameter which has no real bearing upon what will be the response to the material to heating or to ignition .
Many energetic materials give no clue to their potential power when initiated under conditions different from those conditions under which their power is fully realized . Certain preliminary tests like those I am doing only provide some specific information which has bearing upon identifying those conditions where
the potential of the material may be revealed . It may be interesting to know what amount of DPPP will detonate when heated at certain rate to a certain temperature , but such information has no real practical significance . A sufficient amount of just about any primary explosive will deform a spoon to some extent under some condition of initiation , but the data derived from such tests is only pertinent to the long term study of the various parameters of techniques for the destruction of tableware . If there is another point , someone please tell me , as I lack the imagination to see the scientific relevance of the spoon destruction experiments , particularly in the absence of good data concerning the comparable effects on forks and knives , while wondering also if cultural bias has spared chopsticks , or if the wok is being reserved for larger scale tests involving a recipe for DPPP "stir-fry" , when the protective barricade and remote sensors are installed :D

Am I going to get heard ?

Matsumoto_Hideki - 21-1-2005 at 09:39

I get really frusterate with people when they fly to conclusions about what was said/
Sorry I overeacted.
I guess roomate was right "Pyroz" weight could have been more than 1-3mg. I don't know. I will stick to my story as I am somehow getting it to detonate in MUCH smaller quantities than Rosco is. I have not got anything close to Wavefront's picture though which i am sure was several 100mg detonated or ..............?
***************************************I am taking the DV camera tommorrow for sure up to the local range to test fire some BIG DPPP devices and some APAN for fun. One device is a 300g modified Al butane cylinder with a wedged rounded cone at the bottom. I will also use some 150g/m homemade detcord against a target.

PainKilla - 21-1-2005 at 11:33

Instead of bitching and moaning that we arent listening why don't you take a fucking picure or movie. We are going pages and pages off topic because you are exxagerating and then claiming that we are "not reading post."

I will be doing my test today, Ill report later today but probably late tommorow.

WaveFront - 21-1-2005 at 13:41

Matsumoto, maybe it was 100 mg, maybe a little bit more. Edit: maybe 200
This can be slighty off-topic, since it is HMTD, but can help to distinguish between AP and explosives which are really more brissant. Observe how the aluminum dust is burnt in the air, producing metallisations in the proximities.

edit: I agree entirely with Rosco that is necessary a bigger amount to determine the true potential.

http://webs.ono.com/rym/TAPA.WMV

[Edited on 21-1-2005 by WaveFront]

[Edited on 21-1-2005 by WaveFront]

Don't worry movies and pics coming!

Matsumoto_Hideki - 21-1-2005 at 13:49

You will see movies tommorrow late.
I am going to the range, You will have some proof soon enough.
:P

video clip #1

Pyroz - 21-1-2005 at 19:50

Here you are, a video clip of just how explosive DPPP is in small amounts. I honestly didn't expect a detonation in quantities less than 100 mg but I was wrong. In the video I placed 30mg of DPPP into a spoon and spread it out evenly to insure that the crystalline material has equal opportunity to melt. It did not take very long for it to liquify...and then "BANG" I recieved a sharp detonation. AP by comparison just deflagrated and that video is also coming soon.

[Edited on 22-1-2005 by Pyroz]

Attachment: 30mgDPPP.mov (533kB)
This file has been downloaded 1295 times


15-20mg DPPP?...

Matsumoto_Hideki - 21-1-2005 at 22:34

Geeze would you look at that. Rosco I think we have totally different material than what you got if your "DPPP" just sizzles. That detonation on the video nearly bent the spoon. About that amount was detonated by me in a small pile, it liquified and detonated with a bit more power and bent the spoon back into that U shape I was talking about. Try it if you like.

rate of temperature rise

Rosco Bodine - 22-1-2005 at 06:52

You are incorrect to assume we have different materials .

Try a candle and slow gentle heating and you'll see that's the difference . Nearly any explosive can be rapidly heated or dropped onto an already heated surface is even more effective at demonstrating this "cooking off" which has zero to do with the amount or the power of the explosive . Actually this is one of the effects which is responsible for the behavior of "putty" , a few test pellets of which I have drying now . Putty combines the effect of a local cookoff induced detonation with the confinement and densifying effect of the binder which also is energetic and amplifies the output .
By comparing the output of putty made from AP and putty made from DPPP , using equal weight samples of each resting upon a witness plate , some data will be provided of how the small mass cookoff performance compares . This will be useful information , even though it is in no way definitive about what will be the performance of DPPP in different firing schemes where larger quantities are involved . For example HMTD putty detonates in smaller masses than does AP putty , while the loose crystals of AP detonate in smalller diameters than HMTD . So each of the tests I am choosing
are intended to reveal some practical data about the behavior of the sample material , in *weighed * quantities . My tests are working systematically through a series of comparisons with the effects of control samples of already known materials , increasing the quantity incrementally and the performance demands of each test sample so that a good picture of the properties of the DPPP is revealed . And I do have on hand control samples of bona fide 8500+ m/sec test charges for side by side comparisons of metal cutting effects when the tests are up to 3 gram quantitites . By the time I have finished my tests I will know enough about the material to make some intelligent conclusions from not only such physical tests but also from the chemical tests . The residual unused free peroxide remaining in the filtered reaction mixture is one of the chemical tests which should be very revealing . The thermal curve which the reaction follows during synthesis is one factor alone which suggests that Mackowiak's alleged "pentachlorophorone" intermediate is a reach , and perhaps the identification of the reaction endproduct as well is therefore misidentified . But no number of mangled tableware will prove or disprove that . Only pertinent tests involving *measurable* quantities and properly interpreted results accurately reported will tell the true story about DPPP .

Oh ok Rosco, I though you said it woulden't detonate?

Matsumoto_Hideki - 22-1-2005 at 08:51

Rosco, earlier I was under the impression that I was full of it for claiming this material would detonate in (unmeasured) 1-3mg range, turns out this was more like 10-20mg as i stand corrected by my room-mate. OK, but you still have no detonation at this amount, even? BTW I tried a candle and it melts much more effectivly (cooler flame) and then detonates just as you saw in the film. ie) not much difference.

BTW I have an initial report from my university about DPPP, and the results are quite interesting.

[Edited on 22-1-2005 by Matsumoto_Hideki]

ARG! WTF?

Joeychemist - 22-1-2005 at 09:14

Well are you going to share it or what???

We don't like to be teased like dogs Hideki.:mad:

You say you have very interesting findings, and you dangle it right in our face and then you don't deliver?WTF?:mad::mad:

Pyroz - 22-1-2005 at 10:15

Hideki, I have warned you not to mess with this forum...pls post somewhere else for everyone sake.

..just sharing my finding guys.

Thanks for your feedback Rosco and others. I'm doing my best to show some of my findings here. I hope something can be gained by this video data. More tests today, and more video evidence.

[Edited on 22-1-2005 by Pyroz]

WaveFront - 22-1-2005 at 10:24

Rosco, I encourage to you to continue with your scientific method, you will achieve reliable results... and you could even discover other things to do with the precursor, or similar precursors that could be lead to more powerful products :).

Many of us just don´t have laboratory equipment to do measurements or just do small explosions for fun.

vulture - 22-1-2005 at 10:27

The real problem, Matsumoto, is you. You pulled off too many unbelievable stunts for anyone to believe you anymore.

It's called a rep. You might want to read about that and how to conduct scientifically valuable experiments instead of bloating your results to fairytale proportions.

Joeychemist - 22-1-2005 at 10:32

It’s rather suspicious that you two do not act like roommates. I mean hell, if all of us lived in the same building we would have this DPPP puzzle solved by now, you know why? Because we could *talk* about it face to face and we could perform the tests *together*, but it would seem (from you’re posts) that you guys almost don’t even *talk* to each other outside of the forum?

Here is a thought, maybe you guys could do us and this thread a favor by combining you’re posts together from one user name. That would help to slow the growth of this thread.Just a thought.

I know everyone feels that this thread is just too big, and it is becoming harder and harder to go back and find something that was said 2 weeks ago. Maybe we could carry on with this conversation in another thread?

Pyroz - 22-1-2005 at 10:40

"t’s rather suspicious that you two do not act like roommates."

I have been meaning to get rid of Hidekis account for good... I asked the admin to take it off line. But no can do. So Hideki can post somewhere else...I have had it.

I barely speak with Hideki, and I'm not fond of his attitude.

KemiRockarFett - 22-1-2005 at 10:55

Quote:
Originally posted by Matsumoto_Hideki
Geeze would you look at that. Rosco I think we have totally different material than what you got if your "DPPP" just sizzles. That detonation on the video nearly bent the spoon. About that amount was detonated by me in a small pile, it liquified and detonated with a bit more power and bent the spoon back into that U shape I was talking about. Try it if you like.


Hey you!!! Thats not even possible even if we say that the DPPP goes off with 9000 m/s on your spoon it will not be bend at all! The VoD is so high that the result is a hole but than you have to have a BIG amount like several grams on your spoon. PRESSED and maybe forming an jet-beam.
If compare the DPPP with an much more powerful explosive as penthaerytthritoltetranitrate all people reading this can se that you are telling us garbage the hole time. I am sure you never even have seen an acetone or hydrogenperoxide bottle.

putty test 300 mg spherical charge

Rosco Bodine - 22-1-2005 at 11:39

Spherical 300 mg chunks of putty made from DPPP and AP were tested side by side on the lid of a candy tin . Loud reports were produced by each test charge and each produced deep dimples in the thin sheet metal , but neither punctured or cracked the metal and the diameter and shape and depth of the dimples produced is identical .

humm... more curious

Pyroz - 22-1-2005 at 12:12

okay, Rosco
Have you tried putting equal amounts of AP and DPPP into brass rifle cartidges? For example 2 grams side to side...? I am curious as to why my witness plate has two very different marking indicating a power difference. Maybe this is my problem and I did not compress each material with the same pressure? humm,

Rosco Bodine - 22-1-2005 at 14:15

The 300 mg charges are the largest tested so far side by side under identical conditions involving ordinary flame ignition
and self-accelleration of the materials under minimal or no confinement . So far the AP and the DPPP are behaving
* exactly * the same , which is very curious to me too . They even sublime at about the same rate , even though the crystals obtained by sublimation look different . I think a melting point test which I haven't done yet , including a a mixed sample melting point test , is getting higher on my list of priorities for tests to do , at this point . It isn't looking good in the preliminary tests for DPPP , but there are still more tests of the "fire for effect" type larger charge tests to do , especially the picric acid initiating ability tests which are about as definitive as it gets for small charges . With complete detonation of picric acid the test chamber is full of black smoke and coated with black carbon dust like lampblack . An incomplete detonation produces a yellow dye smoke and covers everything in the test chamber with the micronized yellow dye residue dust of undetonated picric acid .

One thing I can point out from the test results so far is that if you are firing a 2 gram compressed chage for a test , you need a loose amount of maybe a quarter to a half gram on top of the compressed 2 gram column , because the self accelleration upon ignition of the compressed material is slow in the open ended capsule tests , while the loose powder achieves low order DDT at the same diameter with greater predictability .
The compressed column will therefore be more desirably initiated by shock from the low order DDT of the loose material , and then the compressed material will lose less potential for its own acceleration from low order to high order detonation .
It is always a good idea in a single component cap of this sort to apply the strategy of using some of the loose material as a primer for the pressed material for this reason that the loose material establishes the detonation wave far more readily than does the compressed material . The rule is general . Without the loose priming layer ,
two compressed charges of identical material could demonstrate very different plates , merely because of the variation in how each accelerated in unpredictable fashion following ignition . If enough charges were tested , indeed some of them might even fail to detonate at all , but only burn , while some others may give excellent plates , and others give a range in between . Eliminating this variable is one of the reasons why matchheads and ignition charges have been standardized for commercial devices so that predictable performance is achieved from one device to the next .

[Edited on 22-1-2005 by Rosco Bodine]

Pyroz - 22-1-2005 at 15:07

Quote:
Originally posted by Rosco Bodine
One thing I can point out from the test results so far is that if you are firing a 2 gram compressed chage for a test , you need a loose amount of maybe a quarter to a half gram on top of the compressed 2 gram column , because the self accelleration upon ignition of the compressed material is slow in the open ended capsule tests , while the loose powder achieves low order DDT at the same diameter with greater predictability .
[Edited on 22-1-2005 by Rosco Bodine]

I have been using a loose powder primer for initiation in all of my tests. But just to make sure I haven't messed up somewhere i'll redo my plate test..on video. I'll show you how I'm loading the cartidges as well. I'm even planning a synthasis video late sunday as well.
A bit of a set back today as the road to the firing range is closed due to heavy rains so I'll have to try again tomorrow. I appriecate your pointers! I would like to contribute as much as I can and solve this "DPPP" mystery once and for all.
Thanks, cheers all!

Rosco Bodine - 22-1-2005 at 15:54

No video is required really , just state precisely what you are doing with loadings , because the performance can definitely vary considerably because of any detail
for small charges particularly , including any priming scheme . The behavior of many explosives can be deceptive below a certain threshold amount which can even be several grams or more . I have seen reports by others testing certain compositions in amounts below their threshold for high order , and using inadequate initiation sometimes too , and have results which speak poorly of those compositions potential . I am not going to make any premature conclusions about DPPP , because I know from tests on HMTD to not be too hasty about the small quantity and small diameter evidence , which may not hint at what occurs next when the quantities and initiation schemes are increased in intensity . And it could also be that DPPP is a "crossover" type of "primary" whose performance is docile as a primary sort of like lead styphnate , and yet has excellent performance when fired as a secondary by another material which has much better performance in small amounts as an initiator . I haven't yet tested DPPP being shock initiated by another primary , even in the scheme where the loose DPPP is used to fire the compressed material . That is likely the method which accounts for your results with the 2 gram charges , where the combination of loose and compressed material in tandem actually constitutes a "firing train" . So far my tests have involved single density , single component charges in only threshold amounts . I look forward to seeing what the heavier loadings and tandem firing train tests will show . I generally go to electrical firing for the larger stuff , and use a low order DDT composition in the electrical squibb ,
like a tenth gram of basic lead picrate .

[Edited on 23-1-2005 by Rosco Bodine]

Dodoman - 22-1-2005 at 17:16

Just performed a few tests today with the 40 or so grams of DPPP that I had.

I made a chaped charge using 2 gm of DPPP. The cone had an acute angle and with a 4 cm standoff. The whole thing was standing on a fome plate. I placed a coin under the charge and lit the fuse. After the detonation I found the plate intact :o. And the coin was not found. I'm sure that nithing happened to it as the plate was not even broken. But the strange thing was that it was covered in fine black dust just like lamp black.

I also made two AN/DPPP (10% by weight) charges and used one to detonate ANFO. Complete detonation.
And the other to vaporise some gasoline in the direction on a flame. The charge detonated but the FAE device failed I guss it had too much gasoline in it.

I have a few pictures and a very low quality video of the failed FAE device that I can post if you want.

Rosco Bodine - 22-1-2005 at 19:55

There is a patent which describes a synthesis of trimeric AP under moderately acidic conditions which are similar to the conditions of acidity for synthesis of DPPP .

GB620498

Mostly the patent describes the use of sulfuric acid , but does mention
that HCl can also be used in lesser concentrations . On page 3 line 29 of
the patent , it states that too large a proportion of HCl particularly at
elevated temperatures favors the formation of chloroacetone . Of course
there is plenty of free acetone in the reaction mixture of the patent so
it is different in that respect from the reaction mixture for DPPP . Anyway
it would seem possible that any traces of acetone in the DPPP reaction mixture
could also be a source for chloroacetone formation , although the potential
concentration would be lowered . From what I have read about the reaction
of H2O2 and HCl , the reaction takes place only slowly , and produces Cl2 , and
also some HClO by the further reaction of the chlorine with water . I have speculated
that the initial reaction of the DPPP precursor during "peroxidation" which is actually
a chlorination , may be favored by warm temperatures , but at the same time it
is also possible that no advantage may be taken of this if it is true , because of
the undesired simultaneous production of chloroacetone or other undesired byproducts .
This is still an open question not fully resolved for me with regards to the synthesis
of DPPP . If the reaction of the H2O2 and HCl does occur slowly , then the rate of
formation of the pentachlorophorone would be limited by that slow reaction providing
the chlorine . In my estimation the chlorination of the precursor is the least well
understood part of the synthesis of the DPPP .

chemoleo - 22-1-2005 at 20:32

Hmmm - it seems you are posting exactly the same thing at the E&W forum. I don't quite understand what the significance of this is.
It doesn't prove or disprove anything.

Chloroacetone - maybe this is a later product that makes you all cry literally, but certainly NOT during the reaction between HCl and acetone (having done it myself - it's harmless).
Btw, I found that leaving the mixture of 37% HCl and acetone for one week at room temperature would still produce this dark red oil, visibly no different to the mix that was heated at 65 deg C for 90 min.
I am tempted to believe that the production of the 'DPPP precursor' is a temperature-dependent process, I.e. if heated, it will go faster, if not heated, it will just take its time (a week). But the reaction is the same nonetheless, no? I will test for the appearance of water-insoluble oils that somone described above, using this particular mixture.
Nice and proper science :)

Btw, if someone is interested as to what conditions are NOT to be employed to get 'DPPP', here is an attachment on the formation of acetone peroxides in the presence/absence of acid. THanks for forwarding this Bromic :)
It gives a full mechanism for which conditions are required for producing AP, and, more interstingly, the conditions required to form acetone peroxides which are NOT cyclic. Check it out.
If someone pursues this. please create a separate thread, as this thread is big enough as it is!

Attachment: acetoneperoxides.pdf (582kB)
This file has been downloaded 1225 times


Rosco Bodine - 22-1-2005 at 20:59

Quote:
Originally posted by chemoleo
I don't quite understand what the significance of this is. It doesn't prove or disprove anything.
The significance is that with elevation of temperature of a mixture of H2O2 and HCl that chlorination activity increases , and chlorination is what is being done to the precursor to form the next intermediate for the DPPP .
Quote:

Chloroacetone - maybe this is a later product that makes you all cry literally, but certainly NOT during the reaction between HCl and acetone (having done it myself - it's harmless).
Right , it isn't the reaction of the acetone and HCl , but the reaction of the H2O2 and HCl which is producing chlorine that then reacts with the acetone to produce chloroacetone . This production of chloroacetone is analogous to the production of pentachlorophorone , only the precursors are different . The chlorination mechanism is the same .
Quote:

Btw, I found that leaving the mixture of 37% HCl and acetone for one week at room temperature would still produce this dark red oil, visibly no different to the mix that was heated at 65 deg C for 90 min.
I am tempted to believe that the production of the 'DPPP precursor' is a temperature-dependent process, I.e. if heated, it will go faster, if not heated, it will just take its time (a week). But the reaction is the same nonetheless, no? I will test for the appearance of water-insoluble oils that somone described above, using this particular mixture.
Nice and proper science :)
That squares with what I am seeing too . Only with the ratio of 95 ml HCl 31.45% to 100 ml acetone , my sealed bottle is reaching the "cloud point" at 3 1/2 days , 84 hours , and then the surface accumulation of insoluble oily byproduct begins . I know the reaction rate is sensitive to the molar ratio of HCl to acetone , and of course to time and temperature . Freezing the mixture tends to virtually stop the reaction , but not totally .

This discussion of DPPP which began here at this forum has followed a parallel at times over at E&W with similar thoughts and experiements , and many of the same people having membership at both boards . So I ask your understanding to simply paste any pertinent posts here and there when it fits into the point of discussion , avoiding having to retype and reword saying the exact same thing in lengthy posts at the separate forums .
The information as follows fits this parallel discussion and elaborates on the chloroacetone / pentachlorophorone "connection" .

Nobody that I know of is talking about the formation of chloroacetone from
reaction between acetone and HCl . What is being described by the GB620498 patent is that in a reaction system containing acetone along with hydrogen peroxide and HCl , that increased concentrations of HCl combined with increased temperatures favors increased chlorination of the acetone to form chloroacetone as an undesired byproduct ,
instead of the intended trimeric acetone peroxide . This is good information about the reaction condition where hydrogen peroxide reacts with HCl to produce chlorine , which is different from the condition where peroxidation would be the desired purpose for the hydrogen peroxide . The intended reaction for the phorone dihydrochloride is to be a chlorination reaction resulting in conversion of the phorone dihydrochloride to pentachlorophorone . The chlorine is being supplied by a side reaction from H2O2 and HCl , the HCl being present in some excess in the red phorone dihydrochloride solution , because more HCl than required by theory was used to form the precursor
originally , and/or some extra HCl was added to the red precursor solution just before the addition to it of the H2O2 is begun . The production of chlorine is favored by warm temperatures and excess HCl , according to the GB620498 patent . And from what I have read elsewhere about the reaction of H2O2 with HCl , the reaction takes place slowly ,
therefore it is reasonable that a very slow addition rate of the H2O2 to the warm and HCl rich reaction mixture would favor the chlorination reaction preferentially to a
peroxidation reaction which would be favored by opposite conditions , such as cold temperatures and lower concentration of HCl .

Early in the discussion of the chemistry of the reactions stated by Mackowiak for the
formation of DPPP , I stated that I had reason to wonder if perhaps the formation of the pentachlorophorone would be favored by warm temperatures , followed by cooling of the pentachlorophorone solution for completing its conversion to DPPP . That was a "guess" about the reaction which is supported by the additional information which is provided by GB620498 . So it would seem likely that since 6 of 11 of the moles of H2O2 to be added to the phorone dihydrochloride are consumed in the chlorination reaction producing pentachlorophorone , that 6/11 of the portion of total peroxide should
be added to the reaction under conditions which favor that intended chlorination reaction . To reiterate , the conditions favoring chlorination are excess HCl , warm temperatures , and slow addition of the H2O2 . Of course it may not be possible to exploit such a strategy for the chlorination unless the pentachlorophorone is a stable intermediate
which may form in increasing concentration without peroxidative decomposition in advance of the point where the mixture will be cooled for conditions favoring peroxidation of the pentachlorophorone to DPPP . Ideally , if the pentachlorophorone is a stable intermediate which cooperates in accumulating to a high concentration without any further tendency towards decomposition , then the formation of the pentachlorophorone intermediate could be accomplished by performing the reaction *warm*
during the time of addition of the first 6/11 of the peroxide required for the eventual formation of all the DPPP . When all of the pentachlorophorone intermediate has formed , the mixture would be chilled very cold before the remaining 5/11 of the peroxide is added . So the addition of the peroxide would be done in two stages , with the first portion being added to a warm reaction mixture favoring chlorination , and then the second portion of peroxide added to a cooled reaction mixture favoring peroxidation of the chlorinated intermediate having accumulated during the warm first reaction stage .

The volume of H2O2 stated by Mackowiak at 2 volumes of 30% H2O2 for each 1 volume of acetone is deficient the amount of theoretical requirement for the reactions as Mackowiak has the reactions written . A minimum of 2.55 volumes of 30% H2O2 for each 1 volume of acetone would be required for the stoichiometry to be satisfied where 6 moles of acetone are eventually converted to 1 mole of DPPP .
Closer to 3 volumes of 27% H2O2 for each 1 volume of acetone would be required by theory . Anyway , I find such an error in stoichiometry found in a patent
to not be reassuring since the technical disclosure of chemical reactions is a highly proper place for exactness about such quantities .

[Edited on 23-1-2005 by Rosco Bodine]

RANGE TEST COMPLETE w/ video

Pyroz - 23-1-2005 at 19:25

Here is the range test for an 80 gram shaped DPPP charge. The test target was 4mm thick stainless steel pot...enjoy.

update for anyone who wants to recreate this experiment...here is how to do it.

1)get a small metal butane refill cylinder. The bottom of the cylinder is shaped for a perfect punching charge as it is concave
2) fill the cylinder with 80grams of highly compressed "DPPP" material and insert a detonating cap 1/4 of the way into the filler---I used a 1.6gram cap which was a crimped .223 remingtion shell casing with a 1 meter long cXa thermalite fuse attached to it. I had 30seconds to retire behind a steel reenforced backstop---:D

[Edited on 24-1-2005 by Pyroz]

Attachment: 80gramDPPP.mov (938kB)
This file has been downloaded 2287 times


Joeychemist - 24-1-2005 at 13:48

See hideki, you have told too many lies to even remember what you posted a few days ago.

I was referring to one of the videos you posted at RS, (The 20mg spoon video, not the new 80g video, the one before) the same spoon video that pyroz posted page 26 of this thread, but he clearly said it was 30mg. the title of the attachment you posted at RS clearly reads 20mg DPPP but is the same video. I find it very suspicious that pyroz would post the same video saying it was 30mg and you say its 20mg.So again I ask you again, what was it? 20 or 30mg? It is obvious that “one” of you or “both” are exaggerating.


Edit by Chemoleo:
Good idea, let's not waste more bandwidth on pointless arguments, which includes yourself too. I deleted the relevant posts above. Harsh measure, yes, but this is where the buck stops :)
Guess we have to live with some exaggerations/errors, as the constant criticising does produce nothing but more bickering. Blatantly false posts will be just corrected.
And, 20 vs 30 mg is already an improvement to 1-3 mg vs 100 mg.
Apart from that, you are always welcome to correct the errors/exaggerations with hard data, that is, your own experiments :)

[Edited on 24-1-2005 by chemoleo]

Lets get down to the recent video and thoughts?

Matsumoto_Hideki - 24-1-2005 at 14:45

Thank you chemelo..
I appreciate your kindness very much. I really wanted someone to analyize the video that Pyroz posted. I see something major here as it seems that there was a signifigant enought energy to atomize the aluminum can and ignite it hence the white flash before the pot starts to get airborn. This is what it looks like to me?

:o ?? any thoughts

Oh and bTW just on that "remembering and supposed lying thing" thing chemeleo, I have short term memeory loss due to a car accient I was in while I was finish school at Tohoku Daigaku near Sendai. So I can't help much.
Understand plz. My memory short term is bad = Brain damaged. yes it may be funny to you guys, brain damaged Japanese person.
:mad:

[Edited on 24-1-2005 by Matsumoto_Hideki]

[Edited on 24-1-2005 by Matsumoto_Hideki]

chemoleo - 24-1-2005 at 14:54

Sigh. Matsumo you aren't off the hook.

I don't think you can conclude much from the video, except that it is an explosive with a reasonable VoD.
Atomised Al ... you meant stainless steel I thought.

Regardless- this video is interesting, but not really of great significance as it doesn't show the comparative power to another HE, or even that of AP.
And this is what we should be after. So please let's focus on that.


[Edited on 24-1-2005 by chemoleo]

Butane cylinder is Aluminum not steel

Matsumoto_Hideki - 24-1-2005 at 14:57

Chemeleo I think pretty sure pyroz did say the can was Al not steel.
The pot was 4mm steel that I do Know.

Any comment on the shockwave and other things in the video. VOD I cannot measure nor can pyroz.

[Edited on 24-1-2005 by Matsumoto_Hideki]

Rosco Bodine - 24-1-2005 at 15:25

A more revealing test would be what a film canister size charge does to 1/2" thick plate . No shaped charge is needed .
Something comparable to PETN will hole the plate with no problem .

See page 2 of US5140908 for some plate test data for 35 ml volume charges fired against 12 mm thicknes steel plate . Sensitized nitromethane which is only something like 10% stronger than ordinary TNT blows a hole more than six inches across through 12 mm plate .

[Edited on 24-1-2005 by Rosco Bodine]

Pyroz - 24-1-2005 at 16:43

I am planning on doing a film canister filled with some compressed "DPPP" sometime next week when i get around to it. It is very difficult for me to say that this material is in fact as powerful as the patent claims to be...but hey, who knows ?
I saw a pretty decent sized explosion yesterday but that doesn't mean much...and this video was more for general info and such. One thing i left out was the dime sized indentation left behind on the 3cm thick steel rebar which was also bent from the force of the blast..which looked like a oxyacetlyene torch was been used to slice into it ---if i'm not mistaken this is a product of high velocity jetting? I think one of the reasons why the shape charge didn't do more damage to the plate below was the fact that most of the gasses had time to escape out the sides thus lowering the downward velocity of the jet. As well the steel pot (top to bottom was 15cm) --- so that may be another reason.

a note to everyone:
The previous video on pg 26 was 30mg of "DPPP" powder melting and detonating...not 20mg as hideki keeps posting.

Rosco Bodine - 24-1-2005 at 17:16

There have been a few experiments done by me over the years with different organic peroxides , and while some of the compositons are "in the neighborhood" of TNT , *none* of the compositions are anywhere near the nitrated polyols in power . The strange thing is that the peroxides make a helluva bang like they are really high output just going by the noise , but when you look at the actual work done on the target you just don't find
the sort of damage that the noise would have you expect to find . It is sort of the same story for lead styphnate and lead azide if you detonate say 50 mg of the loose crystals of each on a thin sheet of aluminum . The lead styphnate will make a helluva loud noise and barely scratch the metal . The lead azide will make more of a short quick snap like the sound a plastic ruler makes if bowed up slightly and allowed to fly downward against the surface of a desk , a sharp snap more than a loud echoing bang , and yet the difference in the work done to the target is astonishing because a clean edged hole is found to be cut right through , complete with the "missing metal" effect and not a lot of banana peeling on the underside either , the metal which was in the opening is just gone , atomized . So never be deceived by the noise signature of a particular composition as it has nothing to do with the power or brisance of what made the noise .

Pyroz - 24-1-2005 at 18:12

Quote:
Originally posted by Rosco Bodine
...yet the difference in the work done to the target is astonishing because a clean edged hole is found to be cut right through , complete with the "missing metal" effect and not a lot of banana peeling on the underside either , the metal which was in the opening is just gone , atomized .


Well, that makes perfect sense. The charge itself was shaped --the bottom of the cylinder was concave so wouldn't that cause a "punch" and "peel" type of blast regardless of VoD? i don't know because I've never tested PETN or RDX before..my loss, oh well. I've included a close up image of the top and the bottom of the pot itself...the video quality stills aren't great but the picture quality from my digital camera is much better... so have a look :)

update:
I think I will try making a conventional shaped charge with a standoff w/ copper insert. This should blow a hole in 1" thick plate steel --- and make a clean hole if the velocity is anywhere near 9000m/sec.

[Edited on 25-1-2005 by Pyroz]

endresult.jpg - 151kB

WaveFront - 25-1-2005 at 01:03

Want data? Repeat the same experiment with AP

Want fun? Mix with KClO3. In small amounts it is close to HMTD. :)

EDIT: and I am not talking about noise, but shattering power

[Edited on 25-1-2005 by WaveFront]

.. I don't understand

Matsumoto_Hideki - 25-1-2005 at 08:34

Quote:
Originally posted by WaveFront
Want data? Repeat the same experiment with AP

Want fun? Mix with KClO3. In small amounts it is close to HMTD. :)

EDIT: and I am not talking about noise, but shattering power

[Edited on 25-1-2005 by WaveFront]


Sorry mix what with what to get shattering power?
AP with KClO3?

WaveFront - 25-1-2005 at 12:00

My "DPPP" was pretty bad making holes in thin metal plates; in a similar way to AP, it tends more to bow the plate. (I use only small amounts).
On the other hand, HMTD is very good in this task. (As seen in my video posted before)

When I mixed my "DPPP" (or whatever the impure thing that in fact it is) with finely powdered KClO3, there was little if any increment of BOOM, but the plates are perforated. It is not a clean cut, but you will appreciate clearly the difference.
I use the product by heating it in aluminum foil. The Aluminum metallisations are better too.

AP and Chlorate? May be I do tests with both mixes to compare


The HMTD also makes good mixes with chlorate, but what I remember is an increase of the power (bigger hole and more noise)

DPPP chemistry related , 90+% yield conditions

Rosco Bodine - 25-1-2005 at 13:30

After doing several experiments under varying conditions , I have found a set of conditions which has produced very good yields which are in close agreement with the DPPP patent . The conditions for achieving the highest yields so far obtained are as follows .

100 ml acetone was placed into a bottle and then 95 ml of HCl 31.45% was added and the bottle sealed . After standing for 30 minutes the bottle was warmed in a water bath at 65 C until the solution had an orange color . The bottle was removed from the heating , and allowed to stand at room temperature for 72 hours and then placed into a freezer to cool overnight at -10 C . 280 ml of 27% H2O2 in a plastic bottle was placed in the freezer also overnight . A 1000 ml tall form beaker was placed in a 3000 ml plastic bowl and set upon a stirplate . Into the beaker was placed a 40 mm diameter cross form stirbar and a thermometer leaned diagonally with the tip against the bottom wall of the beaker .
An addition funnel was set in a support above the beaker . 1500 ml of ice cubes was distributed around the outside of the beaker and about 75 grams of sidewalk deicing salt ( calcium chloride / sodium chloride ) was sprinkled over the ice cubes . The cold precursor was poured into the beaker , and the addition funnel was filled with the cold H2O2 . The stirrer was started slowly and the temperature reading was -10 C . 40 ml of HCl 31.45% was poured into the stirred precursor and the temperature rose to -2 C . The addition of peroxide was begun immediately at about a drop per second and then gradually increased allowing a fairly rapid rise of temperature to 15 C , and regulating the rate of addition to maintain 15 C , which appeared to be a very smooth reaction temperature allowing a fairly rapid run in of the H2O2 , in a small stream as the addition proceeded . Temperature actually began falling on its own towards the end of the addition even with the valve nearly full open . The mixture had the appearance of eggnog , a smooth emulsion like appearance with no crystals visible , and the mixture gradually thickened , requiring higher and higher stirring rates to maintain the mixture in circulation . There was only a trace of any insoluble byproduct globules , a very tiny droplet maybe a tenth gram in mass . The mixture gradually cooled down to about 0 C after an hour past the end of addition . Stirring was stopped for intervals of 1 hour and then the mixture stirred up again . This was repeated twice and then the mixture allowed to stand overnight in the salted ice . The next morning the mixture was at - 4 C and had set up into a semisolid floating mass of nearly white crystals occupying three fourths of the volume of the mixture with clear liquid underneath .
200 ml of distilled H2O was added and the mixture stirred up to a pouring consistency so it could be filtered . The
mixture was poured into a filter and the residue rinsed from the beaker into the filter . The filter was removed and set onto a blotter to remove residual liquid ,
and then the filtered mass was rinsed from the filter into a clean beaker with 300 ml distilled H2O . A stirbar was added and the mixture stirred up with the distilled H2O . 10 ml strong ammonia water was diluted to 200 ml with distilled H2O and poured into the stirred mixture for neutralization of residual acidity . After 10 minutes stirring the mixture is filtered and dried . The material dried to a free flowing powder weighs 98 grams . A few percent of residual moisture remains but not much . 88.6 grams would be 90% of theory and 98.5 grams would be 100% of theory . So this yield which I have gotten is nicely in agreement with the patents reported 90% yield .

This result also presents an opportunity for testing the residual reaction liquid for unreacted H2O2 . If the substance produced has a structure agreeing with the patents designation as DPPP , then there should not be much H2O2 left unreacted in the mixture . What I propose to do is to repeat the synthesis under the same conditions as what are supposed to be producing a nearly quantitative yield of "DPPP" , and when the reaction is complete , to then add an equal amount of acetone as was used to form the precursor to the "spent" reaction mixture and allow it to react further in the cold and produce any more precipitate that it would produce from any residual H2O2 ( which shouldn't be present ) if the reaction mixture *did* form DPPP originally . After adding more acetone , if there is a substantial precipitate of AP produced , increasing the weight of product substantially beyond what is the 98.5 gram theoretical yield for DPPP which had been "supposed" to be what was the first product , then it will be a certainty that the first product was actually not DPPP , but likely some AP isomer or variant instead . This will have been established by the "proof by synthesis" method which will have stoichiometry revealed not consistent with the first product having been DPPP . This weekend
I hope to get around to doing this experiment for "chemical sleuthing" the nature of the spent reaction mixture , to see if it is or is not what it is "supposed" to be , making the case for or against DPPP ........ quietly , by one entirely shockwave free method :D All this is in keeping with the axiom there is more than one way to skin a cat .

[Edited on 25-1-2005 by Rosco Bodine]

fatkangaroo - 25-1-2005 at 14:26

I just attempted the DPPP.
150ml of 30% hydrochloric acid was added to 140ml 100% acetone. I put a lid on the jar and put the jar in a hot water bath in a electric frypan on 80 .C for 3 hours. I saw the same colour changes that have been reported in the thread from clear to light yellow to dark yellow to brown to amber. I stoped heating and put into frezzer overnight. By morning there was a couple of drops of black oil floating on the top and and gram of green- yellow crystals on the jar lid. Added the 50% peroxide in a ice bath. The second the peroxide hit the solution crystals formed straight away and there was a temperature rise. 5 minutes later the jar was just about full so I filtered and washed the crystals. They came out white and looked and smelled just like AP. I have put the filtered solution back into freezer in the hope maybe now the DPPP might form.

Pyroz - 25-1-2005 at 16:39

Quote:
Originally posted by fatkangaroo
By morning there was a couple of drops of black oil floating on the top and and gram of green- yellow crystals on the jar lid. Added the 50% peroxide in a ice bath. The second the peroxide hit the solution crystals formed straight away and there was a temperature rise. 5 minutes later the jar was just about full so I filtered and washed the crystals. They came out white and looked and smelled just like AP. I have put the filtered solution back into freezer in the hope maybe now the DPPP might form.


Well, the indication of yellow green crystals means that phorone-isomer has formed... so at least his part of the reaction sounds correct. The addition of HCl after the phorone solution has been chilled to -5C or less as a catalyist must be done before the slow (drop by drop) addition of conc. hydrogen peroxide. I have found that when the temperature gets above 10 degrees C for the peroxidation process of phorone isomer seems to produce a very similar material to AP, but further investigation reveals that the crystal structure is vastly different. The best explosive properties are obtained when the material stays in a temperature below 0 degrees C throughout the reaction process. You should be left with a very pale sulphur yellow/green crystalline material that should smell slightly camphorus after purification in pure water/carbonate and isoproply alcohol.

[Edited on 26-1-2005 by Pyroz]

Rosco Bodine - 25-1-2005 at 18:53

The reaction temperature has a definite optimum range where good yields are produced , and excursions even briefly outside the range , particularly in the upward direction will cause the yield to be reduced substantially . The 15 C which I have found is limiting is in contrast with the limiting temperature of 30 C described by a patent GB620498
for trimeric acetone peroxide . I find this difference in limiting temperature to be interesting .

The temperature for the DPPP reaction does give best results in the cool to cold range . But the greatest yield which I have gotten with very good cooling and careful control of the rate of addition is with the temperature not above 15 C . Also for the temperatures in the cool to cold range there is not produced the irritant byproduct , and the odor is very mild and the color very nearly white especially after the mixture stands in an ice bath for six hours or more after all the peroxide is added . The high yield batch which I described a couple of posts above actually had a pleasant odor and no irritant properties . The smell reminded me very much of the smell of ripe bananas on the wet material and faded as the material dried . The smell of the dry material is very faint and to me smells almost exactly like pyrethrin based aerosol mosquito spray . The true color of the material is colorless , as proven by sublimation , where all colored samples leave a tiny amount of yellowish residue after the sample is sublimed away , and all the crystals which condense from the vapors are colorless .

P.S. The limiting temperature is possibly related to the amount of excess of HCl which is present . It is my guess that the more the excess of HCl , the colder will be the limiting temperature .

[Edited on 26-1-2005 by Rosco Bodine]

Pyroz - 25-1-2005 at 19:55

I am curious if just about any acid could be used to create Phorone -isomer. How about replacing Hydrochloric Acid with concentrated Nitric Acid w/ concentrated Sulphuric Acid? I wonder if it might help create a more energetic substance?

Rosco Bodine - 25-1-2005 at 20:05

If the chlorine containing intermediates are essential , and it looks as if they would be for the DPPP , then other acids would not work , except for other halogen acids like perhaps HBr or others .

This would actually be a good experiment to see if using sulfuric made no difference and you still got what seems to be DPPP ,
which would pretty well prove that what you suppose is DPPP is actually something else , maybe not AP , but for sure not DPPP either .

PainKilla - 25-1-2005 at 20:07

The purpose of this experiment is to possibly eliminate the phorone part (i dont beleive its possible this way) from "Dppp" ( non existant). If any acid can be used then it is completely relevent towards H+ instead of Cl-. If this is the case, then most likely phorone is not part of the process since h2so4 with acetone makes*mostly* mesitylene. However, if I get small yields of DPPP, then it is probably a phorone derative. We will see....

O yea, it is quite possible that this is merely tetrameric AP. I mean, there is no other way to form it except via CHLORIDE salts. Therefore, if my experiment doesn't bear fruit to a product, then this is either a phorone derative OR tetrameric AP, which has only been SOMEWHAT succefully formed using chloride salt catylsyts (sncl2, sncl4 etc). Even using these methods, note that yields are 40% so therefore it is part tri/dimers too.....

In other words, theres an excellent chance this is not DPPP bit simply TeAP. I think this is much more plausible. It's obviosuly stable enough to exist, which is more than we can say for DPPP.

[Edited on 26-1-2005 by PainKilla]

Rosco Bodine - 25-1-2005 at 20:25

One thing I can say pretty conclusively is that our suspected DPPP is *not* tetrameric AP as I have on hand thirty grams or so of tetrameric AP and it is a quite different material in volatility , density , minimum quantity for DDT , ect .
And the synthesis of tetrameric AP is very straightforward . It is a room temperature synthesis too , no cold temperatures required .

PainKilla - 25-1-2005 at 20:30

The only REAL TeAP i have seen is with the use of SnCl4 for even decent yeilds. I ahev not seen any other ways. I almost positive that what you have is not TeAP. TeAp is supposed to subliminate almost not at all.

Rosco Bodine - 25-1-2005 at 20:49

What I have is definitely tetrameric AP and this was confirmed several ways ,
volatility way lower than AP , different explosive properties , and different crystal density and appearance . The yield was 44% using 75 ml of acetone with 125 ml of 27% H2O2 which was mixed at room temperature , and while rapidly stirred
was treated very slowly by an injection below the surface of 6 ml of H2O solution containing 2.5 grams of SnCl2 , which made a "frying sound" upon contact with the mixture from the vigorous reaction . The yield was 42 grams of sparkling crystals . In a loosely covered container the weight loss after one year was 25% ,
which is less than half the loss for a like control sample of AP stored beside it in an identical container .

PainKilla - 25-1-2005 at 20:53

Ah I see you used the SnCl2 way, but you msut take into account that not only TeAP was formed. I think its like a 35% yield using SnCl2. We will see soon though :p.

fatkangaroo - 25-1-2005 at 20:59

My batch is now fairly dry. I also made a batch of AP at the same time. The differences between the two substances that I have are. The DPPP powder has a very faint yellow tint not pure white like AP. AP is very "sparkerly" the other powder is not. I guess the true test is the explosion test which I will do. I will use tic tac containers containing 25 grams of both powders and see if there is any difference in power. They are both primarys explosives thats for sure. They look pretty similar when a tiny rice grain is ignigted by a match in the open. They smell similar but not identical.

Rosco Bodine - 25-1-2005 at 21:39

My intuition about the DPPP is that the structure likely would be different from
what is Mackowiaks idea and diagram in the patent . I am more inclined to believe in a different more compact symmetry for such a possible compound produced by reaction conditions of this sort , as opposed to the page wide DPPP molecule which the patent shows . To me what seems more plausible is a symmetrical tetrachlorophorone or hexachlorophorone intermediate , which is then peroxidized to a monophorone triperoxide , that is a six oxygen monophorone derivative . This just seems more believable to me than
the more complex molecule which the patent proposes . I can see where these
monophorone triperoxide molecules could add to each other at the ketone carbonyl group including yet another peroxide bond there in formation of dimer , trimer , or tetramer , cyclizing in the same ways as does acetone peroxide . This would seem to be more consistent with the known molecular models for ketonic peroxides . As strange as it may sound , I can actually visualize a cyclic triphorone tetraperoxide ( three phorones with four peroxide groups each ) as being more likely for reasons of symmetry and cyclization , than the "diphorone pentaperoxide" linear compound proposed by the patent .

[Edited on 26-1-2005 by Rosco Bodine]

Chris The Great - 25-1-2005 at 23:11

I beleive that the DPPP is very likely to be a large mixture of many chemicals. Hideki's videa actually sorta supports my view. When the explosion happens, directly after there is alot of deep orange flame. This doesn't look like the flame of CO or C burning, but like heavier compounds. Of course, they would probably all be broken down in the explosion....still, usually fire isn't seen after a detonation.

The shockwave seen in the video looks more like heat to me as well. Certainly is loud though :)

Near the beginning of the thread a link was posted to a google group where this was discussed (4 replies I think, about a week ago). It was suggested by someone who seemed to know the theory behind chemistry, that chlorine will be added to the phorone as the patent states, but not to the methyl groups. If the chlorine could be added, then there really wouldn't be any reason for it to stop either, and so all four methyl groups could get a chlorine on them. Even if the chlorine doesn't go onto the methyl groups, I would except four chlorines to stick to the main carbon chain, rather than three.

This wouldn't happen to all of them, so the total curve might seem to follow the route shown in the patent. However, it's probably going to be a mix of very large molecules with alot of O2 groups and some small molecules without any O2 at all.

Also, what about the O=C bond? In acetone this is broken down, perhaps tetraphorone derivatives are formed as well by peroxidation of these bonds?

Just some thoughts, don't really know if any of them are actually correct however.

video thoughts pt2

Matsumoto_Hideki - 25-1-2005 at 23:55

1) Video belongs to Pyroz not me.

2) That distortion was most defently a high speed shockwave as this was conformed by a physics assistant prof at University.
BTW He also enjoyed the video. :) nice to know that people still enjoy a good detonation once in a while:)

3) I don't think my DPPP was a mix at all as this material was filtered many times with pure isopropylene alcohol. the material left behind was totally prismatic in structure, "cubic". I still am NOT 100% sure it was totally pure, but I am at least 95% sure that it was.

4) Orange flashes can also be seen from PETN, TNT and RDX I am not so sure this has much to do with impuirities.???

Rosco Bodine - 26-1-2005 at 06:46

Quote:
Originally posted by Chris The Great
I beleive that the DPPP is very likely to be a large mixture of many chemicals.
The crystals obtained from slow sublimation are mostly uniform in appearance and this result indicates a relatively pure single compound .
Quote:

Near the beginning of the thread a link was posted to a google group where this was discussed (4 replies I think, about a week ago). It was suggested by someone who seemed to know the theory behind chemistry, that chlorine will be added to the phorone as the patent states, but not to the methyl groups. If the chlorine could be added, then there really wouldn't be any reason for it to stop either, and so all four methyl groups could get a chlorine on them.
The extent of chlorination is controlled by temperature and the concentration of HCl . If the reaction is run very hot with high HCl concentration , so that the chlorination activity prevails , then no peroxidation occurs , and a dense yellow insoluble oil settles to the bottom of the reaction mixture , which is believed to be a polychlorinated phorone derivative or polymerized product . This heavy oil will not peroxidize even when separated and attempted to be peroxidized directly in a fresh reaction mixture . Cool but not freezing cold temperatures having a moderate acidity present a combination of chlorination and peroxidation potential , so that either reaction may proceed without one or the other being favored . The theory suggesting formation of DPPP relies upon the assumption that the sequence of reactions simply follows the path of least resistance , with the reactivity potential for each possible combination establishing the trend of the reactions which predominates for the pathways "most likely" to occur first , second , and third , from the triacetone dialcohol . My guess is that the pentachlorophorone is not a distinct intermediate , but the chlorination and peroxidation occurs in an alternating fashion through a series of intermediates which are stepwise chlorinated and peroxidized , in a way that pentachlorophorone never even exists as an actual distinct compound found in the reaction mixture . Thus pentachlorophorone is purely a speculative intermediate presented as an explanatory example for a more complex reaction involving many steps and many intermediates which appear as an alternating chlorination and peroxidation .
Quote:
Even if the chlorine doesn't go onto the methyl groups, I would except four chlorines to stick to the main carbon chain, rather than three.

This wouldn't happen to all of them, so the total curve might seem to follow the route shown in the patent. However, it's probably going to be a mix of very large molecules with alot of O2 groups and some small molecules without any O2 at all.

Also, what about the O=C bond? In acetone this is broken down, perhaps tetraphorone derivatives are formed as well by peroxidation of these bonds?
For acetone peroxide this is where the peroxide group is introduced , and never involves the terminal methyl groups whatsoever . The CO group takes on an additional O and then the COO links to the "backside" of the central C on the next acetone peroxide , with three such units forming a cyclic ring bonded at the central carbons as
COOCOOCOO-->( this last "O" to the back of the first "C" )

Pyroz - 26-1-2005 at 07:59

Quote:
Originally posted by Rosco Bodine
...To me what seems more plausible is a symmetrical tetrachlorophorone or hexachlorophorone intermediate , which is then peroxidized to a monophorone triperoxide , that is a six oxygen monophorone derivative . This just seems more believable to me than
the more complex molecule which the patent proposes .


I would agree with this statement... however, couldn't a more complex molecule form if the temperature was kept lower and the exact or double to the amount of hydrogen peroxide were to be added? humm, this part is rather curious to me..

Rosco Bodine - 26-1-2005 at 10:14

Because phorone is a ketone having an active carbonyl group , it is even plausible that the first intermediate is phorone monoperoxide , or phorone dihydrochloride monoperoxide having an O added to the carbonyl as occurs for other ketonic peroxides . This could cyclize in the same way as trimeric or tetrameric acetone peroxide , at the carbonyls , before anything further occurs in the way of chlorination or peroxidation involving the terminal methyls , or middle chain methylene groups . Because of the
potential for either chlorination or peroxidation occurring , it is difficult to visualize what reaction follows what other reaction . The determination of residual unreacted peroxide which remains in the reaction mixture should provide useful information for making an educated guess about what is the true identity of the substance we suppose is DPPP . Really what should be done is some thorough and professional analysis in a fully equipped laboratory , performed by someone who knows what they are doing . Some of the rough analysis can be done with basic technique and tests ,
which is all that I am doing , to satisfy my own curiosity really . The basic tests of sublimation and melting point for separate and control samples , and also for mixed samples should be reavealing when the results in total are examined .
One of the tests I intend to do regarding the experiment where extra acetone is added to the spent DPPP reaction mixture , is to do a sublimation and melting point test on the mixed product if an unaccounted for increased yield is obtained . If that mixed sample behaves in the same way as a separately made sample of "DPPP" made by the conventional route , then that test result will basically nail the coffin shut that DPPP and AP are are chemically identical . There are both chemical tests and physical tests as well as detonation test results which will all three be compared for any inconsistency before I declare any conclusive finding , so that I will have good basis for my own conclusions more than just guessing . With regard to the work done at university laboratories , by students or professors either one or together , those opinions or results are no better than the competency and pertinence of the tests which are done . A fancy technical sounding writeup which is opinion based and involves no revealing test results nor good science and scientific method substantiating its findings is basically nothing but a load of bullshit , even when signed by a PHD . Good science on the other hand speaks for itself with results which make the case for the theory as proposed and validated .

fatkangaroo - 26-1-2005 at 14:20

Just returned from a quick test. Tic-tac containers were used each one had 15 grams of powder untamped. One had the AP one had the yellow AP. The charges were put on a solid steel manhole cover. Both charges were blown-The yellow AP gave a loud bang little bit of black smoke and no smell after detonation. The original stuff gave a louder bang and there was a smell after detonation. Both charges had no effect on the manhole cover. The yellow AP had left a small black stain about 1/10 of the total container size. I would of thought that if the yellow AP was DPPP it would of least done something to the plate. I didnt hang around long had a quick look and took off. I also did some micky mouse basic impact tests, you know just puting match head size bits on the ground and hitting with a hammer and draging the hammer across the powder. They both are very sensitive and the original AP detonates in much smaller amounts. I have plenty of powder left so I will do a couple more tests then flush it down the toilet. I dont think this stuff I have is DPPP.

Pyroz - 26-1-2005 at 16:25

Quote:
Originally posted by fatkangaroo
The yellow AP gave a loud bang little bit of black smoke and no smell after detonation.

This material you have is unpure--- it should not burn with any smoke at all nor should it detonate with any smell either. The material that I created is extremely pale green-yellow, almost white and has a camphorus/bugspray odor to it with cubic crystals. I find it quite stable in comparison to other organic peroxides. It is also quite a bit denser material as well.

Trauzl test

Joeychemist - 26-1-2005 at 21:28

Since each family of explosives has different properties and acts different it is best to perform this test with substances from the same family(peroxides -O-O-)And since there is so much question about whether or not this DPPP is or isn’t AP, I thought it best to compare the DPPP with AP and HMTD and not against PETN.


Lead block test,(LBT).
I packed 10g Of HMTD and 10g of DPPP under 2000PSI (give or take) and 1½g AP loosely on top into regular plastic film containers then the charges were fixed with a #8 equivalence cap consisting of Lead Azide and PETN. The lead blocks were placed on 1” steel plate and were at the temperature of 5C, it was cold out today. The results speak for themselves, if the DPPP were anywhere close to 9000m/s it would have destroyed the lead plate turning it into a puddle of hot lead.

lead2.JPG - 12kB

Witness plate test

Joeychemist - 26-1-2005 at 21:29

5g of AP and 5g DPPP pressed into pill containers initiated the same way as the other charges were placed on a metal witness plate 2mm thick.The witness plate was place on top of 6” of snow. The pictures are self-explanatory.

AP vs DPPP.jpg - 10kB

I can't see the picture clearly.

Matsumoto_Hideki - 26-1-2005 at 23:34

I don't see anything. can you maybe take a higher res picture.

point 2# Joey if you compressed DPPP or HMTD at 2000PSI they would both go off on you. And no just because something detonates at 9000m/s dosen't mean you will reduce your target to a molten state. I would expect more shattering than what you are describing. ie) a big hole blasted in the plate that is round. How thick is your plate? You have filtered your DPPP out with isopropylene alcohol, no? Your DPPP has got moisture in it?

Every test that I have done idicates that DPPP is the winner. ie) the 1.6g of DPPP vs TCAP test.pdf clearly indicates this.
I will do another 2 tests the 1.2cm plate vs 2 film canisters TCAP and DPPP and a lead block test.

[Edited on 27-1-2005 by Matsumoto_Hideki]

[Edited on 27-1-2005 by Matsumoto_Hideki]

Joeychemist - 26-1-2005 at 23:49

I can’t take a better pic, I tried and that’s the best I can do.

I already stated the plate was 2mm thick.

Lead is a soft metal so it does not shatter like other metals. It more so expands, and when a high explosive is DDT on a lead block it actually does turn it into a molten puddle, (much like a copper liner).The pictures speak volumes to me.You can look at the pictures whichever way you wish, either way DPPP is not even close to 9000m/s and the patent has one more hole in it.

2mm thick? I think you mean 2cm?

Matsumoto_Hideki - 26-1-2005 at 23:57

what!! you have got to be kidding and you were using a film canister? .. well , Then why would a .223 remington filled with 1.6g of DPPP almost punch a hole in a 3.5mm steel plate and 1.6g acetone peroxide barely scratch the surface of the witness plate?
can you explain that one? I think you should retry the test. BTW thin lead can shatter even though it is a soft metal, I have seen it happen before although you probably wouldn't believe me anyway.



[Edited on 27-1-2005 by Matsumoto_Hideki]

Joeychemist - 27-1-2005 at 00:12

The lead probably was ripped, strechted or torn,I doubt it would shatter, and I don't know what I believe when it's comes to you.:(

If you want Hideki, I will re-do the test any way you want.:D:D;)

It won't matter though and I will seem very repetitive I assure you. The DPPP may be a little stronger than AP but it is not stronger than HMTD nor is it 9000m/s, I don't know why you're tests say otherwise. Frankly, I could really care less about you're posts or you’re findings, as you have told one too many lies already for me to believe you.:(

Any way you want, I will conduct the re-tests exactly the way you tell me to,I will make the DPPP exactly the way you tell me to, and if you can tell me a way to make this stuff work at 9000m/s I’ll apologize for ever doubting you.
;)

[Edited on 27-1-2005 by Joeychemist]

Really?

Matsumoto_Hideki - 27-1-2005 at 00:40

Well I wouldn't pretend I was a server admin either.

Anyway, we are trying very hard to ruin this thread and make everything into "false", if something is one thing is out of place it is deemed fake or flase, if another person trys the test and gets different results "they are lying.. i do see a pattern here.
I see something totally different and Pyroz sees something different as well, physicists and chemists at my university see something quite interesting in terms of it's power and you happen to see nothing. weird.
Are you still working on that Doctorate in physics of yours? How goes your theisis?

Rosco Bodine - 27-1-2005 at 07:13

How is the thickness of the witness plate material being determined ? Is there being used a micrometer or dial caliper , or is the thickness being estimated ? How is the weight of the charge being determined ? Is an accurate scale being used , or is the weight of the charge being estimated ? There have been claims and opinions offered which relate to yields and power which are biased and which do not withstand scrutiny and which follow no conventional scientific method , and yet when these matters are pointed out , there seems to be a reaction of taking offense instead of taking a closer look to clarify the facts . Why should anyone get emotionally invested in a science experiment ? If one was testing the performance of various loading combinations for ammunition to be used in a benchrest shooting competition , then the choice would be the components which produced the smallest group on the target , not which favorite brands were already decided would be the ones declared to perform the best before any testing began . So let's just tell it like it is and let the chips fall where they may . I have at least two more experiments to do related to the chemistry aspects of alleged DPPP . And I have yet to do some of the physical properties tests like melting points . I have carefully dried and weighed and labeled the samples from various syntheses for the tests to follow . There are a couple of discrepancies which I have already identified which have not received any attention in this topic .

(1) The supposed DPPP is actually colorless , as evidenced by sublimation tests which all produce a colorless sublimate and all leave a yellowish residue whose quantity increases with the tint of the sample before sublimation .
The more pale the color of the sample , the less the amount of residue . Control samples of AP sublime completely leaving no residue .

(2) A discrepancy has been noted with regards to the stoichiometry , establishing that the amount of H2O2 specified by the patent would limit yields to well below the 90% claimed by the patent . This is a mathematical certainty ,
and though I have pointed this out , what comes back here in this thread is "no comment" . I find that very curious .

PS: The cause of the crackling sound produced by the burning of some small amounts of DPPP has been identified as not being associated with the DPPP material itself but the presence of the material responsible for the yellowish tint , which is a resinous material acting as a local binder for clumping crystals together . It is this small amount of bindering of crystals which causes the snap crackle pop sort of burning which on first examination might seem to be a burning property of the crystals themselves , when it is actually an effect being caused by the yellowish resinous impurity . Crystals of ordinary AP will behave similarly when treated with a small percentage of some binder just sufficient to cause some clumping of small crystals into granules . Binders actually lower the threshold amount for DDT so the snap crackle pop is something like a series of "mini-detonations" where the leap is not quite made to a sustained detonation of the entire mass .

[Edited on 27-1-2005 by Rosco Bodine]

My results are fact

Joeychemist - 27-1-2005 at 09:44

Quote:
Quote:
Quote:
Originally posted by Rosco Bodine
How is the thickness of the witness plate material being determined ? Is there being used a micrometer or dial caliper , or is the thickness being estimated ? How is the weight of the charge being determined ? Is an accurate scale being used , or is the weight of the charge being estimated ?

I have already said that the plate is 2mm thick, and if you must know the means of which it was calculated by, I used a dial caliper. The charge weights have already been stated, and no I am not estimating, I measured them with a Newton drop scale, the best I have.

There have been claims and opinions offered which relate to yields and power which are biased and which do not withstand scrutiny and which follow no conventional scientific method , and yet when these matters are pointed out , there seems to be a reaction of taking offense instead of taking a closer look to clarify the facts . Why should anyone get emotionally invested in a science experiment ?

Opinions are like assholes, right Rosco:D, The test pictures show the facts period, and I take no offenses to them, and if others do, that’s not my problem, there was no bias during these tests, I do not want these tests to fail so, but as you said Rosco, let the chips fall where they may.

I already knew the yellow water insoluble stuff acts as a binder and my DPPP was clean for the test. I dissolved in acetone then precipitated by dumping into ample water, filtered then washed again. It was dry and very light pale mint green, (pretty much white like AP) when fired.

I too was once sick with the “holy grail” fever but now, well, look at the pics, flat out. You have my test results, un-biased and factual. Take it or leave it for what it is.fact.;)

[Edited on 28-1-2005 by Joeychemist]

Chris The Great - 27-1-2005 at 09:47

Ok. Thanks for your answers. So, DPPP (or whatever it's 'real' name is) is a pure substance. However, it will have impurities from other chemicals formed in the HCl + acetone stage, as shown by the black smoke and yellow colours some people have gotten.

Ok, well to me the distortion looks like heat in the fact it goes awa slowly and rises. We could be discussing different things however, but I can sa with 100% certainty that the slowl rising distortion is caused by the (very) large amount of hot gas produced by the explosion.
Also, perhaps you're right about the fire, to me it looks like it burns to slowly compared to other HEs.....

Rosco, you never reall did answer m sorta-question about peroxydation of the O=C bond. I know how acetone peroxide forms, but what I was wondering is if it might be possible for 'impurites' to be formed by peroxydation of this bond in the DPPP synthesis.

WaveFront - 27-1-2005 at 10:22

Even if the VoD was really 9000 m/s, if the "reaction time", the total time to burn all the products of the reaction is slow, the brisance can be low. The brisance is more related with how fast the energy is released.

So VoD should be measured directly, by an electronic micro-second counter or by findind the point of collision of the shockwaves in detcords with one them know VoD, as somebody described.

Anyway, if the brisance is a little bit more than AP and it makes me cry every I make it, the VoD doesn´t matter to me. I will wait for the Brains of the forum to find a better thing to do with the precursor.

fatkangaroo - 27-1-2005 at 10:43

I washed my yellow powder in a metho bath then a good rinse with distilled water. The powder is now white but still not sparkerly like regular AP. There is almost no odor anymore. The powder now looks just like HMTD except there is little bit of clumping.
I am going to a series of small 1 to 2 grams of powder tests today on as many bits of scrap, wood and other junk I can find around the house and hopefully some useful information will come out. One sort of test I will do is put 1 gram of each powder in the middle of a yellow pages and see how pany pages its rips threw.

[Edited on 27-1-2005 by fatkangaroo]

Sorry for my outburst Joey but..

Matsumoto_Hideki - 27-1-2005 at 11:20

Yes Rosco the crackling sound is mesityl oxide decomposing and not the DPPP. The material I have is almost pure white and has that bug-spray odor to it. It is cubic as you say. I also notice that it is FAR more brisilliant than AP as the Test.pdf shows this VERY clearly in "actuall fact" this was the yellow DPPP totally dry that caused the damage. I notice a BIG increase in power when I filtered the mesityl oxide out of the crystals. The 3.5mm sheet steel = no match for 1.6g of DPPP in a .223 shell. So I hardly beleive that lead at 2mm wasn't even dented from Joes test.

I will do a film canister test ( DPPP vs AP vs HMTD) hopefully in the next few weeks.. I am too busy right now.

Joeychemist - 27-1-2005 at 11:44

The steel plate is 2mm thick, and the charges were 5g AP and DPPP toped with 1 ½ g AP, the lead blocks are 3/4" thick and 1 3/4" in diameter, and those charges were 10g HMTD vs 10g DPPP, again toped with 1 1/2 g AP. The lead blocks were the same size at the beginning of the test and are clearly different diameter than each other now. I will do the calculations for the LBT as soon as I can find/remember the formula to correctly calculate the expansion of the blocks.

I will attempt the sand blast tests next which is a fairly good test from calculating brisance.

Edit] Hideki read my previous post. I already stated that I also used #8 equivalence caps. Lead Azide/PETN.


[Edited on 27-1-2005 by Joeychemist]

Ok, maybe so but...

Matsumoto_Hideki - 27-1-2005 at 12:20

The steel plate is 2mm thick, and the charges were 5g AP and DPPP toped with 1 1/2 g AP, the lead blocks are 3/4" thick and 1 3/4" in diameter, and those charges were 10g HMTD vs 10g DPPP, again toped with 1 1/2 g AP. The lead blocks were the same size at the beginning of the test and are clearly different diameter than each other now. I will do the calculations for the LBT as soon as I can find/remember the formula to correctly calculate the expansion of the blocks.

I will attempt the sand blast tests next which is a fairly good test from calculating brisance.


In order to make a good initiator you are going to have to put the AP in a small compressed det cap. This makes your material (x) to detonate evenly. Those .233 shells make excellent detcaps.

Well Pyoz last test was 80g in a butane cylinder and was initiated by this method. 80g of DPPP=
4mm steel pot top was evenly blown in and 3/4" steel braket that the pot was on was warped BADLY and a deep crater 1.5 cm deep was made in the braket. Had the cylider been on the 3/4 " braket the DPPP would have blown right through it with ease even though it was a still a wide angle punching charge. "shaped"

positive complete detonation of picric acid by DPPP

Rosco Bodine - 27-1-2005 at 12:51

Let's not be too hasty about the AP versus DPPP debate , because I just got an anomalous test result involving a complete detonation of picric acid when initiated by DPPP in an unreenforced cap .
This differs from my experience with AP . However I did add an element to the firing train , which may be responsible for skewing the results a bit so I will need to repeat the test with some variations to learn the whole story . What I have gained is useful information however , since this is the *first* time I have ever secured a complete detonation of picric acid initiated by a ketonic peroxide in an unreenforced detonator test . The picric acid used for the test is pure dry pale yellow reflective crystals of the detonator grade variety , obtained by dissolving 120 grams of picric acid in about 3.5 liters of boiling water and letting the hot solution cool slowly for 16 hours in a covered container wrapped in insulation , set on a stirplate and being continuously stirred at
a low rate while slowly cooling .

1.5 grams of the picric acid crystals were added in half gram portions with each portion being compressed by hand before the next portion added , in a 5 ml polypropylene Sarstedt brand culture tube 9.5 mm I.D. 12 mm O.D. X 75 mm L.
A one foot length of 3/8" 316 stainless centerless ground round stock was used for the compression ram , and about 15 Kg of pin pressure was applied to each portion being compressed . After the 1.5 grams of picric acid was loaded in three portions , 1.75 grams of DPPP was similarly loaded in portions with each portion being compressed until the 5 ml culture tube was filled to within about 10 mm of the very top . A .25 gram spherical chunk of AP putty was placed on top . A piece of visco fuse was inserted through a hole drilled through a snap cap and secured with duct tape . The loaded test detonator was taped to the surface of a 16" length of 1" square 1/16" wall extruded aluminum structural tubing , and the tubing was marked with a pencil showing the position of the picric acid section of the detonator . The test detonator was fired and a complete detonation of the picric acid was achieved , severing the tube into two pieces . No colored residue or colored smoke was produced , and no washings of the metal fragments produced any yellow coloration to the water in which the metal shards were immersed , so the detonation of the picric acid was complete . Metal fragments from the front wall of the tube which were in contact with the detonator were impact welded to the twisted shards of the back wall of the tubing , confirming high order detonation of the picric acid in the marked section of the tube . However the section of the tube which was adjacent the organic peroxide was *not* showing evidence of the same sort of brisant high order detonation as was witnessed by the metal adjacent the picric acid . The metal adjacent the DPPP was deeply indented all the way to the inside of the back wall of the tubing , and the metal was split , but not shattered to fragments as it was in the section adjacent to the picric acid . The deepening trough from the point of ignition revealed the accelleration over a distance of ~50mm to the point where the impulse was sufficient
at the transition to the picric acid to cause its complete detonation . It may be that this result is simply general information which may be translated to detonator design for AP as well , knowing that the critical diameter is large , for example 3/8" and above , and that a relatively long column of organic peroxide primary is required , along with a rather solid starting shock , so that it can reach sufficient velocity to have initiating capability for picric acid in an unreenforced detonator . Whatever the analysis reveals from more experiments , this is an interesting development for me that an organic peroxide other than HMTD can detonate picric acid in a capsule of reasonable dimension . This could be exploited for improvised compound detonators made from rather common materials , although the detonators would still have to be nearly double the dimension of their commercial counterparts , they would also be double the output which would be an advantage provided to compensate for their bulkier dimension which would appear mostly as length . The increased length is due to the low density and slow accelleration of the organic peroxide . So a detonator can be built using this material , but it will be at least 30% larger diameter than for other materials , and about 50% greater in length to get the job done . Hmmmm. very interesting .

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