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BASF
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What a surprise... - The dead patient DPPP awakes! 
I still have about 7 g of commercial phorone, and don´t know what it could be useful for.
However, on the contrary to Organikums statement, i was not able to peroxidize it.
- I tried an AP-like procedure, but it failed.
One problem surely is to find a suitable solvent. If anybody could assist with some advanced organic-chemistry-knowledge, i would still be loving to
give it some additional tries on the micro-scale...
Maybe it is worth mentioning that a mixture of acetone/HCl/H2O2 (AP-proportions) behaved quite unreactive(no ppte!) with some dissolved phorone.
I doubt that a peroxide like DPPP could have a density much higher than 1.3 .
Create some peroxide-compounds in chemsketch, for example. While its density predictions seem completely off the range for high-densities(+2.0g/ccm)
it seems quite reliable for low density-C,H,O-compounds. Look for other peroxides in the literature...they all have something in common: density below
or around 1.3g/ccm. 
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vulture
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You can always determine the FeSO4 content by titrating your FeSO4 with KMnO4 first. Commercial grade KMnO4 is mostly of reasonable purity because of
it's applications (water treatment).
A slight difference shouldn't matter, because the difference between AP and DPPP should be 2 peroxide bonds per mole, which is a difference of
64g/mole.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Organikum
resurrected
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my way to go
The stuff is set for sublimation now and I will not touch it for some time.
After I decide it could be done, say all AP, TATP, etc. has sublimated away, I will wait for some days more and then do like vulture suggested and try
to determine the peroxide content of the remaining substance.
So this indicates this being DPPP, I will not explode it but do some extensive tests for the properties of DPPP, like solubility etc. to get some data
on this stuff as this is what we lack most I believe.
good idea?
BASF, perhaps you like to do some tests for properties on the phorone you have left, I believe there is almost no data available on this compound
also....
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BASF
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Last year I bought 97% phorone at Sigma-Aldrich, which seemed to be the only supplier of small quantities.
The substance could easily be melted in a warm water bath and crystallized upon cooling(room temperature) in the form of long yellow(-green) needles.
Solubility tests:
-Insoluble in 30% HCl(i also tried heating)
-soluble in commercial acetone
-excellent solubility in 98% acetic acid
-Insoluble in commercial denaturated 98% ethanol(i also tried heating; absolute ethanol needed?)
(These are for RT)
Not that i am expert in peroxidation of unknown substances...i tried the following:
phorone(1ml) in 98% acetic acid (5ml=excess to prevent seperation of phases upon addition of the aqueous peroxidation-mix) and then adding a 1:1 mix
(by volume) of 30%H2O2 and 30%HCl(total of 2ml) in a test tube.
It heated up strong (+50°C) and i repeated the whole procedure with proper cooling(ice bath), no ppte occured.
For the sake of it, i added some mL of water...no surprise, only the phorone left the solution.
The last experiment i did was to dissolve phorone in acetone and then tried to peroxidize both.
I was surprised that the phorone seemed to prevent the formation of the usual white AP-ppte.
Organikum: falls noch sinnvolle Ideen...es sind noch um die 7g da...
[Edited on 18-2-2004 by BASF]
[Edited on 18-2-2004 by BASF]
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Rosco Bodine
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| Quote: | Originally posted by Organikum
The precipitated white substance is now spread out for drying.
I will recrystallize it from IPA as soon it has dried out completely.
Question:
Is the information correct that AP sublimates away and breaks down by time as Blast X wrote?
Does light fasten the breakdown?
thanks
ORG |
Acetone Peroxide indeed does sublimate away gradually if it is exposed to free air circulation . However it behaves in this way similarly as does
naphthalene crystals , the vapor pressure of the solid is so very low that if the escaping vapors are retained as a captive blanket over the crystals
, the sublimation will almost cease . For example , if the crystals rest in a layer about 3 cm deep in the bottom of a tall container 20 cm tall ,
and the top of the container is firmly covered by a sheet of paper or closely woven cloth secured with a rubber band , the sublimation of AP will
nearly cease from the weight of the column height of trapped vapor . A similar storage strategy
can be to use a tall poly jar or bottle with the closure deliberately left slightly loose or having a piece of string draped across the sealing
surface to allow a very slight venting of vapor . AP can be stored for several years before evaporative loss of 50% occurs , by using this method of
lightly covered but not sealed storage .
When AP is stored in a completely sealed container whose dimensions are more nearly equal in diameter and much lower in height , an interesting
phenomena of sublimation and recrystallization occurs . The fine mesh crystals stored in a sealed container will gradually grow in size after a
period of months storage in a sealed container , kept outdoors and exposed to the natural temperature changes which occur daily , until all of the
crystals are on average like aquarium gravel or rock salt , with some crystals 6mm by 3 mm in size or larger . A soft poly food storage container
with a sure sealing , non threaded cover should be used for any experiment to observe this phenomena of sublimation driven recrystallization . Easily
characterized crystal samples can be obtained by this method for comparison of bona fide AP samples with
other unknown samples of similar materials , such as "suspected DPPP" .
So what was the eventual *finding* concerning your sample of suspected DPPP ? 
[Edited on 26-12-2004 by Rosco Bodine]
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Pyroz
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| Quote: | Originally posted by Organikum
My 2 cents:
Acetone + HCl doesnt polymerize so easily to phorone.
[Edited on 10-2-2004 by Organikum] |
Really? It doesn't occur easily? The temperature around Acetone + HCL has to up around 110C for at least 40-50minutes. I leave the solution for
an extra 2hrs without the heat on...the solution matures quickly.
You will see the colour change in that time from yellow to orange then to red and then it will finally go black. The reaction will continue until the
solution thickens to motor oil consistancy and become Phorone diHydrogen Chloride. Its as pure as you can get.
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Joeychemist
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It has already been proven fact that HCl will cause acetone to polymerize to phorone very easily even without heat, it just takes longer, (about two
weeks longer). This has been tried several times and proven successful every time. The reason we use the heat is to speed up the reaction. Another way
to speed up the reaction is to bubble Cl through acetone.
[Edited on 28-12-2004 by Joeychemist]
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Pyroz
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..err, I'd be REALLY careful with adding straight Chlorine to Acetone. That make just makes chloroAcetone which from my understanding can't
polymerize into a phorone -it is a base for nerve gas though--->
maybe i'm just out to lunch here--- I've never had success using this method.
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Joeychemist
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Chloroacetone is a form of tear gas IICR, and I was joking.
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Matsumoto_Hideki
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Tear gas ... nope, how about blister agent?
Chloroacetone is listed under chemicals used in WWI and a blister gas agent. It is also considered to be a carcinogen
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Tweenk
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How do you heat acetone to 110*C when it boils at 56*C? Is it a gas phase reaction?
Still wondering why the condensation of acetone happens in very acidic soln while all other aldol condensation reactions happen in basic ones...
[Edited on 30-12-2004 by Tweenk]
And now we add powdered sugar to the previously liquefied chlorine dioxide...
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Pyroz
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I'll explain:
--- when the temperature is raised up slowly over a long period of time--- acetone and HCL boiling point will raise once the reaction starts taking
place. Past 65C ---and the mixture will begin to boil. At my last step to take off any water or left over HCL, I boil the solution at 110C using a
salted water bath for 2 minutes---I reallise the the inside of the conatiner may only reach 85C or so.
Then I cool the mixture down for several hours
[Edited on 30-12-2004 by Pyroz]
[Edited on 30-12-2004 by Pyroz]
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Rosco Bodine
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Pyroz is correct . In the other thread you can read my observations about the reaction of 3 moles acetone with 2 moles HCl in a sealed bottle . A
condensation of the acetone occurs spontaneously after mixing and the reaction is exothermic enough to boil away a lot of the acetone *if* it is
permitted to escape . However , if it is in a sealed bottle it continues to react until after 45 minutes to an hour from the time of mixing , nearly
all the acetone has been converted to a higher boiling point material so there is little to no unconverted acetone remaining . Then a second reaction
takes place upon continued heating and a highly colored yellow material is produced . I have been deliberately performing this reaction slowly in an
effort to observe definite "markers" for the progress of the reaction , to identify the point in the process where is the highest yield for
the desired precursor for peroxidation to DPPP . Presently 3 distinct reaction development stages have been observed , even though the analysis of
what is occurring is just getting started .
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Polverone
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Please resize attached file
Not only is it large and unwieldy to view, it takes up almost a megabyte of board space and will consume considerable time for people on dialup to
download.
PGP Key and corresponding e-mail address
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