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Rosco Bodine
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Look on the bright side , good information obtained
Serendipity has its worth in experimentation . One thing I did learn from my experiments is how to get AP to initiate picric acid in an unreenforced
detonator , use a generous amount in a larger diameter than usual , and kick it good at the start with a ball of AP putty .
That's a piece of information worth knowing that I didn't know before , and haven't seen it mentioned anywhere else either .
There's so much bullshit been published both in print and on the web ,
about all sorts of energetic materials . I love it when an experiment develops a piece of *good information* tried and true , which can be added to
my own *no bullshit* files regarding such things as have been confirmed by my own experiments and then known for damn sure from direct observation and
direct personal experience . Nothing quite like a good eyewitness report for your own convincing , when the eyewitness is yourself 
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vulture
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Volunteers wanted
Painkilla made a good suggestion of summarizing this topic to get rid of all bloated speculation, but unfortunately I don't have much time on my
hands right now, so therefore I'm asking if there are a few members who'd like to condense this into a new thread.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Rosco Bodine
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Sounds like a job for 9 KM/sec No-such Pentaperoxide Man , no , ....wait a minute ... he got banned .
The printable text only word file for this thread is 256 pages long and is 1.4 MB ,
converted to pdf is not much smaller .
Please give everybody a chance to archive the complete thread before it gets edited or locked or whatever else fate is contemplated for it . There
are still a few test results like density and melting point to do , but that could be added later .
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chemoleo
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I was thinking of removing needless unrelated/flaming/arguing posts to reduce the amount of gibberish in this thread.
But a good summary, with the experiments attempted, and the respective results, might be a wise idea. For instance, right in the beginning of this
thread, Brainfever tried this very method of heating acetone/HCl, and claimed that the product seemed like AP. There is a lot of redundancy here.
But please no random speculations such as 'THIS IS mesityl oxide', 'this is mesitylene' if the only evidence is its aromatic smell
or whatever.
There are way too many chemistry -related claims in here, with little experimental confirmation other than theories...
Rosco don't worry, the essence of this thread won't be changed. That wouldn't be in anyone's interest.
[Edited on 30-1-2005 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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PainKilla
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I am gonna filter out my "DPPP" soon. I think giving it a new name would be approtiate also. I am positive no phorone is involved. The
reacion procedes seemingly with NaOH and any strong acid. I will test crystals and if this is true, then no phorone is used. Therefore, IMKP I think
it sould be called (isobutenyl methyl ketone peroxide, to alliveiate peopel thinking its methyll iso butyl ketone) While I have no direct evidence
that it is this, its obviosuly not phorone nor is there proof anywhere that phorone is ever made....
Or it can simply be TeAP, sicne it could be this too.
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Rosco Bodine
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In a very real sense this thread is a " Classic "
It may serve a useful purpose to just leave the thread as it is , because it shows the contrast between scientific method and tests designed to
develop pertinent data versus intuition and anecdotal but non-conclusive approaches ,
applied to the task of learning an unknown by experiments intended to reveal what is secret . Reading through the thread , there are portraits of
various persons struggle with methods and tools for investigation , verification or dismissal of a set of reactions descrbed by an obscure patent .
The result is an "epic" work , which is sort of
the "War and Peace" of organic peroxide threads
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PainKilla
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Yes, I agree, but I do think we should at least make some sort of new thread or maybe a document with the info. I can happily do this. Just let me
finish my experiments with H2SO4. I have a strong feeling this is TeAP or IMKP. IDK, I think we should see what all my acetone condesntation
experiments work out to be. So far we have these agents that do something:
H2SO4
HCl
NaOH (presumably KOH, BaOH etc if its not too strong)
any other acid
I think we should try using salts and see what happens.
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Rosco Bodine
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I keep reading your posts but you aren't making it clear what is the purpose of your experiments , or how the results of your experiments tend to
support or otherwise have bearing on what you are trying to prove or discover . There are "shoot in the dark" sorts of experiments , and
then there are very focused sorts of experiments which serve to reveal one very specific piece of information . It is difficult to know where you are
going with your experiments unless you are very specific what is your purpose and how the particular experiment is relevant .
[Edited on 30-1-2005 by Rosco Bodine]
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PainKilla
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I am trying to see what effect other chemicals ahve on acetone, like H2SO4 vs HCl. I am trying to see whether it is HCl that causes that
peroxidisation or no. Obviosuly, this is not the case. Now that I know no phorone is made (sicne Cl is not used, and also no solid precipate etc) I am
trying to see what will turn acetone into this yellow stuff. Obviously, H2SO4 has been used to make mesitylene/oxide so I think it could be a derative
of it. If NaOH, works then I shall try and find literate on what NaOH condesnes acetone to. This will give us insight on what to call this.
I care more about what this is than how powerful it is. Properties of the prodcut don't interest me unless its a lot less senstive than AP, which
will most likely remain my choice primary since it's so easy.
If we can figure out the precursor, then we can figure out the name molecule, OB etc. it will make much more useful things. Since any mineral acid
works seemignly, then I think I shall try bases too, just for the hell of it. Obviosuly, this has similair results too. If I can peroxidise the
NaOH'd acetone then almsot defiently no phorone is made.
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Rosco Bodine
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It is already known that acetone reacts with NaOH to produce triacetone dialcohol , particularly at cold temperatures . A patent was posted
describing this many pages back in this thread . As for the mesityl peroxide angle , why do all those speculative experiments when a good yield of
whatever is the "unknown product" has been obtained by an HCl process whose quantities have already been carefully worked out ? The present
yield of whatever unknown energetic material we have is a mixture so filled with crystals as to be impossible to stir . The reaction mixture sets up
like ice cream , a semisolid sludge of crystals . Are you investigating a new compound or simply looking at alternative methods for what is
probably the same compound , and very likely is trimeric acetone peroxide ?
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PainKilla
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Well, I got no small amount of crystals etiehr, I have maybe 2mm of liquid and the rest is a slur of crystals that IS hard to stir actually. The
yeilds with H2SO4 are jsut as good. I am just trying to see what precursor forms peroxides. The more choices we have common with many chemicals the
more liekly it will be that. If the NaOH stuff can be peroxidsed and we have soemthign in common with all of them then it will be that. I think this
is jsut TeAP, not trimeric. Or IMKP.
[Edited on 30-1-2005 by PainKilla]
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Mickhael
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Just another shot in the dark...but
Just to make mention of it, I took the several week old mixture of black fluid (supposedly phorone but now who knows what...)
100ml of that ^
100ml MEK 99%
50ml HCl 31.5%
350ml H2O2 35%
Drip added the H2O2 and have now left it stirring in a -15c freezer for getting close to 24 hours now. The results will be posted below...I hope this
isn't too useless to tell, I'm hoping to see whether it ends up as all liquid peroxide possibly = MEKPAP
\"I shall not fear, fear is the mind killer...\"
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PainKilla
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Actuallly that is intersting, I would like to see what happens with ketones in general because perhaps in the end most simple ketones form this same
black goop that cna be peroxidised.
[Edited on 31-1-2005 by PainKilla]
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Chris The Great
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Hmmm, since I have a big stack of the thread in paper form sitting on my desk that I am reading through, I'll also help sum up the thread.
I think a summary thread, seperate from this one could be made, where the results and findings of everyone can be summed up, ignoring all anectodal
evidence (well, not ignoring but presenting it as "so and so found that DPPP did such under such non-controlled situations" . It probably wouldn't be too hard to reduce the entire thread to two pages
(although Rosco insists on having such big, long descriptive scientific posts! Why must he make things hard! )
Painkilla, I'll contact you over AIM, since we are kinda doing to same type of experiments with acetone + acid (though you don't seem to
have you'r boil over and spill all over), and make sure we don't both sum up the same parts of the thread.
Now, some thoughts on me accident with sulfuric acid. I hypothesize (I do not conclude, I'm making educated guesses) that it reacted too quickly
because I had as many moles H2SO4 as there should normally be HCl, thus twice as many H+ ions. I may go slower (realative to that) with maybe a
quarter the amount, and end where it should (nice red colour). I say a quarter as HCl can keep reacting to far as well, so perhaps less could be used
with sulfuric acid, the much faster reaction time being able to make up for the less acid used. More tests, of course.
The reaction occured in anhydrous conditions, and reacted extremely fast, so perhaps the water slows down the reaction rate. Perhaps another test can
be conducted using a drying agent to pull water out of the reaction. I'll try to test this later today.
I think that regardless if this produces can explosive, it is still useful knowledge. We can learn what to be avoided in making DPPP, try to figure
out exactly WHAT is going on in the reaction, since we really don;t know for sure, and we might even stumble completely accidently onto a better way
(unlikely however).
Also, just thought I'd point out that methyl nitrate has a very low density (1.2) but still detonates over 8000m/s. I mean, it's highly
unlikely DPPP does this, but density doesn't always determine VoD. I mean, I don't think DPPP is anywhere near what it's claimed to be,
but I thought I'd mention this.
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Rosco Bodine
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| Quote: | Originally posted by Chris The Great
Hmmm, since I have a big stack of the thread in paper form sitting on my desk that I am reading through, I'll also help sum up the thread.
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The whole thread converted to pdf is a whole lot easier to navigate . I could upload the
pdf version of the thread if anybody wants it . | Quote: |
I think a summary thread, seperate from this one could be made, where the results and findings of everyone can be summed up, ignoring all anectodal
evidence (well, not ignoring but presenting it as "so and so found that DPPP did such under such non-controlled situations". It probably wouldn't be too hard to reduce the entire thread to two pages
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*TWO PAGES* ??? You gotta be kidding . | Quote: | | (although Rosco insists on having such big, long descriptive scientific posts! Why must he make things hard! ) |
Hard ? How about thorough , attentive to detail in a realm of things where details are important . There has to be a certain
formality about the descriptions of experiments for clarity , and I plead guilty to being long on details so if it takes a page to describe a process
, then there aren't needed ten more pages of questions from other people about precisely what I did and why . | Quote: |
Now, some thoughts on me accident with sulfuric acid. I hypothesize (I do not conclude, I'm making educated guesses) that it reacted too quickly
because I had as many moles H2SO4 as there should normally be HCl, thus twice as many H+ ions. I may go slower (realative to that) with maybe a
quarter the amount, and end where it should (nice red colour). I say a quarter as HCl can keep reacting to far as well, so perhaps less could be used
with sulfuric acid, the much faster reaction time being able to make up for the less acid used. More tests, of course.
The reaction occured in anhydrous conditions, and reacted extremely fast, so perhaps the water slows down the reaction rate. Perhaps another test can
be conducted using a drying agent to pull water out of the reaction. I'll try to test this later today. |
Never just dump together reactants for experiments where you are unprepared for boilovers or explosions from a reaction which is
unfamiliar . It is good practice to go little by little with additions and have a thermometer or otherwise watch for unexpected exotherms , evolution
of gases , or explosion hazard . Small quantity test reactions on a small scale are a good precaution since the magnitude of any surprise is also on
a reduced scale . | Quote: |
I think that regardless if this produces can explosive, it is still useful knowledge. We can learn what to be avoided in making DPPP, try to figure
out exactly WHAT is going on in the reaction, since we really don;t know for sure, and we might even stumble completely accidently onto a better way
(unlikely however). |
This is still an interesting thread , and an organic peroxide energetic material is
produced in good yield , whatever it may turn out to be . Acetone is converted entirely to acetone dialcohol by refluxing through a Soxhlet apparatus
whose thimble is filled with barium hydroxide . It would be an interesting experiment to see what product may result from peroxidation of acetone
dialcohol , and if that product might be trimeric acetone peroxide , obtained by rearrangement during peroxidation of the acetone dimer . Something
similar may be occuring from the precursor made from acetone and HCl , which simply acts in peroxidation as an acetone contributor , substituted for
ordinary acetone and reacting the same as if it were ordinary acetone to form the same end product .
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PainKilla
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I filtered my H2So4 stuff, It looks exactly the same as every describes. I got a good 30-40g estmating, dry. It smells like AP, but not as pleasent. I
will weigh it out ocne it dries and test it out.
Which book has the procedure for TeAP. I think it's urbanski, but I am not sure. I know it uses H2SO4. I can't recall the procedure though.
I started off using 70ml of the dark red mixture. I added 100ml of H2O2 30%. I am also peroxidsing the left overs, just in case.
More interesting results, the mixture left over from the IMKP or AP, was the light color mixture that didn't peroxidise! I think then that it is
that final thing that NaOH seems to make also, that is the thing being peroxidised. This Polymer? probably breaks up with the addition of H2O2, and
forms peroxide bonds. This is MOST likely TeAP! In fact, now that I think about it this IS TeAP. Urbanski had some properties of it and it would be
wise to compare them.
EDIT: Ah damn it wasn't tetrameric it was tri, and it was in Koehller. I do think it is some sort of polymeric peroxide. (like teap or pentaAP or
something who knows)
[Edited on 31-1-2005 by PainKilla]
GOOD GOD, I HAVE SEEN THAT PAPER. I KNOW. STOP saying like I dont know what TeAP is. I am still saying it is possible. Not as much anymore. I think
its probably a ketone polymerization peroxide.
I don't know why it cant be and why everyone is so stubborn to suggestions.
[Edited on 31-1-2005 by PainKilla]
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Rosco Bodine
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| Quote: | Originally posted by PainKilla
Which book has the procedure for TeAP. I think it's urbanski, but I am not sure. I know it uses H2SO4. I can't recall the procedure though.
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It's a journal article . Japanese IIRC . The catalyst is tin chloride , not sulfuric aicd . In fact
the presence of mineral acid prevents the formation of tetrameric AP and results only in trimeric AP being formed as the product . | Quote: |
More interesting results, the mixture left over from the IMKP or AP, was the light color mixture that didn't peroxidise! I think then that it is
that final thing that NaOH seems to make also, that is the thing being peroxidised. This Polymer? probably breaks up with the addition of H2O2, and
forms peroxide bonds. This is MOST likely TeAP! In fact, now that I think about it this IS TeAP. Urbanski had some properties of it and it would be
wise to compare them. |
No , sorry the product is not tetrameric AP , no way , no how , not even maybe . If tetrameric AP was even discovered at the time of the last Urbanski
publication , it would be news to me .
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Chris The Great
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| Quote: | | *TWO PAGES* ??? You gotta be kidding . |
Well, as a thread, not as actual paper! By comparison this thread is on it's 31st page, so 2 is a substantial improvement. Of course, the total
length will still be long but at least it will be nice and easy to navigate.
| Quote: | | Hard ? How about thorough , attentive to detail in a realm of things where details are important . There has to be a certain formality about the
descriptions of experiments for clarity , and I plead guilty to being long on details so if it takes a page to describe a process , then there
aren't needed ten more pages of questions from other people about precisely what I did and why . |
I meant that as a joke, it's great to have such detail that you provide. The more detail that is provided the happier I am. I love reading
about an experiment that has very detailed observations compared to more general ones.
| Quote: | | Never just dump together reactants for experiments where you are unprepared for boilovers or explosions from a reaction which is unfamiliar . It is
good practice to go little by little with additions and have a thermometer or otherwise watch for unexpected exotherms , evolution of gases , or
explosion hazard . Small quantity test reactions on a small scale are a good precaution since the magnitude of any surprise is also on a reduced
scale . |
Yes, that is much better laboratory practice. I'm kinda lucky that I learn all these things that hard way with fairly benign reactions.
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The_Davster
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For PainKilla's sake, I have attached the TeCAP file. There is no way "DPPP" and TeCAP are the same.
I also find Rosco's in depth write ups very beneficial. They are also better than such "writeups" by Hideki that are a few sentences,
but prompt dozens more posts acking for clarification.
[Edited on 31-1-2005 by rogue chemist]
Attachment: TetramericAcetonePeroxide.pdf (95kB)
This file has been downloaded 1571 times
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Rosco Bodine
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Here's another file of interest
There are some interesting pieces of information regarding solublility in various
solvents , ect. in the attached file .
Attachment: TATP.pdf (139kB)
This file has been downloaded 4981 times
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Chris The Great
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Well, more experimentation, this time without catastrophic failure 
Earlier today I added the 300g toilet bowl cleaner (40% NaHSO4) to 115mL Acetone, which is kinda like slush now. The colour changed in about 6 hours
to a very light yellow, signifying it is reacting slowly. The NaHSO4 picked up a lot of water however, and was very moist, so this may be slowing
down the reaction.
My mixture of 105mL 32% HCl and 115mL acetone had turned yellow in the 24 hours it had been sitting, at a temperature of approximatly 10 degrees.
My remaining sulfuric acid/acetone (115mL acetone, 55mL H2SO4) had turned a black colour with a very think black oil floating on the top after sitting
outside in occasional light rain for 24 hours. I added water to the mix and it formed a orange, opaque colour, the oil floating to the surface. The
stuff is very thick and sticks to glass very well, it took some time to clean out the jar it had been sitting in (it has a lid that fits, and so I
needed it for the next experiment). The oil formed a grey colour when being rinsed out with water, similar to the opaque orange formed from the
liquid and water. It seemed to have solid gunk in it too, this was removed with methanol and acetone.
Next, I measured out 55mL of acetone and put that into the jar, then added 14.5mL of 97% H2SO4 over a peroid of about 30 seconds using a syringe. The
acetone did not boil at all this time. I rapidly screwed on a metal cap to prevent the acetone from evaporating away from the reaction. The liquid
had turned the colour of my HCl mix at this point. The mixture heated up very rapidly, but did not boil. The colour deepened to a deep red after a
minute, and acetone was condensing and running down back into the mix very rapidly. After two minutes the colour was deep enough that it could not be
seen to be red without a strong light source.
The mixture kept 'refluxing' for about ten minutes before acetone stopped noticably condensing. The jar felt very hot to the touch. The
colour at this point was even darker than before.
After 15 minutes the mix was hot, but not hot enough to be uncomfortable, perhaps about 40 degrees on the outside. I think this is where the reaction
was done, as the temperature had fallen very rapidly in the last 5 minutes. After 30 minutes the temperature was about room temperature on the
outside. It was very dark at this point, it needed to be swirled so the mixture would run down the sides in order to see the red colour with a bright
light. No seperate layer was formed, it seems to be a single liquid, though this may change. When only traces of the liquid remains on the side
after swirling it seems to be more of an orange colour although this may be because there is just a trace of it left when it looks orange.
The smell is very strong and unpleasant, although not irritating to me. I opened the jar and smelt the vapour, there was no trace of acetone at all,
so the reaction is complete. Because the smell was very strong it was seeping out from the metal seal (it's not perfectly airtight it seems) and
it needed to be sealed with electricians tape as it is now in my room.
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Joeychemist
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Holy shit!
I got exactly the same results as you Chris when the H2SO4 was added to the acetone, a very thick viscous solution results, (thick like cold
glycerin). The temperature difference is also definitely greater than that of the HCl/acetone.When I added water to clean out the beaker received two
layers.
I added 5 drops of 35% H2O2 the H2SO4/acetone precursor while stirring and received instant boiling and ebullition which consequently produced a lot
grey and white smoke and it splashed the precursor all over the place. I then allowed the precursor to cool down while I cleaned up. I the began to
introduce the H2O2 drop wise very slowly while stirring vigorously, the temperature continued to rise at an astonishing rate even after adding only a
few drops. I was going to water the precursor down and continue but I decided to forget about it, and dumped it out.
I don’t recommend adding high% H2O2 to this solution, whatever it is as it seems kind of dangerous. Any way others are welcome to try but be warned
and take cautions.
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Chris The Great
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Hmm, perhaps the solution can be diluted by adding it to a small amount of water before adding the H2O2. According to Painkilla, he still had a large
amount of acid present after the polmerization (using 25% H2SO4) and so a large amount of the heat could be from H2SO4 sucking up water.
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Mickhael
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latest results....
20 hours of being stirred in the -15c freezer, has left a slightly milky looking yellowish liquid, with several large globes of dark red liquid
sitting on the bottom of the container. And there seems to be a very thin layer of another clearer liquid on the surface. No crystals of any kind to
be seen, unless they are extremely fine suspended within the liquid, there are also various small globes of clearish liquid hanging in the main mass
of milky yellowish liquid.
32 hours after synth (left at 18c for 12 hours) Dark red globes on the bottom of the container have now risen to the surface and for a very pale red
upper layer, seemingly mixed with a yellow clearish layer just above it, yellow milky liquid still remains as 90% of the total liquid, small bubbles
noted to be rising from the bottom, no other layers noted besides the 3: Estimated %
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| Pale, clearish layer ^ 4% |
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| Light red layer ^ 6% |
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| Yellow milky layer 90% ^ |
Small plastic dipstick was inserted into the top layer and the 2 drops roughly, that cling to it where lit with a lighter…it instantly deflagrated
in a 5 inch fireball…absorbed and contained firing tests to come soon.
Any thoughts on what I’ve made, and how I should try to separate it? I have no plans on neutralizing the batch until I know more, for fear of
destroying needed research liquid.
\"I shall not fear, fear is the mind killer...\"
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Quince
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Greetings everyone, new guy here. I've been lurking around this thread for a while, and finally decided to register.
I became interested in acetone peroxide because I can't find any OTC nitric acid, which seems to be necessary for most explosives, and I'm
only interested in small amounts anyway.
It's not clear from this thread (which I did read in full) whether the faux-DPPP really has any more power than AP.
I also want to ask about peroxide strength. The only thing I've found here (Vancouver, Canada) is 3% peroxide. Is it at all possible to use
this in the procedures that Rosco made, just increasing the volume? Or does the concentration maybe dilute the acid too much or something?
I tried making regular AP by chilling all chemicals in the freezer then mixing them in the usual AP order, and letting it sit in the fridge. Out of
40 mL total liquid (using this weak peroxide) I got 1/8 tsp translucent crystals floating at the liquid surface, and it took two days in the fridge.
I pressed that in a bit of aluminum foil, hit it with a hammer and -- nothing. Putting it over a gas flame, however, did the trick -- large flash and
the aluminum foil was in pieces.
As I was reading this thread, I got excited at the prospect of something I could also make with things easy to obtain, but more powerful. You can
imagine the disappointment. But I may still try, even if there's only a small increase in power. So, can I use the weak peroxide, or if not, I
hope someone from BC can suggest a source of a stronger one.
Thanks.
PS Does anyone know if it is possible to have the email notification be on for all my replies by default? I've seen such an option in most other
forums, but I can't seem to find it in the Control Panel here.
[EDIT] Has anyone tried reversing the order of mixing for other peroxides, such as MEKP (i.e. ketone and acid first)?
[Edited on 31-1-2005 by Quince]
\"One of the surest signs of Conrad\'s genius is that women dislike his books.\" --George Orwell
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