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WaveFront
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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.
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Dodoman
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Just finished my exams the other day and I finally have some time to do experiments and I did  . 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]
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Joeychemist
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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.
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Dodoman
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| 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.
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Joeychemist
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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?)
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Dodoman
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| 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]
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Rosco Bodine
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Some thoughts and some preliminary tests
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]
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Matsumoto_Hideki
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Instead of relying on reports
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]
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chemoleo
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Neutralisation of the black stuff
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!
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Rosco Bodine
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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
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Matsumoto_Hideki
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LIGHTEN UP ROSCO!
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]
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Rosco Bodine
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I melted 100 mg DPPP , pffftttt , no detonation
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 ?
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Rosco Bodine
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| 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 .
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FrankRizzo
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Blaster's Spoon
http://www.sciencemadness.org/talk/viewthread.php?action=att...
On review, this one may have been faked by shooting with a gun.
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Pyroz
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::
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!
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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]
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Rosco Bodine
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DPPP minimum DDT diameter 5.5 mm
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
.
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Matsumoto_Hideki
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Your DPPP is NOT dry ! DANGER !!!
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)
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Rosco Bodine
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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 ?
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chemoleo
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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.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Pyroz
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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.
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PainKilla
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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.
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Pyroz
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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]
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Matsumoto_Hideki
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Never mind... You guys are not reading the posts
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!!! 
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Mickhael
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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]
\"I shall not fear, fear is the mind killer...\"
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Pyroz
Hazard to Self
Posts: 76
Registered: 27-12-2004
Member Is Offline
Mood: curious...
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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]
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