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K9
September 1st, 2004, 09:55 AM
When I'm using a low concentration of peroxide, as long as large portions of H2SO4 aren't dumped in, there is no immense temperature rise. With higher concentrations you have to go a bit slower. But then again, HCl always has that it's cheaper than H2SO4.

On a separate note, isn't HCl technically a stronger acid than H2SO4?

ProdigyChild
September 1st, 2004, 06:07 PM
@Arthis: I assume, this thread is meant as for collecting data about AP. I've just read the current AP beginners guide again and have a few remarks:

1) AP does sink in water, even DOES sink in density 1.1g/cm3 solutions. The only reason why not all of it doesn't sink are air bubbles sticking to the tiny crystals. So in reality you have part of it sink, part of it floating and part of it is still undecisive where to go. Throbbing the contrainer makes some floating crystals sink, while some sunken ones which cought a bubble out of the water moves up.

2) hydreated (H2-added) Naphta (Pentane, Heptane; 'Coleman Camping fuel') is an excellent solvent for AP, similar to Acetone. This might be useful to know as Naphta does not dissolve in water. Like with Acetone, the solubility increases with temperature.

The dimeric / trimeric warnings are not very clear to me. Honestly, I don't believe what is said. I tried to produce dimeric AP intentionally by using temperatures above the recommended ones. I cannot distinguish the product from the one I made by observed the rules. Not by density, not by crystal shape, not by explosive power.
I've never got any AP that was as unstable as dimeric should be.

I have theory about that: My production always yields the trimeric!
I use much less acid (2ml HCl 33% per 30ml 30% H2O2)
I use Mega's ratio of H2O2 and Acetone (30ml : 50ml)
I wait one week for the completion of the reaction
I react it in the cooler (about 6° ) most times
I do not evaporate the Acetone before filtering
I do not wash
I never use H2SO4 (not volatile -> washing needed)

What I believe is: I do get dimeric, too, but not much. The remainder of Acetone in the finished reaction still dissolves all of the dimeric.
When drying, I soak the moisture with toilet paper. Hence only traces of dimeric can coat the trimeric cristals.
Drying in the air evaporates some of the AP and it's obvious that most likely the outer cover of dimeric falls victim to this evaporation.
That's why I get trimeric only :p

If I washed, I could precipate larger crystals of dimeric and perhaps linear peroxides, too. Because of lowering the solubility of the solution.

If I used H2SO4? I don't know! But I've already prepared a batch of AP made with sulphuric to investigate.

What do you think about that?

Complete nonsense?

Is there anybody else trying to find out more about AP?

Chris The Great
October 13th, 2004, 04:56 AM
Ok, I read the manual, I really like it as it's really simple, down to the point and accurate.

However, it mentions that AP in acetone is only a fire hazard. This is not true. The acetone burns away, and the AP crystalizes, and will then explode. If your jar of acetone conatining AP ignites accidently or purposefully, it will explode after burning for a bit. This was discovered by dissolving 0.5g of AP in about 1mL acetone, and igniting on a spoon. The AP made a fireball like it was wet, except it also sprayed a bit of flaming acetone/AP around (which is why I only used a mL of the stuff). This really should be mentioned, as it means that it is not safe if it burns, it is still an explosion hazard. I'm pretty sure it's the same with all flammable solvents, although I haven't tested it.

I've also never had any problems with heat, I mixed 125mL H2O2, 100mL acetone, and poured in 25mL HCl (30%) without any cooling during or before. I stirred it up, and it never went above 40C. AP resulting from this was ~90 to 95 grams after 48 hours of sitting at room temp.

Do NOT use nail polish remover for your acetone, it sucks. Do NOT use lower concentrations of H2O2, unless you HAVE to. Boil down your H2O2, even with decomposition, you'll get more AP out of it. 3% makes almost no AP, even if I let it sit for a week. It really pays to get acetone from the hardware store as well as 35% H2O2, it's not worth it with 3% (I haven't tried with 6% but I suspect it also has really bad yeilds). I boiled my H2O2 in a tin can, it worked fine and I got about 40% conc. (theorectical 60%) after a couple hours of boiling. It works fine at a full boil. But, it's easier and much cheaper just to buy 35% H2O2 from your local garden store in the 1L or 4L containers.

Perhaps letting AP sit out for a while after formation will remove the traces of dimeric from the batch, or at least lower it?

Does anyone else have trouble setting off AP by hitting it with a hammer in small amounts? I cannot make it go off, even when hitting it hard enough to put huge dents in my sheet metal.

Yes, AP definatly needs more study. Most researchers seem to avoid it, I haven't found any "professional" information on it, compared to other explosives such as TNT, NG and RDX for example. I plan on doing some good research sometime, but I don't know when as whenever I plan on a date, it never works out since I have bad luck with planning.

NotTheMahdi
October 24th, 2004, 08:46 PM
Well i don't think that 15% h2o2 is so bad after all, i didn't bother to check at hydro because here is not common to see hydro shop (never seen one), and also because the hair whitener is damn cheap, around 1€ for liter...

You Dutchmen have no excuses for not being able to find a hydroponics store, you do know how your marijuana is grown don't you?

PS: I had a strange dream about making my first 'serious' explosive last week. I managed to get a decent yeild from 45ml 12% Hydrogen Peroxide Creme, 30ml Acetone and 10ml HCL. I didn't weigh it but the results spoke for themselves, I love you all

Desmikes
October 27th, 2004, 03:57 AM
Recently I learned that AP will NOT form without any catalyst. I always thought that the formation is spontaneous b/c after 3 days, water treatment 35% H2O2 + hardware store acetone mixture will produce tons of large AP crystals. ("spontaneous" is used as an everyday term, not a chemistry term, don't bother correcting)
Few weeks ago I tried AP synthesis with the highest purity 35%H2O2 and Acetone, much higher than what is available to the public. After a week at room temperature, the mixture was as clear as it was originally. Not even a hint of AP formation.
To rule out a mistake in the set up, I added standard amount of HCl and transferred to -20*C where AP had no problem forming.
(that's after It froze solid in matter of minutes in -70*C freezer)

Chris The Great
November 7th, 2004, 04:56 AM
I did a little experiment about testing the explosive properties of wet AP, to see exactly how powerful/nonpowerful it was for information/curiousity purposes. Gloves in the picture are shown for scale. You can also see the filter I used in the background, as well as the nail used to press the stuff into the tube.

About 35mL freshly filtered AP was pressed into a cardboard tube with walls about 1/4 inch thick from wrapped paper, sealed at one end with water putty. An AP pen detonator was pressed into this, and then the whole thing was put in a plastic bag as the ground was fairly damp at this point in time from it raining all day.

http://img114.exs.cx/img114/1708/wetcharge.jpg

This was buried about 8 inches underground, as I'm in a residential area and I don't like making loud explosions in the open. I set it off, and it made a muffled thump and lifted the loose grass I dug up off the dirt, and moved the dirt around a bit. No big blasting dirt into the air, bits of dirt went maybe a couple feet into the air at the most. Half the plastic bag and detonator wires were thrown a foot from the hole. Not very impressive.

The remains where dug up, and pieces of the pen had mostly gone through the paper and into the dirt (I only found one piece, and it was stuck halfway through the paper). The paper was in big chunks, and the water putty plug at the end had not shattered or even been damaged. The plastic bag was melted at the edges and ends.

http://img114.exs.cx/img114/2928/wetcharge2.jpg

You can see that there is still alot of undetonated AP on the cardboard, probably only the center of the charge actually burned (I highly doubt it detonated since the explosive power was so minimal).

And now we know how weak our wet AP really is. I'll do a control with 35mL dry AP in the same setup later this week for comparison.

Randyman
December 4th, 2004, 02:53 PM
I am looking for the AP for Beginners Guide. Could someone point me in the right direction. I've searched on here but there only seams to be bits and pieces.
Thank you in adavance.
Randyman

~Phelixx~
December 4th, 2004, 03:13 PM
Arthis has a link in his singature, called AP beginners guide... Isn't this what you are looking for?

Randyman
December 4th, 2004, 03:39 PM
The link has been removed due to someone using someone else's work from what I understand. So now I'm in search of the original work.

K9
December 4th, 2004, 08:27 PM
I'll host it for a bit so you can download it.
http://aa.1asphost.com/houseofK9/An%20AP%20beginner's%20manual.pdf

Randyman
December 4th, 2004, 11:50 PM
For some reason nothing is showing up where you have it posted. The page refreshes and comes up blank. Could you email it to me please.
Randyman

The_Rsert
December 5th, 2004, 09:04 AM
High concentrated (over 85%) H2O2 will form really large AP cristalls without an catalyst, because the 85%+ H2O2 is acescent.

TIP: You can use zink chlroride instead of HCL; than you will get an better yield I think.

Anthony
December 5th, 2004, 05:48 PM
Is it wise to mix HTP with highly flammable organic solvents?

Randyman
December 5th, 2004, 09:28 PM
Ok folks I'll try once more. Does anyone have a guide to making AP?
Most of the links I had to information are no longer working.
Thank you in advance.
Randyman

K9
December 5th, 2004, 09:38 PM
Make it a link and right click, save as.

Randyman
December 5th, 2004, 10:57 PM
Sorry, Still won't work.
I won't bother you any more.
Randyman

Anthony
December 6th, 2004, 01:54 PM
The link works fine for me.

Copy the link above and paste it into the address box of your browser. Your browser's download manager will open and ask you to save/run the file.

vurr
December 6th, 2004, 05:43 PM
mix equal amount (moles) of acetone and H2O2, and add few %vol. acid.
ratio is 1:1 by volume,if H2O2 is 50% (I messed with such one),
liquid will get warm/hot.
I made one larger batch for Y2K and remains were sucsessfully used at 2004,after being in HN4NO3 slurry for years.

opinion :dimere forming - lower reagent concentrations needed, to close the cycle before third acetone-peroxide part connects...

The_Rsert
December 10th, 2004, 04:58 PM
I made one larger batch for Y2K and remains were sucsessfully used at 2004,after being in HN4NO3 slurry for years.

Really? That's cool! I have heard, that a little batch of unwashed AP explodet by itself after two months. Have you recrystallised the AP? Was it dimeric or trimeric AP? How was it stored exactly?

SimplisticNick
December 12th, 2004, 11:54 PM
Tonight, I began synthesizing my very first batch of Acetone Peroxide; here's the details:
I used 900 mL of 3% H2O2 mixed with 75 mL of 100% (CH3)2CO.
I mixed both chemicals together in a glass container which was suspended in a below-freezing temperature tub of ice water/salt.
When they were mixed, the liquid turned to a white/cloudy colour (I'm hoping this is normal, for I don't remember reading about this white cloud before the acid catalyst was added).
I let the termperature go back down to about, -1c before i added 40 mL of 36.6% H2SO4, slowly but surely.
The temperature barely rised (I'm assuming because of the large amount of excess water in the H202).

I've searched, read, and prepared. Now I wait.
Any suggestions on a better way I could synthesize Acetone Peroxide next time?

Edit: Also, I've found a cleaner called OxiMagic made by Clorox. The product does contain hydrogen peroxide as the main bleaching agent, but does not give a quantity or percentage. Would anyone happen to know the percentages of this product? Searching google.com and the oximagic website gives no help.

ProdigyChild
December 19th, 2004, 01:02 PM
SimplisticNick,

wouldn't it be wise to start with smaller amounts, for the first synthesis???
You could end up with 30-40g AP (estimated) - do you know how to handle?

Yes, it's normal that after mixing the solution turns cloudy.

Silentnite
December 20th, 2004, 05:50 AM
I just made my first batch of AP. Unfortunately it was with DrainCleaner that was VERY dark. But its been said to work so I'll post tomorrow as to what happens. I inadvertantly made a little too much, but practice will make perfect(if i'm using cliche's should I include how curiosity blew up the cat??). I used the formula from the FTP "A beginner's guide to AP" and it seemed to work well.

SweNMFan
December 20th, 2004, 01:34 PM
Any suggestions on a better way I could synthesize Acetone Peroxide next time?

You can use HCl instead of H2SO4, then the AP made have a tendency to have the trimer structure, H2SO4 (atleast when using a hi conc) have a tendency to make dimer structured AP.

You can also try boiling your H202 to make it more concentrated..

If I have to do a peroxide I rather do HMTD.. as I think of it as slightly more stable..

K9
December 20th, 2004, 02:43 PM
When I've used 3-6% peroxide I find that there is hardly any temp rise even with conc. H2SO4. But you are much better off using a higher concentration of H2O2. Even so, that seems like a lot of H2O2 to be using as compared to the amount of acetone.

But if you going to use a higher concentration of H2O2 then I'd suggest using HCl. When I dropped H2SO4 (concentrated mind you) into the 35% H2O2 and acetone, there is a puff of vapour and isntant formation of AP. Even with the HCl the temperature rise is noticeable but not as bad.

I personally also like HMTD more than AP. I think it's more powerful than AP, but you just have to make sure to keep it away from metals.

draco aster
December 21st, 2004, 06:25 AM
Im new here (please correct me if I have done anything wrong) and I have a question : "When making AP, can it be cooled in a fridge or does it have to done in an ice bath".

Thank you.

SweNMFan
December 21st, 2004, 01:23 PM
"When making AP, can it be cooled in a fridge or does it have to done in an ice bath".

The colder the better .. and when starting out ONLY make small batches.. A few grams of AP can remove your hand.. 200g can turn you in to minced meat

K9
December 21st, 2004, 04:24 PM
If you think you're going to have trouble keeping the temperature down without an icebath, then use one. I personally just use a freezer though.

Cyclonite
December 21st, 2004, 11:02 PM
Before the acid is added chill the acetone and H2O2 in the freezer then just add acid and put in the fridge

Silentnite
December 22nd, 2004, 02:53 AM
It didn't ignite, but I got the process down pretty good so I know a little better what to expect. Also I'm going to try to cleanse the H2SO4 from the contaminents. And a fuse burnt out in the ignition system...

knowledgehungry
December 22nd, 2004, 08:27 AM
The colder the better .. and when starting out ONLY make small batches.. A few grams of AP can remove your hand.. 200g can turn you in to minced meat

I'm sorry to be redundant but I am going to say it again, you should NEVER make large batches of any organic peroxide, unless you are a suicide bomber and your planning on walking into Israel the next day. It is never worth the risk. Organic peroxides will stab you in the back even after years of working with them. I've seen too many people get too comfortable with AP only to lose their fingers. AP will act differently with every batch. Always treat each batch as if it is your first.

Boomer
December 22nd, 2004, 09:45 AM
True, true.

BTW how many fingers got lost that you personally know of? I know of four people her + on APC who lost fingers, one of them a hand an eye. I guess there are many more, plus that Swedish kid... :(

About the big batches: Have you EVER heard of a batch exploding BEFORE drying? I don't think that is possible with AP, and for HMTD the worst is the boiling-away and the stench. I am speaking about normal conditions here, not a cap+booster in the slurry! :p

I asked because I prefer to make 200g AP, but keep it dripping wet, i.e. after washing it is directly put under water. Drying is done gram-wise before use. One gram every few days gives me less shivers than drying 10g every few weeks, and having dry surplus around for ANY time span. Plus, if spread out you got a much better chance it won't DDT in case it DOES ignite than with the 10g!

I am actually more comfortable with this method as I also get over the "I wonder how sensitive it is this time...?" question arising every two weeks. You just have to watch if it gradually changes, though I did extensive testing and found no difference in sensitivity from bigger crystals after a year. If they DO get TOO big, crushing four 250mg portions up with a wooden dowel is not that bad - I use goggles + earplugs, but never had a single explosion. I would rather expect one while (remotely) pressing detonators.

aikon
December 22nd, 2004, 11:16 AM
...I asked because I prefer to make 200g AP, but keep it dripping wet, i.e. after washing it is directly put under water...

It has been discussed to death in other threads, but why are some guys so keen on making huge patches of AP?
PETN, RDX, ANFO or ANNM are explosives good for bigger quantities. To my mind there's no practical use for 200g of AP. AP has also bad storage properties, so storing is an invalid argument.

Cyclonite
December 22nd, 2004, 04:05 PM
I make a good amount of AP, its stored in multiple small quantitys though. I just keep it in a dark place in between two newspapers. Since I use AP for my caps its easier to have some already dried in a SAFE place.

The_Rsert
December 22nd, 2004, 04:23 PM
At low H2O2 concentrations, using HCL as catalyst will make a better yield. But if you use higher concentrated hydrogen peroxide (for example 30%) H2SO4 is better as catalyst.
Wash the AP everytime. Whatever you will use as catalyst.
Dry the AP completly. First in sun an than at room temperature until it's 100% dry. If you have little ammounts of AP, you can dry it in an desiccator.
Don't dry it in an oven, on a radiator or under a lamp.
Cover the AP everytime with a light drapery to avert that dust will set on the AP. The AP will be decomposed faster if there's dust in/on it.
It's good to recrystallise the AP after the procedure an after a long storing period.
Dissolve the AP in hand-warm acetone, filter the solution and precipitate the AP out of the solution with destilled water.
Than dry it covered by a cloth to protect the AP for dust.

Cyclonite
December 22nd, 2004, 04:41 PM
Yes AP will dry faster in the sun but beware AP can explode with very very very little provoking when exposed to sunlight. The longer the exposure the more you should worry. If your impatient for your AP to dry (Like me) heres what I do. I filter the AP in about 6 wraps of cheesecloth then I wring it out. Then I wash in water with a little baking soda. Wring it out then wash in rubbing alcohol, smear on some newspaper and setup a fan to expedite drying. I find it best to change the newspaper after 20mins or so then move the pile around every so often. Also its safer to use HCL, by the time its dry any HCL left over should be near gone. H2SO4 will sit untill you get rid of it.

Joeychemist
December 22nd, 2004, 04:44 PM
At low H2O2 concentrations, using HCL as catalyst will make a better yield. But if you use higher concentrated hydrogen peroxide (for example 30%) H2SO4 is better as catalyst.

(Stupid fucker couldn't even use a drop-menu properly! :rolleyes: NBK)

What do you mean by this? I would think that when using higher concentrations of H2O2 (since there is less water) with H2SO4 would cause hot spots to form, and since TCAP is mainly produced at lower temperatures this would result with DCAP forming almost instantly. So you might get a better yield but it will be mostly the dimmer form. If you use H2SO4 make sure you’re using low concentrated acid.

"It's good to recrystallise the AP after the procedure an after a long storing period.
Dissolve the AP in hand-warm acetone, filter the solution and precipitate the AP out of the solution with destilled water.
Than dry it covered by a cloth to protect the AP for dust"

I totally agree with you on that, If you store you AP dry it does not matter where or how its dried, It will evaporate and decompose leaving some crystals (mostly the top layer) Thinner and weaker and thus more unstable than the day it was made. I recommend storing in water or re-crystallizing any AP stored (if you re-crystallize the AP be sure you don’t dry into one solid cake, that’s asking for trouble).

knowledgehungry
December 22nd, 2004, 04:45 PM
BTW how many fingers got lost that you personally know of?

I know someone personally who has lost 3 fingers, fortunately they were on his non-dominant hand. While it is highly unlikely that wet AP will "go off" I dont like to make batches that will kill me if by some stroke of luck it does go off.

Also any tests that you make with AP concerning sensitivity may change for your next batch. So don't use the it could withstand this much heat once to justify putting it anywhere near that heat etc.

vurr
December 24th, 2004, 08:09 PM
Really? That's cool! I have heard, that a little batch of unwashed AP explodet by itself after two months. Have you recrystallised the AP? Was it dimeric or trimeric AP? How was it stored exactly?

it was not recrysted,only washed with dish washing liquid(few millilitres per litre) and enough amount of NaHCO3 (until no more bubbles +little extra); then "coffe-filtered",and air-dryed; + 6 to 8 parts NH4NO3 with traces of org. solvent...
di or trimer = ???. but melting point of product is little below water boiling point.
was stored in not-zip-polyethylene-bag(become wet).

nbk2000
December 24th, 2004, 09:34 PM
Vurr:

You used a detergent with your carbonate wash? Assuming it was completely removed in the rinse (distilled water), I don't see any harm in it. It might even improve efficiency.

zambozan
December 25th, 2004, 06:32 PM
Hallo,

I have bought some 3% hydrogen peroxide and, I've read that it
contain aqua, hydrogen peroxide and methylparaben.
Would this last interfer in the AP reaction?

excuse me for bad english

Merry Christmas to everyone!

The_Rsert
December 25th, 2004, 06:54 PM
di or trimer = ???.

If you will use HCL as catalysator you will get a tendence of dimeric AP; If you will use H2SO4, you will get get a tendence of trimeric AP

Which catalysator have you used?

grendel23
December 26th, 2004, 05:06 AM
The_Rsert,
On what do you base that statement?
We know that temperature affects ratio of dimeric to trimeric AP, with lower temperatures favoring trimeric.
I have read speculation that because H<sub>2</sub>SO<sub>4</sub> produces more heat than HCL when added, it may tilt the ratio toward the dimeric. I am not sure if this is true, since the heating would be of a very short duration, and I have no reason to believe the temperature in the first minute is more important than the next twelve hours. I am not aware of anyone doing a controlled study to check this effect.
PATR2700 mentions both dimeric and trimeric made with H<sub>2</sub>SO<sub>4</sub>, but the first is done at 50<sup>o</sup>C and the second at <10<sup>o</sup>C.
If you have a source which states that H<sub>2</sub>SO<sub>4</sub> produces more trimeric than HCL at a given temperature, I would love to see it.

The_Rsert
December 26th, 2004, 04:23 PM
I've read it, somewhere. ;)
Maybe it was in the German e-book "der_kleine_Sprengmeister" or in this forum or in the Sciencemadness Forum.
...

SweNMFan
December 26th, 2004, 05:08 PM
If you have a source which states that H2SO4 produces more trimeric than HCL at a given temperature, I would love to see it.

They both produce the same structure at the same temp, HCl just doesn't make it heat up as much as H2SO4.

Mr.ANFO
December 27th, 2004, 01:06 AM
No I don't think so, I have pure Trimeric AP every time I use 30-42% HCL.
H2SO4 (aq) as far as I know creates more heat. ??? I may be wrong? ?? In fact I don't really think it matters what you use as long as you controll the temp well.

FUTI
December 27th, 2004, 01:08 PM
I think SweNMFan is trying to explain that the property of H2SO4 to generate more heat makes that reaction little diferent since you must take into account local "over heating" of reaction mixture so that termometer is measuring average of bulk mixture but in reality reaction takes palce mostly on the surface of drop of acid solution and acetone/hydrogen-peroxide.

I also have question: can posible formation of peroxysulfuric acid take part in possible different (if there is any) action of these two catalyst?

draco aster
December 28th, 2004, 11:23 PM
My first batch of AP did not work :(

This is how it was made:

First 10ml of 99.9% Acetone was added to 2.5ml of 30% HCl and put in a fridge at 2 degrees celcius.
Once cool it was removed and 50ml of 6% H2O2 was slowly added.
The solution formed an orange colour and was put back in the fridge and left overnight......got nothing :confused: .


DID I DO ANYTHING WHONG :confused:

kingspaz
December 31st, 2004, 03:37 PM
Add the acetone to the peroxide and refrigerate, then add the pre-chilled acid slowly keeping the reaction temperature below 10*C.

Rosco Bodine
December 31st, 2004, 05:37 PM
When using weaker peroxides like that 6% , your yields will be poor
compared to using stronger peroxide . And your catalyst of choice
will be sulfuric acid for use with the weaker peroxides , as it will
give the best yield . Get all the ingredients cold before mixing
and add the acid last . Acid causes acetone to polymerize so never
mix the acetone and acid separately for making AP . Cool everything
separately before mixing , add the acetone to the peroxide and
then with stirring add the acid to the acetone and peroxide mixture .
The weaker the peroxide , and the lesser the amount of acid , the
more time required for reaction . Using 6% peroxide you are talking
about a week for the reaction mixture kept in the freezer to fully
complete .

draco aster
December 31st, 2004, 11:11 PM
thank you,

Where I live all 30% H2O2 has been put on back order at chemist and chemical supply houses. Even hair salons have been forced to order new types of bleach!
The Reason.....STUPID people who have NO idea what they are doing are making AP :mad:

That is why I only have 6% peroxide (Used to use it as an disinfectant). Its getting harder and harder to obtain chemicals.

K'Luuppo
January 1st, 2005, 02:21 PM
How does the polymeration of acetone show? I've never had any problems even though I always first mix acetone and acid and finally the peroxide. The point of that order is easier temperature control: the peroxide is the largest part of mixture, so it's easier to prevent it from heating.

Rosco Bodine
January 1st, 2005, 02:41 PM
Polymerization of acetone is indicated by an exotherm and color development .
If everything is very cold , then you won't see the polymerization beginning
because it starts slowly at low temperatures . But the effect is there , whether
its rate is observable or not . You won't even notice the insignificant effect if
everything is cold and mixed together without delay , but slow down the work
or work at higher temperatures and you will have polymerization of the acetone .
Yellow is th color you will see first , and the color will deepen as the polymerization
proceeds .

vurr
January 3rd, 2005, 05:20 PM
If you will use HCL as catalysator you will get a tendence of dimeric AP; If you will use H2SO4, you will get get a tendence of trimeric AP

Which catalysator have you used?

H2SO4,labelled:car battery acid; less than 10 millilitres per 500 ml {act+hydperox}

any analytical methods for determing dimer-trimer presence/ratio??

FUTI
January 4th, 2005, 04:57 PM
Color most likely originates from conjugated ketone made in dehydration reaction.

But that is not the thing I wanted to post....just want to say EUREKA. I find a article about H2SO4, H2O2 and acetone and it did prove my guessses about diferent mechanism. It seems that H2SO4 makes more trimeric AP. I will e_mail it tommorow to admin to make it part of knowledge database made here.

EDIT: I read the thread that linked with DPPP. I gained impresion that people here want to work with substance as pure as it can be made under current condition so my comment was linked with that. And e_mail is sent to webmaster of the Forum with files I find relevant to this thread.

SweNMFan
January 4th, 2005, 06:48 PM
Polymeration of acetone isn't necessary a bad thing. Read the Holy grail organic peroxide (DPPP) thread as it seems more stable, but possibly more dangerous due to increased power.

Mr.ANFO
January 4th, 2005, 09:37 PM
Is DPPP possibly more dangerous? Well how does 9Km/sec sound compired to 3.5-4Km/sec for TCAP? Also just to let you know DPPP has roughly 6x the power than AP does.
DPPP is also storable for long periods of time at room temperature when kept dry... just as any old
HE.. Only draw back with DPPP is that is tends to have a low ignition temperature 180-200c. It is only moderately shock sensitive sort of like PETN and doesn't seem to react with metals at all unlike HMTD or AP...etc.

knowledgehungry
January 4th, 2005, 10:02 PM
Mr. ANFO you have been stating rather firmly that DPPP has a velocity of 9KM/sec while this has not been proven. Please stick to things that one knows for a fact as in the scientific world exaggerating or reporting what one thinks as a fact is frowned upon. Just say that DPPP has appeared to be much more powerful than AP in tests. We do not know the velocity for a fact.

Boomer
January 5th, 2005, 01:18 PM
I never bothered with DPPP as I thought it was a myth. If it is real, why is there no mentioning (outside pyro websites) since that old patent?

Now with all that talk starting again, people claiming its great power etc. plus the fact that someone on APC claims to have found a reliable synt, I might give it a try. If only to proove it is just coloured AP boosted by fantasy. :p

If the synth really works, I will of course measure VoD to contradict that silly 9000m/s claim! 4% accuracy will be enough to either say oh-my-god or shout bullshit.

knowledgehungry
January 5th, 2005, 01:28 PM
How do you plan on measuring it Boomer? I really want someone to test it with something other than the "it makes a bigger hole than AP so it must be more brisant". From the tests I have seen it looks like it is much more pwerful than AP, however I would like something more conclusive.

Chris The Great
January 5th, 2005, 01:39 PM
I'm assuming the det velocity can easily be measured by modifying a chronograph (I think that's what it's called) to have a different sensor. I've also read that it's measured used a moderatly high voltage sensor, as when the detonation passes it becomes much more conductive.

I'm very interesting in making something to measure VoD myself, what do you have?

Anthony
January 5th, 2005, 01:48 PM
Boomer has made an electronic timer to measure VoD of explosives in a column. Some details are in the "Making your own detcord" thread:

http://roguesci.org/theforum/showthread.php?t=3833

I will be interested to see the result :)

Mr.ANFO
January 7th, 2005, 11:19 PM
Hey boomer did you bother downloading the DPPP .pdf file? This shows you a compairison between energy of TCAP vs DPPP.

Oh and one more thing, the patent is proving to be correct on many levels , after the damage I have seen done from DPPP I would not hesitate to say it is detonating at 9km/sec.

zambozan
February 20th, 2005, 01:39 PM
Hallo to all,

I've found that hydrogen peroxide in conc. lower than 20% will
lower the yield of AP very much.
Also, the use of additives like methylparaben in commercial
H2O2 would have a influence in the AP reaction?

THe_rEaL_dEaL
March 3rd, 2005, 01:09 AM
In my friends experience, :) , the best ratio of reactants and catylsts is, 6-1-2 by volume, Acetone (Anhydrous), Peroxide 60%, HCL 32% as volume/volume.

The acid ratios can be tweaked 'batch" by "batch" , may need more or less.

Different chems with diff % active could be tweaked accordingly.

MEK Peroxide is another, similar, good fun peroxy-ketone.

Myrol
April 18th, 2005, 11:08 AM
Umm, yes I know. The times are bad for me, but because I was SO OFTEN questioned after TATP, I wanna know something more about that stuff!

Ok, the Explosive properties bla bla are well known to me......I'm just searching for some physical properties wich I really not found via googling or searching in the Web.

The most important values are (wich I dont know):

Energy of Formation, Enthalpie of Formation, Heat of Explosion, Heat of Detonation, specific Energy in mt, Heat of Fusion, Pressure of Sublimation, a small table with some VoD's at different Densities and the diameter from the steel sleeve test.

Density should be 1,2g/cc for the pure trimeric version, right? If not you can correct me of course ;) Ohh, and the Flashpoint is 165°C. I've read often 130°C, but the encyclopedia Wikipedia should be somewhat more reliable than some stupid "cook Book's".

Thanks for any Data. Myrol

Myrol
April 18th, 2005, 11:08 AM
Umm, yes I know. The times are bad for me, but because I was SO OFTEN questioned after TATP, I wanna know something more about that stuff!

Ok, the Explosive properties bla bla are well known to me......I'm just searching for some physical properties wich I really not found via googling or searching in the Web.

The most important values are (wich I dont know):

Energy of Formation, Enthalpie of Formation, Heat of Explosion, Heat of Detonation, specific Energy in mt, Heat of Fusion, Pressure of Sublimation, a small table with some VoD's at different Densities and the diameter from the steel sleeve test.

Density should be 1,2g/cc for the pure trimeric version, right? If not you can correct me of course ;) Ohh, and the Flashpoint is 165°C. I've read often 130°C, but the encyclopedia Wikipedia should be somewhat more reliable than some stupid "cook Book's".

Thanks for any Data. Myrol

Myrol
April 18th, 2005, 11:08 AM
Umm, yes I know. The times are bad for me, but because I was SO OFTEN questioned after TATP, I wanna know something more about that stuff!

Ok, the Explosive properties bla bla are well known to me......I'm just searching for some physical properties wich I really not found via googling or searching in the Web.

The most important values are (wich I dont know):

Energy of Formation, Enthalpie of Formation, Heat of Explosion, Heat of Detonation, specific Energy in mt, Heat of Fusion, Pressure of Sublimation, a small table with some VoD's at different Densities and the diameter from the steel sleeve test.

Density should be 1,2g/cc for the pure trimeric version, right? If not you can correct me of course ;) Ohh, and the Flashpoint is 165°C. I've read often 130°C, but the encyclopedia Wikipedia should be somewhat more reliable than some stupid "cook Book's".

Thanks for any Data. Myrol

Jacks Complete
April 18th, 2005, 12:01 PM
Myrol, I wouldn't read any more explosives stuff till you beat the current rap!

If you show you know all about TATP you might wind up in deeper doodoo!

Jacks Complete
April 18th, 2005, 12:01 PM
Myrol, I wouldn't read any more explosives stuff till you beat the current rap!

If you show you know all about TATP you might wind up in deeper doodoo!

Jacks Complete
April 18th, 2005, 12:01 PM
Myrol, I wouldn't read any more explosives stuff till you beat the current rap!

If you show you know all about TATP you might wind up in deeper doodoo!

Boomer
April 19th, 2005, 06:23 AM
He might make them feel bad by saying THEY made him interested in TATP with their questions... which they will hardly buy.

One thing I can tell you: Steel sleeve test gives max. diameter, meaning it will fail even without an orifice plate. This should have been obvious: 50-100g TATP in a steel pipe with one end plug, heated with 3 burners - did you expect it to just burn ? :D

Boomer
April 19th, 2005, 06:23 AM
He might make them feel bad by saying THEY made him interested in TATP with their questions... which they will hardly buy.

One thing I can tell you: Steel sleeve test gives max. diameter, meaning it will fail even without an orifice plate. This should have been obvious: 50-100g TATP in a steel pipe with one end plug, heated with 3 burners - did you expect it to just burn ? :D

Boomer
April 19th, 2005, 06:23 AM
He might make them feel bad by saying THEY made him interested in TATP with their questions... which they will hardly buy.

One thing I can tell you: Steel sleeve test gives max. diameter, meaning it will fail even without an orifice plate. This should have been obvious: 50-100g TATP in a steel pipe with one end plug, heated with 3 burners - did you expect it to just burn ? :D

tomu
April 19th, 2005, 10:18 AM
Source PATR 2700:

VoD 5290 m/s as detonated in a column of dia. 6.3 mm at d 1.2,
VoD 3065 m/s in 15 mm column at d 0.68, VoD 3750 m/s at d 0.92 and 5300 m/s at d 1.18

Impact Sensitivity:

Bureau of Mines Apparatus: 500 g weight, 10 cm
French Apparatus "petit mouton" 50 g weight 15 cm for 50% detonations


Source Explosives, Köhler-Meyer:

Shocksensitivity: 0.03 kpm = 0.3 Nm
Frictionsensitivity: 0.01 kp = 0,1 N


You may find more facts in Beilstein 1, 645 & 714

tomu
April 19th, 2005, 10:18 AM
Source PATR 2700:

VoD 5290 m/s as detonated in a column of dia. 6.3 mm at d 1.2,
VoD 3065 m/s in 15 mm column at d 0.68, VoD 3750 m/s at d 0.92 and 5300 m/s at d 1.18

Impact Sensitivity:

Bureau of Mines Apparatus: 500 g weight, 10 cm
French Apparatus "petit mouton" 50 g weight 15 cm for 50% detonations


Source Explosives, Köhler-Meyer:

Shocksensitivity: 0.03 kpm = 0.3 Nm
Frictionsensitivity: 0.01 kp = 0,1 N


You may find more facts in Beilstein 1, 645 & 714

tomu
April 19th, 2005, 10:18 AM
Source PATR 2700:

VoD 5290 m/s as detonated in a column of dia. 6.3 mm at d 1.2,
VoD 3065 m/s in 15 mm column at d 0.68, VoD 3750 m/s at d 0.92 and 5300 m/s at d 1.18

Impact Sensitivity:

Bureau of Mines Apparatus: 500 g weight, 10 cm
French Apparatus "petit mouton" 50 g weight 15 cm for 50% detonations


Source Explosives, Köhler-Meyer:

Shocksensitivity: 0.03 kpm = 0.3 Nm
Frictionsensitivity: 0.01 kp = 0,1 N


You may find more facts in Beilstein 1, 645 & 714

draco aster
July 22nd, 2005, 04:51 AM
Hey....I have tried and tried again but still cannot stop the polymerisation of the acetone.

I first mix the acetone and peroxide, cool, and the add the 30% HCL the problem is that as soon as a singular drop hits the solution it turns orange. What could be causing this?

draco aster
July 22nd, 2005, 04:51 AM
Hey....I have tried and tried again but still cannot stop the polymerisation of the acetone.

I first mix the acetone and peroxide, cool, and the add the 30% HCL the problem is that as soon as a singular drop hits the solution it turns orange. What could be causing this?

FUTI
July 28th, 2005, 10:10 AM
Is it stupid to try other way around? Pour cooled mixture of acetone and hydrogen into cooled acid solution. That maybe can reduce polymerisation of acetone due to dilution but then so does it slows down making of AP. I just hopes that since making the AP is slower process by what it appears since product separates slow and afetr some onset time. I never tried that. Any hints from more experienced member?

FUTI
July 28th, 2005, 10:10 AM
Is it stupid to try other way around? Pour cooled mixture of acetone and hydrogen into cooled acid solution. That maybe can reduce polymerisation of acetone due to dilution but then so does it slows down making of AP. I just hopes that since making the AP is slower process by what it appears since product separates slow and afetr some onset time. I never tried that. Any hints from more experienced member?

Nope
July 28th, 2005, 02:51 PM
I recently made, AP maybe, by using a product that I bought from a paint store, containing acetone and white spirit, I think... The yield was shitty but there was very big crystals formed. When I finished the acid addition on the ice bath, I put it in the freezer for one day. The other day I left it outside the freezer for ~5 hrs. Then I filtered it. Also, It burned much more violently than ordinary AP :p

The yield was shitty because I left it in the freezer or because the product wasn't pure acetone? Any way. I'm gonna try it again. It was fun :p

Nope
July 28th, 2005, 02:51 PM
I recently made, AP maybe, by using a product that I bought from a paint store, containing acetone and white spirit, I think... The yield was shitty but there was very big crystals formed. When I finished the acid addition on the ice bath, I put it in the freezer for one day. The other day I left it outside the freezer for ~5 hrs. Then I filtered it. Also, It burned much more violently than ordinary AP :p

The yield was shitty because I left it in the freezer or because the product wasn't pure acetone? Any way. I'm gonna try it again. It was fun :p

Chris The Great
July 31st, 2005, 03:24 AM
Adding the H2O2/acetone to the acid is something I wouldn't recommend. You'll probably get a very rapid reaction due to the huge excess of acid you will have in the beginning. Hence you will have to add it very slow, with heavy cooling, and the acid should be heavily diluted. I would think that adding it to concentrated acid would cause a very rapid temperature raise, or something else unwanted.

This orange colour is very strange, I'm thinking that there is something else in the H2O2, since the other chemicals you are using seem to be pure. However, when used as a disinfectant I would think that it would be pure... It's a very unusualy problem and unfortunately I don't know what could be causing it. Perhaps the company is adding some other disinfectants to it or something... Try and find an MSDS through google for it to see if they put anything else in there besides the peroxide.

FUTI
August 4th, 2005, 09:01 AM
Did anyone tried to add activated carbon to solution mixed to make AP and then filter it to remove coloured compounds? Carbon also will decompose little H2O2, but if it is done in resonable short time it may help - unless it react with AP which can lead to serious troubles:(.

FUTI
August 26th, 2005, 06:57 AM
Chris they put some phosphoric acid(or derivative of) and phenacetine AFAIK to hydrogen-peroxyde for stabilisation. Color could be coming from some kind of aldol type reaction, but aditive can make it worse.

Greggonzalias
June 17th, 2006, 09:50 AM
[QUOTE=Mr.ANFO]
Also just to let you know DPPP has roughly 6x the power than AP does.
QUOTE]

Dosn't power have to do with the amount of gases released and
pressure than velocity on detonation?

That is say 10 grams of two explosives:
A low VoD explosive which has more gases say CO2, NO2 and H2O
than an explosive with a high VoD that has lesser gases - CO2
I understand that some thing at 8km/s would gain a high pressure
faster than some thing at 2.7km/s

I guess there are some variables.
Please don't scald me if I'm wrong. :o I DID A SEARCH
If I am wrong can someone please correct me. :D

bcc1985s12
June 22nd, 2006, 03:30 AM
I used the recipe to make AN as posted at totse.com, but the yield was horrible! I doubled the recipe, and after 36 hours at the proper temperature, made less than a gram.
I was using 3% h2o2. Does this low concentration affect the reaction more than simply having to increase the amount of h2o2?

I used 1000ml of 3% hydrogen peroxide,
Put the beaker in an ice bath until it cooled to about 4 degrees Celsius.
I then poured 120ml of acetone into the peroxide, and stirred until thoroughly mixed.
I measured out 30ml of h2So4 and added it to the mix. I then placed the beaker into a refrigerator, and kept it there for 36 hours.

After filtering and rinsing the precipitate, I had a pure white powder that exploded loudly when detonated with a hammer. It seems to be a high quality product, but I got less than a gram.

Something has to be wrong. Should I try it with a higher concentration of h202?

Alexires
June 23rd, 2006, 12:09 PM
Ok, here is what you should do.

1. Kick yourself in the head repeatedly if you ever visit totse again. That site is crap.

2. Use 30% H2O2. I've heard that the yeilds for 3% are crap. If you can't buy 30% H2O2, read the thread on concentrating it.
3. Go to Mega's chem lab and read the synth there. Here (http://www.roguesci.org/megalomania/explo/acetoneperoxide.html) if you can't find it.
4. Read your posts through TWICE before you actually submit. Stops little errors like AN instead of AP...:rolleyes:

I've used 10mL HCl (70% I think) instead of sulfuric and it worked find. Shitloads of AP precipitated.

Remember, keep everything as cold as possible. Using a salt/ice bath, you should be able to get -5*C easy.

....Totse sucks.....alot.....impossible to say how much....keep going there if you wish to loose limbs....and inifinitely worse, possibly your membership here.

bcc1985s12
June 24th, 2006, 01:59 AM
Thanks, sorry about the typo. I will post my results with the new synth.

grendel23
June 24th, 2006, 02:29 AM
There is no such thing as 70% hydrochloric acid, only so much HCl will dissolve in water. Muriatic acid at about 31% is common.

I have seen foaming drain cleaners, and a foaming laundry stain remover which are two part products, one of which contains H2O2. Has anyone tried to make AP or HMTD with one of these?

I looked online for an MSDS for "Spray 'n Wash Dual Power" stain remover and "Liquid Plumber" foaming drain cleaner, but didn't find one for either product, so I don't know the strength of the peroxide.

H2O2 from this source, fingernail polish remover (acetone) and a bit of toilet bowl cleaner (HCl) would be as OTC as you could get.

inventorgp
June 24th, 2006, 04:50 AM
You should of got about 86.5g

well if you used...

996mL of 3% hydrogen peroxide
86mL of Acetone
and
10.5mL of 35% Hydrochloric acid

Stoichiometry does help:D

bcc1985s12
June 24th, 2006, 02:44 PM
So should I boil my h202 down to concentrate it? It says that you should on wikipedia, but also says that you risk explosion. I think that the excess water in the h202 was the problem, as I seemed to have done everything else correctly. (except for adding too much acetone.)
h202 + C3H6O---->C6H12O4 (dimer)C9H18O6 (trimer)
I guess I will use stoichiometry before blindly following any more recipies.

Chopper
June 24th, 2006, 09:38 PM
Yup, just do it slowly - i.e simmer it.

Have a bit more of a search around here re: boiling and explosions. It needs to be fairly concentrated > 70% IIRC or have dust fall into it to become dangerous.

This has been discussed fairly extensively. As have sources of H2O2 that are stronger than 3%. Mentioned also are easy ways of seperating Dimer and Trimer.

Good luck, and for god's sake man - keep your fingers attached.

c.Tech
June 24th, 2006, 10:45 PM
as I seemed to have done everything else correctly. (except for adding too much acetone.)

BINGO!!!
There’s your problem. As acetone peroxide is soluble in acetone (and very slightly soluble in water) it was probably in a solution.

Next time if you add too much you could use heat to drive off the acetone, although this would be risky.

inventorgp
June 25th, 2006, 08:15 AM
I've actually tested acetone to its autoignition point.

It's pretty cool 463..464...foomp, 4650C.

Lots of vapour before autoingnition:p

Alexires
June 25th, 2006, 12:14 PM
From experience I know that boiling H2O2 down at 75*C takes fucking ages. Do it in pyrex, not metal.

I've read somewhere that H2O2 starts to decompose at 80*C so I attempted to keep it below that, but on the same token (I think it was the thread on concentrating H2O2) it said that boiling it down as hot as you can didn't effect it at all (100*C ish).

Have a look in the OTC threads for a source of H2O2, or search a few hydroponics stores.

Excuse the bit about 70% HCl. I haven't had to check up on the concentration in a while.

Just a little question about AP. If its neutralised, what kind of forces are we talking about to set it off? It seems pretty stable compared to my expectations (think NI3).

Just curious, because I'm going start some experiments soon, which I think at least some of you will find interesting. No more till I have something chewy to post ;) .

- Edit: My god, while searching for AP sensitivity, I uncovered this. (http://www.totse.com/en/bad_ideas/ka_fucking_boom/162660.html)
I went there thinking it would be good for a laugh, but lo and behold, it isn't totally crap. He actually stresses safety and gives some figures based upon possible research. Goes to show that not every single person on totse is an idiot.

Ok, everyone besides him is an idiot.

bcc1985s12
June 25th, 2006, 06:30 PM
c. Tech:
Thank you! I knew that acetone dissolved AP, but for some reason didn't connect the dots. I can't believe I wasted almost 85 potential grams of AP by throwing it out!(safely)

Chris The Great
June 26th, 2006, 06:29 AM
AP isn't soluble at all in water/acetone mixtures, so none was in solution.

If you want to test this, dissolve AP in acetone, then add some water, and all the AP comes out as very fine crystals.

inventorgp
June 26th, 2006, 09:08 AM
Chris the Great,

I get fine crystals all the time when I make TCAP.
My method is to mix the acetone and peroxide(50%) then, slowly,
i.e. one drop ever three second of 35% hydrochloric acid whilst
rigorously stirring. I find this does not past 30OC.

The liquids precipitate within minutes. Then I put the TCAP in to
a coffee filter in a funnel, give it a bicarbonate wash, the a acetone
wash.

Then I open the coffee filter and put on top of a paper towel and let
dry.

To get ten grams of TCAP I use:

10mL of C3H6O
7mL of 50% H2O2
2mL of 35% HCl

I find this also to be pretty stable.

Kleng
June 26th, 2006, 04:05 PM
inventorg:

I'm also using exactly the same way as yours. When using 50% H2O2, the crystals seems more stable, the liquid precipitate quicker and you get a better yield.

I really recommend using 50% H2O2. In addition it is very easy for me to get. I got a 25litres can in the garage...

bcc1985s12
June 26th, 2006, 04:45 PM
- Edit: My god, while searching for AP sensitivity, I uncovered this. (http://www.totse.com/en/bad_ideas/ka_fucking_boom/162660.html)
I went there thinking it would be good for a laugh, but lo and behold, it isn't totally crap. He actually stresses safety and gives some figures based upon possible research. Goes to show that not every single person on totse is an idiot.

Ok, everyone besides him is an idiot.

That post has innacurate info, because I followed it down to the letter, doubling the recipe, and came up with less than a gram of AP. It has way too much acetone.

Alexires
June 27th, 2006, 11:51 AM
That post has innacurate info, because I followed it down to the letter, doubling the recipe, and came up with less than a gram of AP. It has way too much acetone.

*rolls eyes* Which part of my post did I say to follow it because its absolutely perfect in every way? Note the use of the phrase " not totally crap" as in "I wouldn't follow it, but it doesn't look like your usual blow-your-fingers-off recipe from totse".

If I remember, I said follow Mega's synth, not totse's. Just because I said it wasn't totally crap doesn't mean that I would actually try it.

K9
June 27th, 2006, 09:12 PM
You could always work out the numbers for the reaction and test for yourself to see what works for you. This may help in providing you with a synthesis that works best for your particular chemicals, procedure etc.

Alexires
June 28th, 2006, 11:14 AM
You COULD work out the numbers yourself I suppose, but have you ever looked at the equation for AP? Screw working that out yourself. As well as it being a bitch for balancing, there is also taking into account the formation of the mono/di/trimeric forms of AP as well as reaction involving the catalyst.

Unless you have a degree, have done at least first year or a very healthy interest in chemistry it is unlikely that you would be able to work that out yourself.

If you felt the need to work it out yourself, congratulations to you. But personally, I would be checking it against a good source (Mega) before I made it.

If I felt the need to optimise the procedure, I would do it by trial and error. Make a batch Mega's way, then another batch with a little more acetone, then another batch with a little more peroxide, then another with stronger acid etc....

Mega's has always worked for me, often giving me more AP than I knew what to do with, and I'm rather happy with it.

inventorgp
June 28th, 2006, 11:35 AM
Just practice your Stoichiometry.

K9
June 28th, 2006, 04:39 PM
If you want to look at it that way then it is near impossible to work out many reactions due to all possible side reactions. The point is that you can work out what you should need based on what you want. It is actually not all that hard for AP. Of course there are side reactions etc. that can happen that may be unwanted, but you can still work something out that will give you good results. The reaction based on making the cyclotrimer is not all that complicated to work out.

Checking against someone else's numbers is great of course, but sometimes you may be using slightly different reagents and the case can change.

You can work out what should be proper amounts stoichiometrically and then test to see how it works for you.

Alexires
June 29th, 2006, 10:10 AM
Checking against someone else's numbers is great of course, but sometimes you may be using slightly different reagents and the case can change.

You can work out what should be proper amounts stoichiometrically and then test to see how it works for you.

I would assume that there is only really one correct synthesis eg X amount of Acetone, with X amount of Hydrogen Peroxide with this many hydronium ions at this temperature will yield X amount of AP after X amount of time. (If that made sense)

Regardless of your reagents, whether its 3 or 30% H2O2, HCl or H2SO4, as long as the essential values are correct, your yeild will be as good as its going to get.

Thats how I see it anyway, I have never really been told otherwise (unless its an equilibrium reaction).

Still, arguing this is rather pointless. I don't mind if I right or wrong, but the general consensus so far seems to be -

A stronger acid is better (more likely of a trimer product, or so I've read)

More Acetone is better than not enough (easy enough to evaporate off or precipitate by adding water)

Keep below 10*C during the addition of the acid, and while the AP is precipitating (Personally I keep it at -5*C ish)

Higher concentration (30-50%) Hydrogen Peroxide is preferable to low concentration (3-6%) as the reaction takes a hell of a lot longer at low concentration, and the yield isn't as good as the high one.

Neutralization is must. Personally, I'd work out how much base would be needed to neutralize all the acid that you added, dissolve the AP in Acetone and neutralize, precipitate, wash with distilled water, check pH, dissolve and precipitate from Acetone (neutralizing if necessary) then washing with 0*C distilled water twice more after a pH of 7 has been reached.

You may loose product, but its better than loosing fingers.


Correct me if I am wrong, that is just what has occured to me so far as useful for an AP beginner.

ozz
June 29th, 2006, 10:44 PM
Sorry to bother, but I have not been able to find an answer to this question...

Can Chlorine bleach be used in place of other non-organic acids (sulphuric, citric, hydrochloric) seeing as it is acidic?

++++++++++++

No.

NBK

Cyclonite
June 30th, 2006, 12:58 AM
You could boil H202 in a vacuum at a low temperature if needed, you can order 30% on the internet. I would use HCL opposed to H2SO4, the reaction is cooler and any leftover HCL will lower in strength when the AP is dried. If you’re looking at larger yields then I would add a little sodium bi-carbonate to the AP after neutralization.

I use cheesecloth to strain the AP and dip it in a bi-carbonate solution. Anything that falls through can be filtered through a coffee filter.

c.Tech
July 1st, 2006, 07:12 AM
AP isn't soluble at all in water/acetone mixtures, so none was in solution.

If you want to test this, dissolve AP in acetone, then add some water, and all the AP comes out as very fine crystals.

I had done that previously but it didn’t seem to come to mind when I made that last post.

My AP was still wet when I poured the acetone into my filter. The crystals fell through the tissue which I was using as a filter (without breaking).

It left me with a white powder and acetone at the bottom of my jar. Stirring made my AP fully dissolve showing if there is a small amount of water present the AP will still dissolve.

When I finally dry some of my AP I will test how soluble it is in water/acetone mixtures at room temp, unless somebody already has this information.

My AP has been sitting underwater for a few weeks now, would this still be safe to dry?

nbk2000
July 2nd, 2006, 05:48 AM
Assuming it's been kept cool the whole time, there's no more danger than when it was first made.

If it's been exposed to heat, then some AP may have subliminated into the threads of the jar and lid, making it a possible explosion hazard to open it. This is usually only a risk to dry stored AP, but wet can do it too if kept long enough at a high enough temperature.

In the future, use saran wrap and a rubber band on the jar, not screw-top lids.

c.Tech
July 2nd, 2006, 10:01 AM
I had placed a funnel (upside-down) over the top of my AP jar but first I had to remove the acetone it was dissolved in. I put it in a hot bath until 1/10 of the acetone was evaporated, I kept letting more evaporate constantly topping with water until I assumed 90% - 100% of the acetone was gone.

I prefer using a funnel over saran wrap because it can be simply lifted off for easy access, all I need to do is put something over the top to block the hole which bugs and other things could enter.

This was uncovered for quite a while, somehow dirt has fallen in so I don’t feel safe drying it.

The one thing I can be sure of is its pH, as I neutralized it in a solution of acetone.

All that needs to be done now is find a safe way of disposal. Any ideas?

Spudinator
July 2nd, 2006, 10:20 PM
http://www.dfwx.com/h2o2products.html


I've searched through the forum to see if anybody has posted it before, but found nothing. This is the cheapest source of H2O2 I have ever seen hands down, One gallon of 35% H2O2 costs only $36! It is available in the following amounts:

1/2 Quart: $9.65

1 Quart: $15.75

2 Quarts (half gallon): $26.10

1 Gallon (in Four 1-Quart bottles): $44.15

1 Gallon (One-Gallon bottle): $36.17



This list goes on, they sell in bulk up to 20 gallons ($372.77 + S&H $124.40). I've been buying from them for the past 6 months, and I couldnt be happier with them. The H2O2 is food grade, very pure.

SWIM uses it whenever they make AP, the yeilds are fantastic.

Alexires
July 3rd, 2006, 10:02 AM
From my experience, wet (with water) AP won't detonate by flame. Even with a sparkler it only deflagrates into a fireball every now and again.

So, you could probably dampen the AP in water and burn it (in an OUTDOOR fire or something like that), or just dump it somewhere.

Dissolve it in acetone and dump it, the acetone will evaporate leaving the AP which will be so spread out it won't be able to detonate.

AP might be dangerous and due caution must be taken, but don't be afraid of it. If you have done everything right when making it, and treated it with care, you should be safe (Or thats how I see it).

Jacks Complete
July 3rd, 2006, 01:27 PM
We don't normally encourage people to put up links about where to get specific things, since they tend to get mobbed by idiots, then they change the way they do things, and everyone loses out. However, H2O2 is not that uncommon, and the link will be restricted to those who log in, so...

Skean Dhu
July 3rd, 2006, 04:06 PM
I got a gallon(in one jug) of 27% a year or so ago for $15, it was a popular brand mentioned on here(which I won't mention for a couple reasons) and used as an alternative to chlorine chemicals for pools. This was found in a chain pool/patio store kept in stock. I only got around to using probably 1/3 of it before it was lost when I moved.

0010110
July 11th, 2006, 06:56 PM
I obtain H2O2 as a topical aniseptic in 3% soulutions. The price is only $0.45 for 500 ml, and all I have to do is visit the local dollar store.

Im not sure how much it costs to boil it down to 30% (500ml to 50ml). but I would much rather do that then order from some website! It works well to lightly boil it about 500 ml at a time. I have done this may times.

As for the sensintivity of AP, I personally find it quite stable. I have handled batches well over 50 grams and havent had any accidents (knock on wood).:D

I have used both megalomanias method and wikipedia's method, and perfer mega's. I like the fact he gives and exact concentrations, when wikipedia just says boil 500 ml down to around 150-250ml.

Surferus
July 18th, 2006, 11:19 PM
One gallon of 35% H2O2 costs only $36! It is available in the following amounts:


It is very strange, here in Russia I buy CC (Chemically Clean by European System) H202 for only about $1 for liter (exactly 33 rubles).
Look here http://vekton.ru/

Cindor
July 25th, 2006, 04:21 AM
I have read everywhere that dry acetone peroxide detonates if exposed to flame, even in small quantities, but my dry AP only deflagrates (I have tried with up a teaspoon of it).

And my AP doesn't detonate unless I beat it with a hammer (and is not a full det.). But in my detonators, it works well (I use 200 mg of flash powder and then 900 mg of acetone peroxide).

I make my AP with nitric acid (I know that for you people that is a sacrilege... but I get it at the same cost of SA and it doesn't make "hot spots"), acetone and 100 vol. or 30% H202 (pH less than 5 so it doesn't need to much acid), with a little bit more H202, and I let it 3-4 days in my refrigerator.

I don't know if I'm getting the tetrameric form or what, but it is pretty stable and storable, once I get it in the refrigerator for over 2 months (...and then I detonated it for safety)

In my country I get 1 L 100 vol. H2O2 for 2 dollars.

++++++++

AP is always capitalized when referring to Acetone Peroxide, Ammonium Perchlorate, or Armor Piercing.

FUTI
July 25th, 2006, 09:34 AM
Nitric acid? Forget the waste of the precious acid...that could be dangerous from the other reasons...I'm not so sure about chemical compatibility in that process...then again maybe you stroke in to a goldmine. If you wanted higher concentration of acid without using sulfuric acid my choice would be phosphoric acid. Did anyone try that? The separate research on this topic is little wastefull. Maybe we should found our institute :D (just kiding but it's a good one).

The_Duke
July 25th, 2006, 11:58 PM
Nitric acid will react violently with Acetone Peroxide, I think I remember someone here actually tried nitrating it with disastrous results. Using a small amount of Nitric acid as a catalyst for AP shouldn’t hurt much, just don’t try and nitrate it!!

FUTI; yes Phosphoric acid will work, but how well will it work...

From PATR 2700;
“Trimeric Acetone Triperoxide was first prepared by Wolfenstein from acetone, 50% hydrogen peroxide and a small amount of phosphoric acid. This method required 4 weeks.”

Cindor
July 26th, 2006, 05:41 AM
"...and a small amount of phosphoric acid...”
Perhaps there where not enough acid. The acid is just a catalyst... For the reaction to take place all you need is a low pH.
If you left the acetone and the 50% H2O2 in a conteiner, after a while you will be able to find AP, because 50% H2O2 has a low pH.

BTW, anyone has tried the metod with tin chloride ?

c.Tech
July 29th, 2006, 10:47 AM
As for the sensitivity of AP, I personally find it quite stable. I have handled batches well over 50 grams and haven’t had any accidents (knock on wood).:D

Just because something hasn’t gone wrong doesn’t mean it wont.

Many people (mostly kewl’s) probably grow evermore confident with sensitive explosives treating them with less respect and handle bigger batches as they go along then BOOM!!!

When you can get the job done with handling smaller amounts put the time and safety into it, what’s to loose? A little bit of time, its better then a hand or two.

Over 50 grams seems quite a bit to me, I've only made AP once and its being stored under water so there has been to opportunity to weigh it. How much is 50 grams in volume, 4 table spoons?

FUTI
August 1st, 2006, 07:58 AM
My idea was that using phosphoric acid (85%) could be beneficial since that acid is more concentrated then hydrochloric acid (36%) and little weaker then sulfuric acid (98%). We would also avoid hot-spot formation that sulfuric acid generates if you have poor mixing. I should stop assume things and try to make it myself maybe.

sprocket
August 1st, 2006, 12:15 PM
My idea was that using phosphoric acid (85%) could be beneficial since that acid is more concentrated then hydrochloric acid (36%) and little weaker then sulfuric acid (98%).
Why not just dilute the sulfuric acid? If you do this beforehand to a sufficient level there will be no significant heat evolution when you add the dilute acid to the acetone/hydrogen peroxide, and no risk of hot spot formation. Battery acid (~37% sulfuric acid) probably works great.

c.Tech
August 20th, 2006, 09:36 AM
Earlier tonight some tests were done on AP, as I said I was going to do in a previously post.

100mg was weighed in a beaker. When 2ml of acetone was added and it completely dissolved. 10ml of was added to the beaker and the AP was still completely dissolved, when a further 10ml of water was added a precipitate was formed.

This shows that excess acetone solution could dissolve some of the yield but it isn’t very likely to be outstanding.

EDIT: The PDF “An AP beginner’s manual” said that, 0.4g of TCAP dissolved in 700-800g of water at 25C (although this was only an approximation after half had dissolved)

15g TCAP dissolved in 60ml of acetone @ 25C. (Also an approximation, there may have been a bit more able to dissolve.)

pearlcrash911
August 21st, 2006, 01:00 PM
Last night I dreamt of making a 20 gram batch of AP, and I followed the synthesis exactly on this page jsmooth7444.tripod.com/id9.html .

I got to the part where it needs to be put in the fridge, and left it overnight. The next morning, I dreamt of taking it out of the fridge to find it had completely crystalized into large 1mm crystals.

Under closer inspection I found that the fridge had in fact broken, and it was only slightly cool all night. This leads me to believe that the product is mostly the dimer, and I am definitely not going to scoop it out with a spoon.

What would be the best way to remove the crystals? I was thinking that it might be possible to fill the jar with water and pour it into the filter. Would it be safe to pour when wet?

festergrump
August 22nd, 2006, 11:17 AM
Would it be safe to pour when wet?
Not a very well thought out dream, was it, if you had to come back here and ask such a question?

Do yourself a favor and do NOT sleep until you figure out the answer (which I'm not gonna give you) for fear of having other dreams which require solutions you have not thought out well enough in advance...

Do I need to tell you not to dry it in a flint bowl and extract needed amounts with a metal spoon, too?

inventorgp
August 22nd, 2006, 11:05 PM
...product is mostly the dimer, and I am definitely not going to scoop it out with a spoon.


It's not nitrogen triiodide!

If you really want to be on the extreme safe side,
the water/filter method is fine.

For sythns and that, use Mega's (http://www.roguesci.org/megalomania/index.html) site.

And I make timer without the fridge. Use higher +30% conc.H2O2.
Try to build up your confidence first.

pearlcrash911
August 23rd, 2006, 01:27 AM
Alright, the water filter method worked great. I also greatly overestimated the sensitivity of my AP.

When I first started testing the crystals every time I moved it I expected a huge explosion at any moment. Then I conducted the hammer test and found that it took three blows with all of my strength to set it off!

Well, its better to be safe than sorry:rolleyes:

c.Tech
August 23rd, 2006, 06:04 AM
If you want to dispose of it safely look up to the third post on this page, by Alexires.

I've burnt quite a bit with a sparkler and it works quite well.

After you fix your fridge you can make some trimer.

EDIT: Even if nitrogen triiodide was wet it still wouldn’t go off.

I don’t think any explosives are very dangerous when wet, except nitrogen trichloride, which is a liquid itself.

Cindor
August 23rd, 2006, 06:43 PM
"Nitrogen triiodide" asi you call it, it's a complex salt: NH3.NI3...
And it does explode in water (just a warning, don't play with it if you appreciate your fingers...)

Cobalt.45
August 23rd, 2006, 07:43 PM
I make timer without the fridge. Use higher +30% conc.H2O2.

inventorgp-
This is interesting. I've always kept the entire reaction at or below 10C, for fear of having an abundance of dimer in the final product. Does w/o fridge mean room temp. or a cooler with ice, or?

What concentration of H2O2 have you found to work best, if I may ask?

How far off is 6:1 acetone to (calculated) 100% H2O2, catalyzed with HCl, to what you use at higher temps? I'm thinking that it's somewhat heavy on acetone, but it has given OK yields in the past.

Anyway, thanks for your time

Cindor
August 23rd, 2006, 08:59 PM
If you use high concentrated H2O2 you have less water for the heat to dissipate, but you get higher yields... And if the reaction it's taking place at more than 10 ºC then you are getting dimeric... and it would be safe until it isn't.

And Cobalt if you have 100% H2O2 (not 100 vol., not the same) don't use it for making AP... you can get really powerfull water-gel explosives with that concentration !. With 100 vol H2O2 (30%) you get greats yields, and save a lot of monney.

inventorgp
August 24th, 2006, 08:33 AM
@ Cindor what do you mean by complex? As I would not of thought of
NI3 having a more complex structure than Acetone Peroxide
C9H18O6(trimer).

@ Cobalt.45, Room temp or just above (25O - 35O), 50% H2O2, 35% HCl, constantly, rigorously stirring.

@ c.Tech, do you use tape around the sparklers? I don't use sparklers
because, fear of deafness from; hot surface, and sparks as you all
know - it causes it to detonate.

Cindor
August 24th, 2006, 01:01 PM
I mean this:
when you mix ammonia water and iodine you are not getting NI3, but NH3.NI3.

Making AP at 25-35ºC is suicide, at that temp. only form of AP made is dimer (or even a monomer). At least you don't use 96+% SA.

And sparklers don't reach detonation...

Cobalt.45
August 24th, 2006, 01:31 PM
Room temp or just above (25 - 35 deg. C), 50% H2O2, 35% HCl, constantly, rigorously stirring.

Sorry, but I just don't see how this would result in anything but AP contaminated with the dimer form.

By what criteria are you basing your assumption that you're getting the trimer form?

Am I missing something?

megalomania
August 24th, 2006, 08:24 PM
The thermodynamics do not support TATP formation at temperatures that high. One should qualify that the dimer form is LESS safe than the trimer since neither are safe compared to any other commercially used explosive compound. The dimer form also has a lower velocity of detonation.

As for the sparklers, I suspect that they fail to adequately reach the deflagration to detonation transition, but it might be close enough for the distinction to not matter from the perspective of the casual observer. Just because a “sparkler bomb” gives a loud pop does not mean it is a high explosive. The criterion is it must exceed the speed of sound to detonate, anything less and it deflagrates. I would conjecture some of the forensics journals are the only ones interested in actually testing sparklers for their explosive properties and publishing the results. I cannot for the life of me recall ever seeing any data on the velocities of sparklers, so I can only speculate.

inventorgp
August 25th, 2006, 05:04 AM
Cindor, it is certainly not suicide. The product is extremely fine
crystals. I have done multiple "tests" with the final product, i.e.
hammer/anvil, heat (nichrome wire), and deflagration (long kitchen lighter).

I used a piece of steel heated to 300Oish placed it on the
micro pile of AP and it detonated. Of course I used adequate hearing
protection.

Mega, no no no, not sparkler "bomb", sparkler as a fuse. As you know
sparkler bombs operate on pressure. I beg to differ (thermodynamics), I find
if I use the method with the temp. at zero it is more sensitive.

Since most of you guys can get H2SO4, I can't (yet)
so I use HCl. If I had H2SO4, I could do some more
tests.

You guys might think I'm some sort of "whacked-up idiot", so I am asking,
is there any way of chemically or mechanically testing for sure if it is trimer?

And I only start to get worried when the temp. reaches +50O
and the vapours fill the room when I'm inside and acts like tear gas!
The temperature I specified is the normal room temp!


I hope it doesn’t sound like I am rambling on. :o

c.Tech
August 25th, 2006, 08:37 AM
@ c.Tech, do you use tape around the sparklers? I don't use sparklers
because, fear of deafness from; hot surface, and sparks as you all
know - it causes it to detonate.

Deafness? That should be the least of your worries with sparklers if you're making AP.

I put my sparklers in an empty Milo tin once with a hole in the top just big enough for the sparkler to fit in. no deflagration, just sparks and fire pouring high leaving black soot on the side of a brick wall.

But it really depends on the sparklers being used, as each manufacturer makes them different, the results should be different.

bcc1985s12
August 25th, 2006, 06:55 PM
I have found 35% hydrogen peroxide at 5-10 degrees celcius seems to work the best for me, both in terms of stability and yield.
I did not know sparklers could detonate AP better than traditional fuze, Does it seem to have the same explosive force as with concussion?

I don't want to get sidetracked too much with the sparkler bomb tangent, but from my experience, sparklers can detonate. By this I mean produce a loud boom and shockwave, unconfined. To do this you need 600-1000 sparklers, bound TIGHTLY together with bailing wire. But as c.Tech stated, it varies from manufacturer to manufacturer.

Cindor
August 25th, 2006, 07:27 PM
Inventorgp if you appreciate your life stop doing AP that way !!!
You are worried about more than 50ºC... I usually get worried when if my AP reaches 15ºC...(It won't explode at that temp, but create dimmer)
And using (concentrated) SA will make it hotter, creating hot spotts.

If you are looking to end like Phone you are in the wright way...
Accidents doesn't happens until they happen.

inventorgp
August 26th, 2006, 07:18 PM
Note taken!

I know about Phone, Cindor, he make kilo portions as I
only make a few grams at a time.

Also, when I talk about sparklers I mean for fuses.
We don't have cannon fuse here.

If you were to observe you would see.

Maybe I'll just shut up as I can see you don't
understand what I'm saying.

c.Tech
August 27th, 2006, 05:28 AM
Maybe with users like Phone there rank should be named “dead” instead of newbie/bottle washer etc.

The rank “dead” should link to a short piece stating the dangers of explosives and how “Accidents doesn't happens until they happen.” To protect and teach any newbies about the dangers before it’s too late.

It should also be a prerequisite for registering members to read, like the rules.

inventorgp
August 29th, 2006, 04:30 AM
I don't make AP that way, that was only an experiment
done once. It was to see the difference between the
cold method and room temp. That was three months ago.

It was just a variation of the synthesis, an experiment!

pearlcrash911
September 12th, 2006, 12:25 AM
I've recently noticed that there are many guides that teach beginners to make AP, but the only places that explain how AP works have been way to complex for beginners to understand.

I recently compiled all of the information that I could find on the science and synthesis of AP into a document that can be easily understood by people with a very limited understanding of chemistry.

So far I have only included the science of the dimeric form, but soon I will add the trimeric.

Unfortunately the diagrams I had on the original document didn't work in the pdf, so some of the references to them may not make sense.

https://createpdf.adobe.com/cgi-pickup.pl/Acetone%20Peroxide%20%20Write-Up.pdf?BP=NS6&LOC=en_US&CUS=b1b4ef9ff9e49fdf7bcfd2ffb0ac630d&CDS=4506203A-0DA4-0819A1

Remember that none of this information is original, it is merely a compilation

Let me know if any of this information is wrong so that I can fix it before I add on the part for the trimer.

Alexires
September 12th, 2006, 10:06 AM
Generally when making AP, I keep the temperature below 0*C, and at -5*C if I can. Then it goes into the fridge for an hour or so, with a rather decent yeild.

Also, I'm sure somewhere we have talked about how using sparklers as fuse for AP is a BAD idea. I have learnt from first hand (thankfully I still have both) experience. If your using sparklers, wrap them in some gaffer tape, or duct tape. A few tests will tell you how much you need.

pearlcrash911
September 12th, 2006, 10:24 AM
I keep the temperature below zero degrees when making TATP, but my synth is for DADP, which only needs to be lightly cooled to prevent overheating.

The ice bath is removed 30 minutes after adding the acid so that the crystals form while the temperature is about 50-60 degrees.

Cobalt.45
September 13th, 2006, 10:47 AM
I'm getting denied-Invalid or expired document ID...

pearlcrash911
September 13th, 2006, 09:30 PM
Sorry, I'm not very computer-savvy, here is the link to the file on rapidshare

'http://rapidshare.de/files/33038287/Acetone_Peroxide__Write-Up-1.pdf'

fragout
November 6th, 2006, 01:18 PM
AP is known to be sensitive to direct sunlight. Does anyone have data about the sensitivity of AP to UV radiation? What would the critical wavelenght for decomposition be? What do you think, is it possible to detonate AP using i.e. a flashlight (similar to the experiment with HCl and H2)? I've tried to find some information in literature but there is litte out there...

NoltaiR
November 8th, 2006, 06:34 PM
I am not sure what you are fearing this UV radiation to be coming from.. if you are just talking about sun light there isn't a problem. However just for safetys sake I probably wouldn't be working with this stuff on a tanning bed either~

Having that said, if you are just worried about the AP being outside, your worries should lie somewhere between it evaporating in the open or maybe you didn't wash the H2SO4 off well enough and you are looking for spontaneous combustion.

And for the millionth time.. I will refer back to the fact that mixing AP crystals with rubber cement is the ultimate solution! Much more powerful, no need for a container, less impact sensitive, helps keep moisture out, and best of all, it is sticky. So next time you want to remove and old window, a small ball of this stuff works wonders, and adheres like silly putty :)

NoltaiR
November 8th, 2006, 06:35 PM
And one more thing.. did you seriously just ask if AP could be detonated by a flashlight?!?!

c.Tech
November 8th, 2006, 08:56 PM
And one more thing.. did you seriously just ask if AP could be detonated by a flashlight?!?! According to the media's response in the liquid explosives terrorist threats it can, but that is probably bullshit like the rest of the things they forced into the sheeples brains. :p

As for UV radiation, I would be worried about the sun, it would heat the peroxide changing it into the more sensitive diclo isomer.

When sunlight can be avoided it should be, instead of drying in the sun a lamp would do just as god a job. :)

P.S. NoltaiR, instead of making a new post you should click the edit button bellow your previous post that is active for 24 hours IIRC.

fragout
November 9th, 2006, 04:10 PM
AP will decompose if irradiated with UV light. Nothing new so far. I think it's just a question of energy intake / time. A Xenon flashlight i.e. produces about 6% of the light between ~170 and 400 nm. So what if we switch on an UV-LED? Unfortunately the lower wavelengths are too expensive to think of.
Would be interesting to know if AP will detonate if treated with one 360 nm LED...if not you'll never have to worry again about sunlight.

(By the way sorry for my mistake above... must be CL2 instead of HCl of course)

Cindor
November 11th, 2006, 10:21 PM
Won't be easier (and cheaper) to use a common silicon diode or something like that ?... if the objetive is an aplicable use.

Universal
November 12th, 2006, 12:08 AM
AP will decompose if irradiated with UV light. Nothing new so far. I think it's just a question of energy intake / time. A Xenon flashlight i.e. produces about 6% of the light between ~170 and 400 nm. So what if we switch on an UV-LED? Unfortunately the lower wavelengths are too expensive to think of.
Would be interesting to know if AP will detonate if treated with one 360 nm LED...if not you'll never have to worry again about sunlight.

(By the way sorry for my mistake above... must be CL2 instead of HCl of course)

I have a LED UV torch around 200-400 nm, I will try it on a very small amount of AP next time I make some, if it does set it off, which I think is unlikely, it could be used as a detonator, but that's a bit farfetched don't you think.

megalomania
November 13th, 2006, 11:24 AM
AP may decompose when exposed to UV light, but at what intensity would a detonation occur? To truly test this theory you would need to expose the AP to an increasingly intense UV light source until it explodes. You could test the decomposition by irradiating a known mass of AP for x length of time. The mass would need to be precisely measured and volatilization compensated for. To really do it right I would think a mass spec should be involved to differentiate AP from it decomposition products.

If shining a flashlight on the AP causes it to detonate, good, that proves that. If it does not, you still have not proved there is no decomp because a mere flashlight would not be enough energy.

There are starting to be produced UV lasers that may wind up in consumer applications. If any UV light source is going to set off AP, it would be a laser. At least the decomp could be measured better.

The best bet right now is UV light for counterfeit detection:
'http://www.photonlight.com/UV-Ultraviolet-LED-Lights-Specialty-LED-Lights-p/uv-ultraviolet-led-blacklight.htm'

This place seems to offer a good selection of pro UV light sources: 'http://www.uv-light.co.uk/'

Ultimately I wonder if this topic is suitable for the “beginners guide” eh? Perhaps a more suitable thread should be used to debate this until the question is resolved.

Cindor
November 13th, 2006, 12:08 PM
The "beginners" can read the beginning of the topic, where they are going to find info about the synthesis, tips and advices... and then they can go throw this "more advanced" part of the topic.

What do you people think ?

fragout
November 13th, 2006, 01:06 PM
I think we need to do some experiments to find out if detonation will occur if AP is irradiated with UV light. Maybe someone has a simple blacklight torch or flashlight at home and might want to test it (with small amounts of course...)? My next opportunity will be around christmas. I suggest to use a 405 nm LED operated with a little extra volts to enhance the output (and decrease the lifetime of the LED dramatically) for a first try.

Bugger
November 13th, 2006, 07:55 PM
Sorry, I'm not very computer-savvy, here is the link to the file on rapidshare
http://rapidshare.de/files/33038287/Acetone_Peroxide__Write-Up-1.pdf
That link has already been deleted, after 2 months or less. Can someone upload it again, please?

pearlcrash911
November 13th, 2006, 10:10 PM
Here are jpg's of the file with the pictures:

'http://i103.photobucket.com/albums/m146/acetoneperoxide/DADP1.jpg'

'http://i103.photobucket.com/albums/m146/acetoneperoxide/DADP2.jpg'

'http://i103.photobucket.com/albums/m146/acetoneperoxide/DADP3.jpg'

'http://i103.photobucket.com/albums/m146/acetoneperoxide/DADP4.jpg'


Ignore the dollar sign water mark, I'm using a freeware scanner.

I should be finished with TATP part soon, so once it is done if anyone wants to turn it into a pdf, I'd be more than happy to send them the word file.

tijo77
November 20th, 2006, 07:27 PM
I had a discussion with a person who worked into the explosives domain for the GRC during 15 years and is presently professor at The Montreal Polytechnic. He told me that for obtaining the Trimetric form of AP you need to put the proper ammount of acid catalyser as well as keeping an eye to the temperature. I searched a long time about the subject (I must admit I didn't read each of the 15 pages of posts on the subject) and never had proper information or justification on the subject. The Beginners Guide to Acetone Peroxyde gives an ammount of Hydrochloric Acid to add (from which calculations could be made if one wants to use an other acid such as sulfuric acid) but does not justify it.

I experimented synthesising AP but not enough to conclude anything and, before repeating it, I would prefer collecting more information.

I am willing to discuss about the issue :) .
Thank you.


N.B.:


When giving a concentration, people rarely say if it is by weight or by volume. Is it because there is a common convention ? (I bought 98% Sulfuric Acid and 70% Nitric Acid A.C.S grade from a chemical supplier and there is no specification).

According that the experiment has been well done (which could be not the case), while experimenting, and following Megalomania's procedures, there was an excess of Acetone for the ammount of Hydrogen Peroxyde used and a lack of Sulfuric Acid (even using 98%). This observation seems to concord with The Beginners Guide to Acetone Peroxyde calculations.

Cobalt.45
November 21st, 2006, 01:24 PM
Christ, is there not any end in sight of the strokes who seem to show up on this thread? Reads the first page of 15, and claims to have "searched a long time".

Every conceivable nuance of making AP has been covered ad nauseum here and elsewhere.

Go away.

nbk2000
November 21st, 2006, 11:33 PM
Bad:

Didn't read the first 15 pages, and spelled peroxide wrong too. :(

Good:

Admitted to not reading the first 15 pages, and actually having some decent grammatical skills. :)

Acrolein
December 21st, 2006, 07:10 PM
Thank you for saying that Cobalt.45, it was really needed. AP is one of the most publicised substances on roguesci! I can't believe that someone would post an article on that!:eek: I can't believe that Arthris was let off with that... He must be impaired to write this.:mad: And how on Earth did this post receive have a five star rating?:confused: Next there will be a post on how to make water, and who knowes mabey next it will be candycanes...:rolleyes: And why post this Mega has the synthesis for AP on his site too. Why have this one, because it is posted twice.

inFinie
January 25th, 2007, 04:02 PM
A friend of mine made AP with the HCl, and he was pretty satisfied with the yield and reports that there were no temperature rises at all while mixing the ingredients. (%30 H2O2 50ml, %15 HCl 50ml, %100? acetone 30ml). He washed it several times and he did not let it dry. He tells that he was near a forest (burned forest in fact. no hazard of fire. no more - it wasn't he :grin:) and he suddenly came up with the idea of gaseous acetone peroxide explosion.

He have placed wet acetone peroxide on a sheet of thin aluminium (folio), folded it several times, made sure that all AP stays as a whole in the folded sheet. It was half the size of a CD cover, in both dimensions he says. But how to detonate? He thought that using the leftover acetone is a good idea. He poured some acetone on the ground in a quiet place, he supported the aluminium fold with three small stones over the acetone poured place. Then he ignited the acetone. It started to burn no matter how much is absorbed by the ground, and there was nothing at the first seconds. After that the square folio started to inflate. It was AP first melting and then vapourising(He thinks it is the case.) When it come to an almost spherical shape, It exploded with a very loud, ear-hurting(from ~10m behind a tree) boom. Aluminium folio was collectible as half a dime sized particles.

He thinks it was gaseous AP with almost 100% exploded as opposed to its solid, uncompressed state.

knowledgehungry
January 25th, 2007, 05:38 PM
Acrolein, I belive that Arthis made this post to end discussion of AP rather than begin it. If someone posts the definitive guide to AP than all the noobies can read that as opposed to asking the same damn questions over and over. Unfortunately the desired effect was not obtained.

inFinie the expansion of the Al foil packet was probably caused by the water turning into a gas rather than the AP. Once the water was gone the AP DDT'd due to the heat.

To prove it was the AP sublimating/melting then evaporating you would need to use dry AP as opposed to wet AP. Obviously this makes the procedure far more dangerous. I would suggest using a kerosene burner lit by a fuse, and using a much smaller amount of AP. Make sure the fuse isn't touching the kerosene otherwise the fuse could wick the kerosene and by lighting the fuse you immediately are lighting the burner. I say Kerosene rather than Alcohol or Acetone because you will be able to see kerosene flames better than alcohol or Acetone thus giving yourself a second to duck and cover if it gets accidently ignited.

Make sure the AP is covered so that sparks from the fuse don't land on it and set it off. You will also need an ignition source for the "gas" AP I suggest a candle six inches away, far enough not to set it off accidently but close enough to ignite the gas.

As for my opinion I think that the AP will go bang long before it turns into a gas and detonates.

inFinie
January 25th, 2007, 06:44 PM
Tomorrow I will try if a small chunk of ice wrapped in Al will cause it to expand. I don't think it will but I will try

KillerLight
January 28th, 2007, 09:17 PM
Well I'm making AP for... 6 years now in large quantities but with same process
.
I separately cool

acetone (pure - from local drug store),

12% H2O2 {contains aqua - didn't find anything about it
styrene/pvp copolymer - some complex polymer
disodium edta (C10H14O8N2Na2.2H2O )
and salicylic acid (C7H6O3)
} it comes by default in my hydrogen peroxide
and HCl (19%) to below 2°C

then I make ice bath (salt & ice)

mix following
30ml of 19% HCl
90ml of Acetone (pure)
120ml of 12% H2O2

stir it for 30min in ice bath and then let it sit for 2 days in fridge below 0°C :)

I don't guaranty it, but I found that it is very stable for an peroxide explosive
i would need detailed chemical analysis to determine his chemical structure.
If anyone haves an idea to determine structure of AP...contact me ...plizz

And for the end. Be very very careful with AP it is strong and sensitive.

I probably hate you
January 30th, 2007, 03:28 AM
You know what , this thread has no right to be called the beginers guide to ap it is mostly a bunch of shit piled together with no real meaning , if there is going to be a thread called the beginers guide to anything that is what it should be , not a big balled up pos , I hope this doesnt piss anyone off ( well not really fa q ) but it is a failure of a guide at least a good one .

nbk2000
January 30th, 2007, 05:45 AM
If it's not to your standards, contribute what you feel to be the proper n00b guide to AP. :)

knowledgehungry
January 30th, 2007, 11:32 AM
The guide is not this thread this thread is about the guide that was made by compiled by Arthis, maybe you should read the whole thread, or at least the first post, before you deliver your judgement :rolleyes:.

The link to the actual guide is on the first page...

FUTI
January 31st, 2007, 04:52 PM
I think that he was provoked by mentioning the comercial hair-dye type H2O2 as starting material. For at least two components listed it contains (I must give the author of post some respect for being wise to mention that and/or notice list of ingredients) we can't be sure will it make things unpredictable. There is a danger it will contaminate the product or alter the process yield.

hazmat732
February 4th, 2007, 09:51 PM
As AP tends to sublimate very easily at normal temperature. It is therefore difficult to store however, if one were to use a food saver vacuum system you would be able to prevent the problem of sublimating.

++++++++

Reducing the pressure makes sublimination even more likely. NBK

Boomer
February 7th, 2007, 12:53 PM
... with the added benefit that due to lower pressure in the bag, sublimation is even faster and the crystals grow and prosper to unknown size!

Either you put it under water (i.e. as a very wet slurry) - and even here you will find crystal growth after month to years. Or you store it in acetone solution, then crash into water and filter/dry before use.

Cyclonite
February 26th, 2007, 07:49 PM
Check out the local pool store for some decent H2O2.

mike16
February 28th, 2007, 03:23 PM
I have just made a new batch of AP, my first after a month or so.

I used 10ml of 35% H2O2, 10ml of Acetone and 2.5ml of 75% H2SO4.
Here are some pictures of the finished product:
http://i164.photobucket.com/albums/u6/mrabjak/Picture014.jpg

I will use it to detonate some NG or blasting gelatin in a few days.:)

To see more pictures visit here: http://s164.photobucket.com/albums/u6/mrabjak/?action=view&current=Picture014.jpg

nbk2000
February 28th, 2007, 03:45 PM
Shitty pictures. :rolleyes:

Try taking some where people can actually tell just what the fuck it is that they're looking at.

209
March 1st, 2007, 01:28 AM
Really good article! I have made AP only once and will most likely never make it again, it gives me the creeps :rolleyes: . It's just too sensitive and dangerous for my liking.

On the other hand, I love HMTD!!!! I have always used it the day of manufacture but I want to store it. I have never read anywhere that HMTD can re-crystalize in the threads of a container, so would it be safe to store in a pill containers for a week or so max??

c.Tech
March 2nd, 2007, 09:04 AM
It's just too sensitive and dangerous for my liking.

On the other hand, I love HMTD!!!!

What makes you sure that HMTD is much safer than AP, both are sensitive powerful peroxides.

I have never read anywhere that HMTD can re-crystalize in the threads of a container, so would it be safe to store in a pill containers for a week or so max??

I have heard of it recrystallising to the lid of a container. Some guy opened the lid and it took off a few fingers of his hand. He posted the pictures from the hospital in a thread of another forum.

If you want to store it (I recommend not) you should seal a wide container with cling wrap and put it in a safe location, I would suggest around some bags of sand.

And mike you said your picture was recent, why is it dated back 2 years ago?

Rbick
March 7th, 2007, 10:38 PM
Ok, acetone peroxide IS a very sensitive ring structure. However, it will not detonate if you breath on it.

I've made many batches of AP, and have never had an accident because I practice proper caution. And HMTD is not much safer, it actually reacts with metals and creates heat, thus detonating it, unlike AP.

So be very careful when making any primary explosive, but its not going to go off when a slight breeze passes by.

209
March 7th, 2007, 10:48 PM
I've made many batches of AP, and have never had an accident because I practice proper caution

ahh, I see, cool

we really need to know that.

Shalashaska
March 7th, 2007, 10:58 PM
Whose question was that an answer to?

Rbick
March 8th, 2007, 12:55 AM
It was in regards to 209's post involving HMTD as apposed to AP due to its instability. Just making the point HMTD isn't so much safer than AP. :)

c.Tech
March 8th, 2007, 03:17 AM
ahh, I see, cool

we really need to know that.

I can really see 209 being banned quite soon.

209
March 8th, 2007, 07:50 PM
Apologies.

I was assuming that Rbick was trying to tell us that AP is dangerous and should be handled with caution even though we all know that. Sorry. ;)

jagster
June 19th, 2007, 01:18 AM
Hmm so from what I've seen researching and reading around on these forums there is no set way to make it. People have used wildly varying mixtures of ap/acetone ratios. Mostly from what I have observed, there is a 1.25 ratio of HP/acetone on average, by volume, using 30-35% h2o2. This is what I used and got pretty good yields, albeit not the level of the liquid lines like I have seen others say.

I've seen a few people work out stoichemetric calculations and they aren't alway the same. And megalomania's formula uses excess more acetone then h2o2 if I recall correctly.

So does anyone definitively know what is the proper ratio to use?

209
June 19th, 2007, 02:52 AM
My ass is probably going to get burned for even replying to you, but what the hell, I am in a good mood :) .

I make AP only in minimal amounts for making caps. When I make it, a small Erlenmeyer comes out (for mixing/swirling). 100 mills of acetone into the flask, cool it in an ice bath (many don't bother with an ice bath when using HCl as the catylist, but they often end up with the dimmer form which more sensitive and decomposes fast) Then add 100mills of *about* 30-35% H202 and let that cool. Then I add about 75mills of HCl over the next 40 minutes. Swirl it for about 7-15 minutes and let it sit.

Often, If I only need a bit, I don't even bother to take it out of the icebath, I just leave it there until I am satified with the yeild and filter it right there, wash it generously or use sodium bicarb.

so about a 50:50 ratio for me, the reactants a dirt cheep anyhow. When I use these amounts I end up with 4-6 grams depending.

Grapes Of Wraith
June 19th, 2007, 01:19 PM
That is a horrible yield for the amount of chemicals you use, I never use more than 50 ml H<sub>2</sub>O<sub>2</sub> and my yield is 20 grams, that is if my scale is correct.

DirtyDan
June 19th, 2007, 04:16 PM
Agreed; what consistency is your end solution 209? Do you get a nice thick mixture? Whenever I use H2O2 in excess of 20% I get a slushy of AP.

As well, I always have better results from conc. H2SO4. It seems like everything goes faster and it doesn't require as much effort to wash. I have to admit the sizzle that comes with each drop is a little discomforting though...

Shalashaska
June 19th, 2007, 07:34 PM
I have to admit the sizzle that comes with each drop is a little discomforting though...

Hmm... thank God... I thought that had something to do with my H2O2. I was starting to doubt my memory as to whether you add the acid to the water or vice-versa when that happened to me the first time; I squirted far too much in for one squirt and it sizzled quite violently, startling me quite a bit.

Cobalt.45
June 19th, 2007, 07:52 PM
Remember the old saying- "do like you oughta; add the acid to the water", or some such.

I (personally) much prefer HCl. H2SO4 with its heating, even if only localized, bothers me a little, although tons has been made using it.

209
June 19th, 2007, 11:06 PM
I also perfer HCl. I have used both HCl and H2S04 and there really isn't much of a yeild difference. The problem with Sulphuric is the almost immediate local oveheating. With HCl I think production is acutally quicker. I am curious of what your H202 concentration is. I boil down my H202 (3%) on the stove in the house from 1L to 100mills, and get about 30% H202. It will readily turns your finger white showing that is is indeed a much higher concentration.

I was curious of the consistence of the final yeild for some time, I am glad that you brought up to the topic of the "fluffyness" of the AP DirtyDan. It seems when I filter it out out the AP I scrap it off the filter paper and onto some clean newspaper. I often move it around every 20 minutes so it will dry faster, but one time, I had forgotten that I needed to be someware at 12:00 and had just finished filtering my AP. I left it sitting on the filter paper on my bench to dry and ran half naked to my job interview (I got the job :D ). When I came home I was supprised to find that the AP was nice and fluffy like snow. I don't know why this is. When I stir around my AP like I usually would make it It would be all parted and not very fluffy at all, anyone know why this is?

Shalashaska
June 19th, 2007, 11:42 PM
I boil down my H202 (3%) on the stove in the house from 1L to 100mills, and get about 30% H202. It will readily turns your finger white showing that is is indeed a much higher concentration.

I always trusted the graphs on H2O2.com that said it didn't work to boil down 3% concentrations, because the boiling points become intertwined somehow, but I'm beginning to believe that's bullshit with the purpose of discouraging home-boiling and in turn, selling more Hydrogen Peroxide. I've heard three personal accounts of people successfully boiling down 3% to get 30% and going on to use it effectively for peroxides.

Cobalt.45
June 20th, 2007, 12:02 AM
Boiling your 3% definitely raises the concentration, if yield is any indication. But to what percentage?

"Hard" boiling isn't needed (or wanted, I suspect), especially after the concentration has come up some. Gentle simmer might be better.

But, the first time you use >20% straight from the bottle, you won't want to go back to dealing with 3%, concentrated or not.

HCl, 30% H2O2, temp held at or below 10 degrees C (but not below 0 C) and enough time for the reaction to finish works well.

I think too cold temperatures and not waiting long enough are the primary reasons for low yields, all else being equal. The exact formulas seem to be very forgiving, although everyone seems to have their favorite.

jagster
June 22nd, 2007, 12:29 AM
Why would you get burned for responding to me. Its a perfectly legitimate question which still hasn't been answered. I'm sure other people wonder the same things and I've seen one other person post that question. There seems to be no set ratios or ways different experts (by rule of their rep. power) have posted quite different ratios (megalomania's vs others)...but majority seem to have more HP I guess.

Someone should clarify.

I know this post isn't about MEKP but has anyone had many good results producing this? There isn't near as much information about it as there is AP. I was curious as it seems to be more stable and safe, and then can be mixed with KNO3 to form a similar fuse detonateable substance. What about blasting power though? Would AP be higher? I havn't seen many posts on definate testing of the KNO3 and MEKP fuse detonation tests and results.

If the MEKP can be stored so good without worry (besides stench) then I wonder why its not talked about more?

Enkidu
June 22nd, 2007, 01:21 AM
I have never made or researched Acetone Peroxide. (What is it's purpose?) Take what you will from my thoughts.

I suppose you use an excess of whatever ingredient is easiest to obtain or cheapest. Who cares (to a certain extent) about the perfect ratios so that each reagent perfectly uses the other one up?

If you want opinions outside of The Forum, do some patent research. (Be warned, patents are often bullshit. Always view patent claims and descriptions with skepticism.)

If you really want to know the answer, do research on peroxidation reactions. Try to find The Chemistry of Peroxides Vol. 1 at a university library. I think it's part of the Patai Series.

I would suppose that no one is interested in MEKP because anyone who would be simply makes Acetone Peroxide instead. Isn't there a thread called 'Who Voted MEKP off the Island?'

BTW, be careful with abbreviations. Here AP often means Acetone Peroxide. Almost everywhere else (at least in pyrotechnic boards) it means Ammonium Perchlorate. HP is a rather esoteric abbreviation. (How hard is it to write H2O2?) I try to avoid everything but standard abbreviations for clarity and to avoid confusion. That's just my opinion. :)

209
June 22nd, 2007, 01:44 AM
I was looking at making some MEKP some time ago but then realized the concentration of the H202 needs to be in the neighborhood of 45-50%. Is this true? I would like to make some MEKP, I have never bothered with liquid explosives before so a new synth is always exciting:). Would it work to make MEKP with boiled down H202? I understand that you would get a crap ass yeild if it did work, but its better than nothing, do you think it would indeed work?

jagster
June 22nd, 2007, 03:01 AM
People have made it in this forum using the standard 30% or so H2O2. Just use methyl ethyl ketone instead of acetone in the reaction. That thread you mentioned strays way off subject and doesn't provide very much information. It also talks about making the crystal form instead of liquid. Most people on here who say they have done the synth talk about an oily liquid (which might have crystals disolved in it). I'd assume just buy it and concentrate down but I don't know a good way to do it with heat as it will detonate if you get it too hot...and I tried letting it sit out for 2 weeks and nothing changed it didn't do anything not sure what the deal was. I never tried putting it in the sun though but that scares me....

Yea I understand what you say enkidu but if AP is so dangerous why not make MEKP. I made some AP by the way, and hit it on two wrenches and could not get it to snap off. It must take a pretty solid blow if it was cleaned well during synth. I couldn't find my hammer lol.

Why research the peroxide reactions when so many great minds in this forum could answer it off their head :). Some have even explained this very thing maybe not in detail but the basics. If anything I would want to conserve the H2O2 because its harder to get. But I still want max yield.

Cindor
June 22nd, 2007, 03:26 AM
IMO an excess H2O2 is wanted in peroxidations due to H2O2 decomposition.

In the case of AP an excess of acetone can be dangerous, because your AP is with a solvent, and when it evaporates you are left with bigger crystals, and those can break, leading to an unwanted detonation.

In the case of MEKP the amounts of H2O2 are the ones that defines if your MEKP is a monomer, dimer or anhydrous dimer. (Please correct me if I'm wrong)

Enkidu
June 22nd, 2007, 04:11 AM
If anything I would want to conserve the H2O2 because its harder to get. But I still want max yield.

If that's the case, look around for a recipe that uses the largest acetone to hydrogen peroxide ratio. AFAIK, if yields were solely dependent upon the limiting reagent (which they are not), using excess acetone would not lower yields but instead make sure that all the hydrogen peroxide is utilized.

Why research the peroxide reactions when so many great minds in this forum could answer it off their head :).

This thread (http://www.roguesci.org/theforum/showthread.php?t=5150) is one reason.

In the case of AP an excess of acetone can be dangerous, because your AP is with a solvent, and when it evaporates you are left with bigger crystals, and those can break, leading to an unwanted detonation.

As I said, I'm not sure what 'recipes' people use for acetone peroxide, but if you're worried about large crystals, pour a thin stream of the dissolved acetone peroxide solution into a beaker of water with good stirring. That procedure should precipitate very small crystals.

In the case of MEKP the amounts of H2O2 are the ones that defines if your MEKP is a monomer, dimer or anhydrous dimer.

That's very possible. I was under the impression that temperature controlled the form of the peroxide. I.e., warm temperatures are conducive to the dimer form of acetone peroxide forming, and colder temperatures are conductive to the trimer forming. However, as I've not looked into this, I'm probably talking out my ass.

zeppelin69
June 22nd, 2007, 01:19 PM
MEKP is made in nearly the exact same way. From all of the posts that I have read on here, it looks like most people don't like it. I have made it a few times though, and I LOVE IT!

I usually use it as ANMEKP, and it is surprisingly powerful in small amounts, and only needs a very small amount of AP to set off.

Be careful with it though, and make sure to wear gloves while you handle it, it is toxic, and will bleach your skin (or anything else it gets on for that matter).

Just my two cents on the acetone to peroxide ratio, I always use more peroxide to prevent the AP from dissolving in excess acetone.

Cindor
June 23rd, 2007, 03:06 PM
I made MEKP a few times and always used the 30% H2O2 and got no problem in the synthesis.

Also my MEKP doesn't smells like others useres MEKP, both my MEK and H2O2 are technical grade (I bought them in a chem supply).

PS: I like it too :P hehe

209
June 23rd, 2007, 11:14 PM
I can't seem to find MEK anywere........

Enkidu
June 24th, 2007, 01:10 AM
Where do you live? :rolleyes: It's at my Home Depot. I live in the Southern US. (MEK stands for Methyl Ethyl Ketone.)

Shalashaska
June 24th, 2007, 01:33 AM
Location: Canada

When he said this, I went to the Great OTC survey to find out if Canada had MEK or not. Either way, I would look quite feverishly for it before asking the Forum to tell me where to find it.

megalomania
June 24th, 2007, 09:42 PM
MEK is one of those regional solvents that is not carried by all stores all the time. It is a painting solvent, so any place that sells paint and painting supplies would be the logical place to look. It just depends on the store and the area you happen to be in.

southpoorboy
July 12th, 2007, 02:17 AM
hello, has some of you information about PA's equilibrium constant, energy of formation, enthalpy of formation, Volume of detonation gases, heat of explosion (almost nule isn't it?), specific energy, etc? I am also traying to understand the reaction mechanism that it's megalomania's page but between my obtuse head and the complexity of the subject… well it seems that I've to read more books of organic chemistry… any data would be well received. Thanks (my English is crap, I know)

Rbick
July 12th, 2007, 08:39 PM
Southpoorboy-

This thread is about Acetone Peroxide! Not Picric Acid... But yes I do have the information you are looking for, or at least a good portion of it. If you PM me or post in the Picric Acid thread, I'll be more than happy to give it to you :rolleyes: However, make sure you do a thurough search of the forum for the information you seek, and let me know if you still need it.

If you mistyped PA and meant AP then yes I have some of that information for you as well. I'll just have to do some of the equations myself. Not many books contain info on AP, as people who are mentally stable try to avoid it. I am not mentally stable :D

stephenb25
July 13th, 2007, 01:43 AM
I saw that some people up the top of this page were talking about the correct ratio to use when making AP. As people have said there is no required ratio many will work but I thought I would post stoichiometric ratios to clear things up.

The equation is 3CH6O + 3H2O2 gives C9H18O6 + 3H2O

I did this in grams as it is easier to understand so:

174.24g C3H6O and 102.04g 100% H2O2 gives 224.24g C9H18O6 + 54.04g H2O.

So that means if you are using 30% H2O2 you need 336.73g for every 174.24g acetone.

These are the exact ratios (they can be easily scaled to you need or in program) but as you know they are not always the best and it is often good to use a little more to ensure a complete reaction.

I stumbled upon an excel spreadsheet someone had made for calculating AP ratios in a torrent and I have checked them and they are very close to stoichiometric ratios I thought this could be of help to some people.

Can't seem to attach the file, so I uploaded it to rapidshare.
http://rapidshare.com/files/42621590/AP_calculations.xls.html

++++++++++++

I'd like to point out that Excel spreadsheets can contain harmful macro viruses, so any downloading the linked file, be sure to scan it before running it. NBK

camelslaper13
July 14th, 2007, 06:02 PM
Anybody know how to optimize an AP reaction that uses citric acid as a catalyst? I tried to make some today with lemon juice (couldn't wait to buy some real citric acid...) as the catalyst, just to see if it would work...

50ml H2O2 27%
50ml acetone
50ml filtered lemon juice concentrate

I ended up with a tiny (head of a pin) sized ball of AP filtered from the cloudy solution I let sit overnight.

I also got my hands bleached white from not using gloves when handling the 27% H2O2...

Anyway, I lit the filter on fire, and when the flame reached the AP it just made a little "whoosh".

++++++++++

I have tried both ascorbic acid (vitamin C) and citric acid, and neither worked. Apparently only mineral acids like HCl or H2SO4 work.

nbk2000

southpoorboy
July 19th, 2007, 04:21 PM
Again I request pardon by my badly written English… Yes, by PA quice to say acetone peroxide... I am not mentally stable either! But AP is cheap and easy to produce! Thanks and I wait anxious for all the information available!

Hey! I am not alone! I am just another mentaly unbalanced human being in the world!

The_Duke
July 19th, 2007, 06:00 PM
Remind me why we want a self proclaimed mental case with poor grammar skills and limited knowledge of the English language hanging around our forum…:rolleyes:

Aside from your butchery of our language, that fact that you claim to be mentally unstable indicates that you are not only a danger to yourself and others, but also to the well being of the forum. We simply cannot tolerate such a risk.

I suggest you go back to lurking and pray to whatever god you wish that the beast comes not for you...

Rbick
July 19th, 2007, 06:20 PM
Sorry Duke, I am the one who made the comment towards being mentally unstable. In a joking fashion of course... Then again, what mentally stable means is a matter of opinion I guess. Anyway:

Southpoorboy,
I'll give you some technical data on acetone peroxide, but its more for your own saftey. But you have to promise me two things:

1. Be more careful with your posts, being you only have 3 and first impressions mean a lot. The beast is always hungry ;)
2. You won't attempt to make any until you have all the saftey equipment and knowledge you need

Please be careful when you're making this stuff! And don't wait for me to send it to you, research on your own. Wikipedia has a 5 page report on AP alone.

Cobalt.45
July 22nd, 2007, 02:16 PM
But AP is cheap and easy to produce! You'll get no arguments, there.

But that criteria is not why one primary is chosen over another.

AP has its uses, and its "fans". But using the ideal primary as compared to the cheap and easy-to-make primary, will always be the better choice.

If you are using AP for anything other than a primary, you may be headed for trouble, IMO. It is not a substitute for flash powder.

NoltaiR
July 23rd, 2007, 01:25 PM
Acetone peroxide will always be a hot topic at an E&W forum.
Sometimes I worry that it's a gateway explosive. It gets people addicted to explosives and before you know it they are synthesizing nitroglycerine and RDX. :)

Ah well just a bit of sarcasm; personally I love AP and I never once regretted bleaching my hands white from the peroxide.

Just hope that someone posts some pictures for entertainment ;)

Shalashaska
July 24th, 2007, 03:26 AM
Ah well just a bit of sarcasm; personally I love AP

I agree.
Although there applications for a primary where people try to shove AP into the hole like a jigsaw puzzle, I think it is simply the most convenient and versatile primary there is. Although it is (inherently) very sensitive, all primaries are... simply because that's what they're for; to make DDT with as small an amount as possible.

Sometimes I worry that it's a gateway explosive. It gets people addicted to explosives and before you know it they are synthesizing nitroglycerine and RDX.


And I must second that as well. It was my first explosive, before ANFO, black powder, NC, or even flash powder. It was certainly not the last :)
I think we need to establish APKA (Acetone Peroxide K3wls Anonymous) :D
One second I was k3wlly blowing up bullet shells full of the stuff, next thing you know, I'm a member here, and realizing how incredibly retarded that was :)

blythenator
August 22nd, 2007, 04:33 PM
I just had great success using 3% hydrogen peroxide.

Had 1000 Ml 3% HP (7 cups), simmered it at 155-158 Degrees F until I had 3 cups left.

Cooled it with an ice bath, then added 120 ml of acetone. Waited for it to cool below 8 degrees C. then slowly added 50 ml of hydrocloric acid 30%.

Stirred about 5 minutes, and threw it in the fridge... 8 hours later I am seeing a good yield, way better than not simmering down the HP.

++++++++++

But you failed basic grammar. Banned.

HemiDodge
August 27th, 2007, 04:59 PM
I've read alot on the making of AP. I am trying to find more information on the "pressing" of AP. I have read that the AP should be dampened with alcohol before pressed. Does anyone agree with that? Will the AP dry out okay after being wetted? All should be done behind some type of blast shield with rugged leather gloves being worn. If a person used a standard straw from a grocery store, what kind of device/tool did you press the AP with? Any insight would be appreciated.

I've tried searching "pressing AP" However, "AP" is a letter short of the criteria of 3 letter word length.
I have searched pressing acetone peroxide and i've only found 2 methods of "pressing" AP.

I thought that since so many people out there have done this, that a few might give feed back on "how" they have done it.

With AP being a sensitive primary, I would like to know how hard I can press... Should the mix be wetted? I just want to be sure of everything before I make AP. I have no questions or concerns on making the AP. No questions on storage, just making that blasting cap.

chemdude1999
August 27th, 2007, 06:28 PM
Try "pressing ap" in the Google box in the RogueSci.org advance search page. You should find what you need.

Alexires
August 28th, 2007, 03:47 AM
I would like to know how hard I can press... Should the mix be wetted?

You might want to investigate the term "dead press" in relation to "how hard" can you press.

Rbick
August 28th, 2007, 10:02 AM
Hemi,

I have also heard of people pressing AP while wetted with alcohol, although I have never done it myself. I would assume if you are using high conc. alcohol (say 90% or higher) it should dry quickly. But again, I'm not sure on this.

The way I have found to press AP is by holding the dowel (which should fit perfectly into your cap) with a 16 inch wrench. The cap is held in a clamp, but not tightly enough to cause problems. With your arm fully extended, this should create enough room between you and the cap that it won't seriously hurt or kill you, should it explode. Of course thick gloves are worn and a face shield. I leave as little of my body exposed as possible.

As a way to protect myself, I have reduced the use of AP to a minimum and replaced it with ETN. This is much safer to work with, and 2g ETN can be detonated with as little as .2g AP. Not to mention ETN is vastly more powerful than AP. I would suggest you find a similar method and work with AP as little as possible, unless you're making APAN, in which case you should be extra careful. Good luck :cool:

LibertyOrDeath
August 28th, 2007, 04:36 PM
With AP being a sensitive primary, I would like to know how hard I can press...
Here's a file that gives the figure of "at least 100 pounds" -- which I assume is supposed to mean "100 pounds per square inch". However, I cannot vouch for its accuracy, even if it is from someone at MIT:

http://web.mit.edu/semenko/Public/Military%20Manuals/Single%20Files/Improvised%20Primary%20Explosives.pdf

Assuming that figure is correct, remember that 100 psi is not as much as it might sound like. If your detonator and the fitted dowel you're using to press the AP has a diameter of, say, 0.25 inches, then 100 psi would be applied by only 5 lbs of force on the dowel. This is the stated minimum, though; I'm not sure what a safe maximum pressure would be. If you want to experiment with such things, a shielded press might be a good idea!

That PDF also recommends wetting with alcohol prior to pressing, which sounds like a very good idea. Like Rbick, I've read about others doing that as well.

megalomania
September 9th, 2007, 08:53 PM
Since the military long ago decided AP was unsuitable there is a lack of concrete data on the finer points of its use. Wetting the AP with water or alcohol should greatly decrease its sensitivity while being pressed. You may want to consider using some vacuum aspiration after pressing to remove the wetting agent.

Since there is a lack of data you will have to determine for yourself what is safe. You may want to consider doing some experimentation of different forces of pressing to see what works for you. If you can measure the force of pressing that successfully makes a cap without causing a detonation, there is no need to use greater force. Either way consider letting the RS community know about your results.

chemdude1999
September 11th, 2007, 10:17 PM
If I may make a few recommendations for test pressing AP:

Try using weight plates. You'll have a good idea of the amount of poundage needed. I understand this is not nearly as accurate as using say an arbor press with gauge, but you won't risk damaging the equipment. Plus, if you do get a little explosion the plates should contain it.

Start with a very small, wet amount of AP. Prepare the container, or simply use a flat piece for testing. Record the weight. Start adding the plates and checking your sample each time. For larger samples it may take a few hundred pounds. Record any explosions and examine what happened. Stop once you reach your desired consistency (if you will).

I have several hundred pounds of plates, but don't have the time to do this.

This method would give concrete results for pressing AP. It would provided a table of poundage needed, plus it might create some methods for actually pressing the stuff.

+++++++++++++++++++++++++++++++

Perhaps, one could make up a jig for quickly pressing caps. I'm not sure if this has been discussed. Two plates with the bottom one holding the cap/container and the top one holding a matching rod would be the main components. The rod (wood dowel perhaps) would press the AP into the cap fairly precisely. The plates would be guided on the sides so as to keep the alignment. Using a previously created table of weights and AP amounts, one could quickly generate the required pressings. Maybe over-thought, but might be worth investigating.

iceshrike
September 27th, 2007, 09:25 PM
Hello everyone! I think this is my first post but I just have a few questions.

First of all I read basically this whole thread and I couldn't find a post on how to find out how much catalyst to use in the reaction, and also I wrote an equation using some method a member posted earlier. This synth using 50ml of H2O2, worked out called for 4.58 ml of Acetone. Is this correct?

totenkov
September 29th, 2007, 09:46 PM
I hear NBK coming :D.

This synth using 50ml of H2O2, worked out called for 4.58 ml of Acetone. Is this correct? NO.

God god man. Do you know how many threads, sites and fucking essays written on this damn substance on the web?!!!!! Did you take a single second to UTFSE???

60mls acetone, 50mls H202 60mls HCl.

Rbick
September 30th, 2007, 05:07 AM
Woah there totenkov, take it easy. Part of being professional is also maintaining politeness and courtesy, (despite his obvious lack of knowledge) and professionalism is key to this forum.

Also, seeing as just arrived here, I would be more careful about my words. Leave the insults and what not to the boss. Although I think it would have been best for you not to respond in the first place, here is an answer better suited for you:

"No iceshrike, that is not correct. Please refer to the Acetone Peroxide section on mega's explosives labs page (www.roguesci.org/megalomania). Here will you find the answer you're looking for."

Responses like my example above will get you much more respect here than posts that aim to degrade and insult other members. Good luck, hope you don't get banned :)

totenkov
September 30th, 2007, 01:57 PM
Not at all new to this forum Rbick. Been floating around for quite a while, just didn't bother to get a membership. Ok alright, maybe a little harsh on the guy. Sorry :)

But seriously, AP? Ok fine, I'll shut up now :D

Hinckleyforpresident
September 30th, 2007, 08:36 PM
To Rbick referring to the pressing method:
Are you doing this with plastic or metal? I only ever dare use metal if I'm using a press with armor plating!

Also, (assuming you use plastic) how do you keep the straw from bending/warping/breaking when you press it in a vice? Whenever I put it in a vice and press the pressure sort of wrinkles the straw so it looks like an accordion.

Perhaps I just use bad straws.

Rbick
October 1st, 2007, 04:22 PM
I've always used plastic straws. I have had that problem as well, but only with ETN. I've never tried to press AP hard enough to have that happened, even if it was wetted with alcohol. The straws I use are pretty "heavy duty", and I've never had a problem with my caps being powerful enough.

But I don't think there is really a way to prevent this from happening. You could buy hunting arrows and cut them up. The material used for making arrows is the same used to make commercial blasting caps (I'm unsure of the exact composition), and is sturdy but shatters well. This makes the perfect blasting cap :cool:

Alexires
October 1st, 2007, 11:17 PM
Rbick - Just to shed a little light on what those arrows may be, my arrows at home are carbon fibre adhered together with some kind of resin.

They can splinter if the arrow has been mistreated badly (a bitch if it get in your skin) but tend to sheer off in a line under strange conditions.

They are very strong, and would be a nice touch if you can be bothered buying carbon fibre for your dets.

Rbick
October 2nd, 2007, 12:15 AM
Good call Alexires. The following quote is from wikipedia.org after seaching "carbon fiber":

Carbon fiber is a prime material for use in archery. Many modern-day arrows are made as either aluminium-carbon composites or entirely of carbon fiber

That sparked a memory, as I remember aluminum-carbon fibers being mentioned. I think the use of this type of material for caps was invented by Nobel when he was replacing the unreliable detonators of BP with Mercury Fulminate for detonating Nitroglycerine. Apparently the fiber is easily shattered by the explosive, but is otherwise flexible against bending and pressure. Maybe a few arrows could be bought and tested. It wouldn't be hard to cut one up with a hack saw at the desired lengths, press some primary in, and seal with glue.

nbk2000
October 2nd, 2007, 04:46 AM
Carbon fiber didn't exist back in Nobel's time, so I assume you are referring to aluminum? But that was also very expensive, because they didn't use the cryolite process back then, so aluminum was on par for silver in cost.

Charles Owlen Picket
October 2nd, 2007, 10:39 AM
OT alert....

Perhaps the best source of aluminum cap bodies I have seen or examined, etc was the use of Easton (aluminum) Arrows which are made with very high quality anodizing inside and out. - As well as being very strong, will "shatter" when forces reach the point of shear factor. - When compared to other sources of Al tubing which will be very pliable, the Easton Arrows use a very tough Al that breaks apart in a fashion similar to the commercial DuPont dets I have actually examined years back.

Bert
October 2nd, 2007, 12:10 PM
I think the use of this type of material for caps was invented by Nobel when he was replacing the unreliable detonators of BP with Mercury Fulminate for detonating Nitroglycerine.
Nobel used Copper capsules. These remained the standard for a long time, untill Aluminum replaced it due to reactivity and cost issues.

Copper worked quite well with fulminate/chlorate for a long time-
http://www.roguesci.org/theforum/showthread.php?p=54630#post54630

Hinckleyforpresident
October 2nd, 2007, 02:02 PM
They also sell thick aluminum tubing at ACE. It seems like it's very similar to the arrows but still a hell of a lot cheaper.

Charles Owlen Picket
October 2nd, 2007, 09:33 PM
They also sell thick aluminum tubing at ACE. It seems like it's very similar to the arrows but still a hell of a lot cheaper.

On the contrary; it is exactly what I am referring to when I say that the Easton arrow tubing is extremely brittle and makes for a very professional cap body. The Al tubing sold commercially is VERY flexible and that in itself is of no great importance IF one is using professional materials (azides) however the containment of an energetic material utilized for initiation via detonation will possibly be aided by less flexible containment.

When examining an "SSS" cap some years back it was [pointed out to me] that very unique qualities were imparted via manufacture of that capsule. The anodizing as well as the structure were quite unique. There was no way for me to tell for certain but the capsule did not appear to be as soft as the material designed to be bent (as is sold by Ace).

There is a difference (albeit small) in the detonation of a contained material and these small differences may make a HUGE improvement when all aspects of an explosive train are examined. I have no proof of this; it's simply an idiosyncrasy I noticed in the past.

Hinckleyforpresident
October 3rd, 2007, 02:38 AM
Sorry Charles, I misunderstood you. I thought that you were referring to softer aluminum (aka cheepo practice arrows or tubing).

totenkov
October 3rd, 2007, 12:50 PM
Using metal for caps is not very wise. Sure it works fine in the charge, but when you are using peroxides, your ass in really on the line. I get real nervous packing AP into caps even when they are held in a vise and I am wearing full body armor!

The best casings for caps would have to be vynl tubing from the hardware store. You can press the AP and simply fill one end with hotglue and pack it in afterward stick in your e-match or fuse, thats it.

Another thing it works good for is det-cord, however you probably already know that. (dont be using AP! A more stable one like ETN or Picric is better)

nbk2000
October 3rd, 2007, 03:16 PM
Confinement is a necessary condition for full power detonation. Weakly confined, the tiny explosive charge in a detonator may not be able to impart a strong enough shock to the main charge, to cause a high-order detonation. :(

Hinckleyforpresident
October 3rd, 2007, 03:21 PM
When I press metal AP caps I use a armor plated press. I have tested the armor and the components against packed AP caps and every time they survive with little more than a scratch.

Also, I have always used 1/4 inch copper pipe as the casing. I will certainly have to try using the arrows though.

ETCS (Ret)
October 16th, 2007, 06:51 PM
I had a bottle of 3% household Hydrogen Peroxide that had been in the medicine cabinet for more than 5 years and wondered whether it had any usefulness left.

I poured the contents of the bottle (approx. 400 ml.) into a small stainless kitchen skillet that I had carefully scoured and cleaned and brought the heat up to just below boiling. A cloud of water vapor formed over the surface, as from a cup of hot coffee. After approximately two hours the liquid had reduced to about 70 ml. so I turned off the heat and let it cool.

During the entire process there was no smell or bubbling and the liquid remained clear.

When it was sufficiently cooled I applied a drop of the liquid to my fingertip and observed shortly that the skin turned white.

Wondering whether it would be sufficienty strong to use for TATP preparation I transferred the liquid to a suitable container and added the necessary acetone, approx. 30 ml., and chilled the well mixed solution in the freezer for about 30 minutes.

Upon adding 1 ml. of 93% Sulfuric Acid a small amount of precipitate formed. Letting the solution react for about 12 hours at room temperature resulted in the formation of a large amount of precipitate which, when filtered and neutralized, resulted in about a heaping tablespoon of AP.

Apparently the Hydrogen Peroxide solution degrades very slowly over time and the evaporation process of fortifying it, when done carefully, results in very little loss as well. The results of this experiment are surprising.

ccw8076
November 4th, 2007, 12:55 PM
I have not tried to make AP for several years. I normally use HMTD or some commercial blasting caps I can get from one of my colleagues. Anyway, yesterday I tried to make some AP using the directions on Megalomania's site. It went all well and good, and formed a little layer of white precipitate. But it' didn't look like traditional AP to me. I filtered it using coffee filters, but it wouldn't collect. As soon as it was poured into the filter, it disappeared. I was wondering if anyone could shed some light on what I am doing wrong.

I used:

Pure Acetone as purchased from a hardware store.

3% Hydrogen Peroxide, but I used ten times as much like Megalomania said to.

Floweasy Drain Opener, which by the specs at Plumbest.com, contains 94% sulphuric acid by weight.

If anyone could be of any help, that would be great, thanks

totenkov
November 4th, 2007, 04:57 PM
how long did you give the AP to form?

ccw8076
November 4th, 2007, 06:51 PM
A full 24 hours in the freezer. To be honest it looked more like semen in water than AP crystals.

Hinckleyforpresident
November 4th, 2007, 07:08 PM
Did you also scale up the amount of sulfuric acid with the hydrogen peroxide?

ccw8076
November 4th, 2007, 08:33 PM
yes, I used 7 ML instead of 3 like Megalomania says. I figured, that for such a volume of water added into the mix, the acid must be increased by about 130%.

Hinckleyforpresident
November 4th, 2007, 08:43 PM
You need more.

For 300 ml or hydrogen peroxide (3%) with 50 ml acetone I use 30 ml of sulfuric acid.