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Rosco Bodine
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Hmmm , white DPPP , imagine that 
Soooo exactly what method of recrystallization did you use , and I presume by "rubbing alcohol" you mean denatured ethanol ?
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Joeychemist
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What one minute!
You guys know that wax like insoluble junk that forms as the phorone dihydrochloride is being peroxidated (the upper "oily waste" layer)?
Well when it burns it produces a very thick *black* smoke ok. The “smelly” “yellow” DPPP produces a small amount of black smoke when burned
but the re-crystallized DPPP does *not* smell as bad, it is *white* and now that you mention it pyoz it *DOES NOT* produce the small amount of black
smoke. Any one else get what I’m saying here???
[Edited on 10-1-2005 by Joeychemist]
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Pyroz
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DPPP after filtration using pure rubbing alcohol or ISOPROPLYENE ALCOHOL Color is ever so slightly green---much whiter than before and smells similar
to AP ---but smell isn't as intense. It violently explodes in a compressed clump in open air but will catch fire uncompressed.
[Edited on 10-1-2005 by Pyroz]
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Rosco Bodine
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It still seems possible to me that adding
some chloroform or methylene chloride or trichlorethylene to the mixture before the peroxidation may result in precipitation of the DPPP in pure form
. Such solvents should be inert to the peroxidation mixture but somewhat soluble in it , and would therefore tend to act sort of like an emulsifier
and solubility increaser for the suspended or dissolved materials , to make the reaction more complete while slowing crystallization . And because
they are highly volatile , they would easily disappear from evaporation after they have served their
purpose . If the DPPP could be precipitated pure from the reaction and require no subsequent purification it would be desirable for saving the work
and expense of solvents for recrystallization . And what I am thinking is it shouldn't require much of the solvent
added to the reaction mixture to do the
job if the strategy works , maybe 10% or
less of the volume of the acetone and HCl mixture should be sufficient .
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The_Davster
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It may be unnecessary to use other solvents during the peroxidation. As I mentioned before letting my filtrate sit at room temperature for 24h
yielded a pure white precipitate with no other solvents needed. Perhaps if after peroxidation, the reaction mix is allowed to sit for 24h at room
temperature the same result could be observed.
Those of you who have recrystalized your DPPP, was the smell after just a milder version of how it smelled before or was it a new smell?
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Rosco Bodine
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You are probably right about just letting the mixture stand . But I have some chloroform on hand , and I feel it is only fair that I should
chloroform some DPPP just to get back at it for what it has aleady done to me
That's right ...
take that you little molecular m'f#!*kers .
It really could make a difference also to simply slow down the addition of the H2O2 to a crawl , which would by itself
slow the growth of crystals and perhaps result in a crystal having less occluded impurities . So I'll probably check out that
strategy first , maybe let it stand afterwards for a good while too .
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Joeychemist
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Before=shit smell After=good
Rogue Chemist
I can’t describe the smell, It smells absolutely awful before I re-crystallized it, but after, O dear god, after I re-crystallized the DPPP it was
almost pleasant to smell the stuff. It has a weak sweet smell, somewhat like chlorobutanol, yeah, I guess I can see where you’re coming from with
that, but it more so smells like really “funky” AP to me.
So flat out, before I re-crystallized it smelled fowl but after it smelled like
peaches compared to before.
Maybe even using less concentrated H2O2 will allow the crystals to form at the ideal pace, of course one would have to adjust the amounts used and it
might totally fuck the reaction up. But I doubt it, besides I really want to know what type of a yield is possible with say 3 and 6% H2O2 anyways, so
I’ll try that tomorrow perhaps.
[Edited on 10-1-2005 by Joeychemist]
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Matsumoto_Hideki
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I also filtered my remaining 300g and also discovered...
I would not say the filtered end product it completely white but very very very light yellow, almost the colour of the post reply box..
Coloured material I am drying and sending to university tommorrow, get some sort of answer on...
Indeed it looks as though I was wrong about dppp's colour after all... hmmmm.
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chemoleo
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May I just ask what you plan to have done with it at the university? You are dealing with an explosive substance, and if anything, just anything
happens to it in the form of an explosion/little fireball, while being handled from lab assistants etc, you will undoubtedly be in big trouble.
I myself considered giving it to our NMR people, but the risk it entails is too large - at least for me.
Anyway, if you are giving a sample to the NMR people, make sure it is dissolved, i.e. in a saturated solution of methanol. Not many people do
solid-state NMR, and aside this it is safer. You won't have deuterated methanol, so you will have to live with massive peaks from the methanol.
Else... try to chase down an electrospray massspec. It won't take long to run a sample, and also you won't have to disclose its identity -
i.e. you could say it's a dye you made or something. Calibrate from 0-1000 Dalton.
But NMR would be best of course.
[Edited on 10-1-2005 by chemoleo]
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Rosco Bodine
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rogue chemist is probably correct , irritant is unreacted precursor
The crystals of DPPP which I have been drying for several days are continuing to
gradually lighten in color and lose the irritating vapor which was an unmistakable presence on the freshly made DPPP . The level of the irritant has
steadily decreased around the crystals exposed to the air , and it is now barely detectable after three days of
"airing out" . When the crystals were freshly made , the irritant vapor was quite overpowering even several feet away from the crystals
resting on the filter and spread out for drying . And now after several days the vapor has nearly vanished completely ,
so it is evident the impurity is volatile , and whatever is the impurity , it is not the DPPP , but is a nuisance impurity which by some means is accompanying the DPPP crystals from synthesis , like fleas on a
dog . So there is probably some change which can be made in the way the synthesis is being done , to minimize or exclude the impurity . Rogue
chemist may be correct in that simply letting the mixture stand will allow the reaction to finish more completely and eliminate the impurity which
consists of unreacted precursor . That looks like a very good theory at this point .
In the early part of the discussion at E&W Forum I suggested that reversing the order of addition may have advantages and this still seems like it
may be logical as a possible way of addressing this specific problem . If the precursor was added very slowly to the cold peroxide , and * IF * the
reaction would proceed the same path in spite of this reversal of the order of addition , then the precursor would be exposed to H2O2 in great excess
of its requirement during the early part of the reaction . Normally this
would tend to drive the reaction more assertively in the direction of complete conversion of the precursor , resulting in a more pure product . And
because it appears that the presence of any unreacted precursor accompanying the end product is an
offending impurity due to its lachrymatory properties , then this provides incentive for formulating a strategy for reducing or eliminating that
unreacted precursor from the end product . I am tempted to try the reverse order of addition simply to see if this will
clean up the reaction . I know I asked about this earlier and was told that reversing the order of addition produces AP instead of DPPP , but frankly
I doubt the accuracy of that report . What I suppose and hope could be true is that a white product resulted which was mistakenly identified as AP ,
when it may have actually been pure white DPPP .
That would be very nice if that turned out to be true and clarification on this is no matter of any trivial significance .
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chinamen_6
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Allright after all these 20 pages, has someone really have a good synthesis with a high yield, no lying which everyone could follow?
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Joeychemist
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No!
No we don't, if you would have bothered to read the last 20 pages you would know that we are still tweaking and playing around with things trying
to figure all that out. All I can tell you I the basic procedure is out lined many times in this thread. If you're not even going to bother
reading this whole thread (I don't blame you) at least read a couple pages back.
Hey guys I'll confirm that my crystals are much whiter after letting the reaction continue at room temperature over night. I'm not sure how
bad they are going smell after filtering and drying, but they have gone almost to the color of AP in less than 12hours, it would appear that the
reaction actually does need extra time to finish.
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Rosco Bodine
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How about a reverse order of addition peroxidation ?
I am going to check it out , just for shits and giggles to see what happens .
Will get back later on the results .
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Axt
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Why not try distill the acetone/HCl mixture, and try peroxidation on both the distillate and the mother liquid. I speculate that you will find that
the black condensation product doesn't create a peroxy precipitate, but the distillate will form a precip (which I call AP  ).
Yeh, im still a full blown skeptic! But whatever the case, distillation would provide interesting results.
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Rosco Bodine
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AXT :
Distilling is definitely an idea , but the heat of an atmospheric distillation is likely going to decompose the the phorone dihydrochloride , so
vacuum and low temp
would be a good idea , and even that may
not work or be conclusive , since it is possible that the phorone dihydrochloride
is an unstable transitional compound that
will decompose if boiled at any temperature , existing only in solution .
I do believe that it does exist however ,
and the dyestuff like quality which lends a yellow tint to dilute solutions as surely as does picric acid , lets you know there is more there than
just a simple solution of acetone and HCl . The byproduct which is so irritating is also something not associated with AP , and the dried material
thought to be DPPP looks nothing like AP , and smells nothing like AP . The thermodynamic of the peroxidation isn't the same as for AP either .
So why do you suppose what we have made is just some "tinted" AP ?
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Axt
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| Quote: | Originally posted by Rosco Bodine
So why do you suppose what we have made is just some "tinted" AP ?
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Because everyone is assuming large yeild of condensation product, whose to say that there is still not significant quantities of acetone still in the
mix, which I believe their would be. A quick evaporation session won't release it all! not when dissolved in that quantity of liquid.
The decription of the peroxidation of DPPP closely resemble what would happen if one was to add 1 part peroxide into cold 1 part HCl and 1 part
acetone (the DPPP ratio's), Temperature jumps sharply and a precip of AP forms instantly as a fine powder.
The colour/smell/look of it can be explained by interference from the condensation product.
Anyway, thats why im a skeptic, I'll wait for your performance reports before believing any power claims. Which I really think should be
confirmed first.
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Joeychemist
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Not AP, not 9000m/s
Axt, You may be right, but then again…I would like it if you checked this stuff out under a microscope at about 100X, I would not be surprised if
you changed you’re tune.
I don’t think 7000m/s let alone 9000m/s is possible with this peroxide, but it is not AP.
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Axt
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| Quote: | Originally posted by Joeychemist
I would not be surprised if you changed you’re tune. |
The large mix of condensation solutes in the liquid could explain the interference with crystal growth, thats my point, it can all be explained more
logically then looking at the complex reactions proposed for DPPP.
Im not saying im right, people have looked into this far harder then I have, but distilling it to see if AP can be reclaimed from the "DPPP"
mix would answer a lot of questions. Getting a confirmation on "power" would dismiss my theory.
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chemoleo
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And who's the man well-known for calibrating the power of various energetic materials? *hint*hint* 
PS Axt- one thing that seemingly doesnt add up with the AP theory is its stability and friction sensitivity - so far noone reported friction
sensitivity. But I don't know if anyone tested it.
Also, if someone did a comparative test on its volatility, that would be great. AP should lose a significant amount of weight during a few days, while
the putative DPPP wouldnt. Should be a simple matter.
[Edited on 10-1-2005 by chemoleo]
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Joeychemist
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| Quote: | | Originally posted by AxtIm not saying im right, people have looked into this far harder then I have, but distilling it to see if AP can be
reclaimed from the "DPPP" mix would answer a lot of questions. Getting a confirmation on "power" would dismiss my theory.
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Ahh..., but this is why you have been called in Axt, I do believe that Rosco asked for a crazy Aussie.
We want you to test the power among other things, not only do you have the proper tools but you are trusted and very experienced, plus you provide
visual proof(movies)_(I love you’re movies). I think that you’re tests and findings will prove the most useful in determining the question of
whether or not this is the “holy grail” organic peroxide or not, ( I think not, I think MEKP rules over DPPP but I have yet to test this).
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Matsumoto_Hideki
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No tests? What
I guess you people never bothered to download the test.pdf that has picts of DPPP and AP both at 1.93g being detonated. ie) the witness plate tests,
I guess people have just ignored them? DPPP is very slightly friction sensitive, but will ignite/detonate upon hard impact of a strong hammer blow,
unlike AP which is highly friction sensitive.
BTW I am now having some organic chemists looking into the molecule and synthesis at my university officially, and they are really interested!!!
There should be some answers in a matter of weeks about if this DiPhorone Pentaperoxide is as energetic as the pattent claims!!
Already I have talked with a physics prof and showed him my pics of the witness plate damage, he was really surprised by just how much brissiliance
this material (DPPP) had especially the damage had come from an organic peroxide.
[Edited on 10-1-2005 by Matsumoto_Hideki]
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Rosco Bodine
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Sublimation / Condensation test anyone ?
Suppose we put a small amount of "suspected" DPPP in the bottom of a test tube
( maybe a poly tube ) and then put the bottom of that test tube in some near boiling or boiling hot water .
AP would melt , sublime from the heated portion of the tube and then condense as
rectangular white crystals on the cooler portion of the tube ......right ?
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The_Davster
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Well I returned today to check the odor of both the white DPPP and the standard pale yellow variety. The pale yellow DPPP has lost even more smell,
my nose must be inches away to detect any smell. The odor detected at this range is like "funky AP" as origionally described by Joey. The
smell of the white DPPP which I origionally reported to be surprisingly close to that of chlorobutanol has now subsided to again "funky AP"
but this smell is stronger than that of the pale yellow DPPP. But this is to be expected because of the different times of filtering(1day apart).
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Joeychemist
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Sublimation should work
Rosco, yes, in theory that sounds pretty good. Are you going to be trying it now perhaps????
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Rosco Bodine
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| Quote: | Originally posted by Joeychemist
Rosco, yes, in theory that sounds pretty good. Are you going to be trying it now perhaps???? |
Yeah I'll give it a go if I can find my bag
of 15 ml clear polypropylene culture tubes , give me awhile and I'll dig through
my stored junk to find what I need . I have glass test tubes handy , but I hate heating primaries in glass for tests . So I'll go find the
poly tubes . I know I have a full box , just can't remember where in the hell they are , something I rarely use .
But I got 'em somewhere .
UPDATE : Well there's some good news and some bad news . I'm getting a slight
dusting of glitter on the cool part of the tube as there was a * partial * melting of the quarter gram sample , along with some water vapor . But
the "dusting" of glitter appears to be less than 1% of the sample which first melted and then solidified again after "off gassing"
the little bit it did . I am going to get it a bit warmer for a longer time and see if anything else comes off the sample .
UPDATE : Subsequent heating for a longer period produced no melting and only a bit more moisture and a little more of the same dusting of glitter of
sublimed crystals as the first time . A comparison sample of authentic AP is undergoing the identical test right now .
UPDATE: Well that test told me a big fat nothing because the AP behaved exactly the same way , slight condensation of moisture and a dusting of
glitter of sublimed crystals . I expected the AP to make the larger crystals which sometimes
will grow from its vapor , but no such luck .
Partial melting in boiling water , looks like it would melt completely on a second heating . But I have sealed up both tubes
and put them in a warm water bath for overnight to see what may sublime and crystallize slowly over time . One thing I did note was the difference in
bulk density for the loose crystals , the suspected DPPP is twice as heavy per volume as is the loose crystals of AP ,
that is for the pouring volume without tapping the crystals down at all .
[Edited on 11-1-2005 by Rosco Bodine]
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