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Arthis
June 7th, 2003, 09:21 AM
I tried to make a short synthesis about AP, as we wanted to do long ago (not especially about AP, remember Noltair's project). I had some time (not much) so here it is.


-------------------------------------------
An AP beginner’s manual

Introduction
A few chemistry basics
Synthesis
Precursors
Research and FAQ


Introduction

AP, or TCAP, stands for acetone tricycloperoxyde. It’s a common very sensitive explosive for beginners, as it’s easy to make, does not require any chemistry skills, nor hard to find chemicals.
It has some obvious advantages, some even more obvious problems, but as it’s often made by beginners, it may be useful to compile most common information and research about it, made by members of the Forum. Of course further research and experiences are welcomed.

AP comes in 2 different forms, dicyclo and tricycloperoxyde.
Dimer and trimer picture + the reaction

The dimer form is more unstable, and tends to self-decompose easily while the trimer form is more (relatively) stable.
You should try to get the trimer form, as it’s also more powerful, and for that you need to keep the reaction the coolest possible.
You may have noticed that the acid is not present in the equation: it only acts as a catalyst.


Method to synthetise AP
[Write your own work you plagiarizing bitch. - ALENGOSVIG1]

Precursors: there’s not many things to say about them.
Acetone is a common solvent you can buy in any drugstore, homestore… If you can’t, you may find it in some nail polish remover, but be careful as it’s expensive, and some nail polish remover contain no acetone (subtitutes are used, better for your nails), and there are many other stuffs that may parasite the reaction.
Hydrogen peroxyde is oxygenated water that you can buy in pharmacy, as antiseptic or as hair bleacher. It should then be 3-6 %, just add some more to have the good number of moles in the reaction. It is normally sold to everyone in drugstores, as a bleacher, to the concentration of 30-35 %, and it will be far cheaper. Just ask if you can order some. Taxidermists and hair shops should have some, you can ask there too.
Hydrochloric acid can be found in any store, it is pH relevant for swimming pools. It’s very common. You may want to use another acid instead of this, see in the Research/FAQ section for that.

Research and FAQ
(mostly a FAQ for the moment though)

Concentration of the hydrogen peroxyde
Using more concentrated H2O2 should not change the yield, as long as you put the same number of moles in the mix: if you use 6% instead of 30%, just put 5 times more hydrogen peroxyde. But note that AP dissolve (not much) in water so you may lose some. Some members have noticed that usually, they get better yields with concentrated H2O2.


Acid used
The acid acts as a catalyst and about any acid can be used in AP synthesis. Citric acid and sulfuric acid are also commonly used but some differences can be noted, and must be taken into account.
Sulfuric acid: adding it will cause immediately a local overheating and ebullition. You must add it drop-by-drop. A good solution to avoid a temperature elevation is to dilute your acid and let it cool (e.g. from 95+ % to 30%).
Hydrochloric acid: easy to get, it may be the best suited acid in this synthesis, regarding to its low cost. It is safer too, as pouring the whole acid at once in the mix will not cause (even local) ebullition or overheating; however, the global temp of the mix will rise thus favoring the formationof the dimer, or even producing tear gas. Don’t forget that it’s easier to keep the reaction cool than cooling it down once the temperature has raised.
Citric acid: this is not a strong acid, but it works well too. The main interest, excepted the ease in keeping the reaction cool, it that it’s way easier to wash the AP and make it neutral, compared with the use of strong acids.

Toxicity
Pure AP is not toxic, doesn’t go trough the skin. The problem may only come from (unwanted explosions ;) ) the acid kept in, if not well neutralized.

Color
Normally AP is pure white. However colors may appear with impurities, for example rust if you used an iron spoon to stir the mix. Impurities may also be due to impure reactants like acetone from nail polisher.

Volatility


Pressing AP


Thanks

All those who have made experiments, my family and my cat for all the love they gave me, sniff,… Alengosvig1 for the method I copied from his website. [Yeah, without even asking me. - ALENGOSVIG1]

------------------------------------------

it's far from being complete. I typed it on word, so it doesn't look very beautiful here, maybe I'll put it in pfd if I find something to do it. Pictures of the molecules and reactions are ready, too bored to post them though. (and there's no real need here, just note that they exist, I'll put them in the final version).

I'm waiting for your comments, and if any of you wants to make a part of it feel free to send them.

I'll try to complete it when I have some time, I'll send the different add-ons as soon as they're ready.

zaibatsu
June 7th, 2003, 10:46 AM
Arthis, if you need someone to turn it into a PDF file for you, I can do that. However, I would require you to email the pics etc to me.

knowledgehungry
June 7th, 2003, 11:12 AM
I have noticed that when using low concentrations such as 3% H2O2 it is best to use concentrated H2SO4. With such a low percentage of H2O2 there is very little trouble with overheating, and as many other people have mentioned the amount of acid requires varies inversely with the percentage of H2O2. When using HCl with 3% H2O2 i have to use the same amount of HCl as acetone:eek: for me to get any results, and it is still a smaller yeild due to the increas of H2O for the AP to dissolve in. Just thought you might want to drop a footnote about that.

inFinie
June 7th, 2003, 12:57 PM
So, what's the solubility of TCAP in water?
(in x gr TCAP in 100gr H20 @ 25oC)

ALENGOSVIG1
June 7th, 2003, 04:03 PM
Mix the actone and the hydrogen peroxide in a beaker and cool it to 5 degrees celsius in an icebath. When the liquids are mixed, it will begin to heat up a bit and turn slightly cloudy. When it's been cooled to 5 degrees, you must slowly add the hydrochloric acid to the acetone/hydrogen peroxide solution. Add the hydrochloric acid 2 ml at a time. If the temperature of the acetone/hydrogen peroxide solution approaches 10 degrees, stop the acid addition and wait for the temperature to drop back down. The addition should take about 20 minutes. After all of the acid has been added, let the solution sit in an icebath for 4 hours. You may have to replace the ice

After 4 hours, there should be large amounts of white precipitate in the solution. This is acetone peroxide. Filter the solution through a coffee filter to collect the precipitate. Throw away the filtrate (liquid left after filtering out the solid). Add the acetone peroxide to a beaker containing 1L of distilled water and stir it with a plastic drinking straw for 5 minutes. Again, filter out the acetone peroxide and add it to a beaker containg 1L of 5% sodium bicarbonate solution and let it sit for 12 hours with occasional stirring. Filter out the acetone peroxide and add it to 500 ml of distilled water. lastly, filter out the acetone peroxide and let it dry. To the left is a picture of the solution 1 hour after adding all of the hydrochloric acid.

ALL of the above has been taken from my website WITHOUT my permission. REMOVE IT NOW. Wait, i'll do it for you. Most of it is copied word for word except a few lame instances where there has been some slight changes. You didn't even take the time to remove the parts where it says "to the left is a picture of whatever". Fucking sad.

kingspaz
June 7th, 2003, 07:05 PM
arthis, for an older member i would have expected better. such as inventing your OWN synth via chemistry and some practical quantified experiments other than taking other peoples methods without permission.

Arthis
June 8th, 2003, 03:40 AM
Oh I'm so sorry, really I am. In fact I wanted to ask your permission, I wanted to say that if any ripped info in here was to be removed then just ask, but I forgot to put it (got out of my mind).

The fact I was trying to make other more interesting parts, and I was too bored to write a synthesis, and yours is well known. Note I didn't try to 'steal' your method I mentionned in credits that I had.

So far I've made other parts, included schemes, etc... I found in a software my mother had, Acrobat 3, so even if it's not the latest stuff (version 6 is out), it still works.

I need to make a few experiments myself, about the dissolution in acetone/water, soon, maybe this afternoon (if my AP is ready, since I don't have some stored).

Again excuse me for taking your method, gonna write mine right now.

---------------------
OK this is done. I've just modified the method, since Alen doesn't want me to use it. The new pdf should a pretty good overview and not a lame stuff like you said.
I made all the calculations, they should be correct, if you notice any error, tell me, I'll modify it.

The dissolution experience is still to come.

The link to pfd:An AP beginner's manual (http://membres.lycos.fr/arthis00000/An%20AP%20beginner's%20manual.pdf).

There's no more credit, I don't think I've ripped any info excepted the H2O2 concentration/density graph, from www.h2o2.com. Any add, answer appreciated.

inFinie
June 8th, 2003, 12:44 PM
There are some typos, in fact one with many instances;)
cristal should be crystal

Arthis
June 8th, 2003, 01:06 PM
Oh right, I'll modify this. The fact is in French it is cristal, and I was tricked. I gonna modify this. I should install the word ortograph check btw, too.

My AP is drying in the sun now. I don't think I'll be able to make the dissolution experiment today. (maybe, who knows ?). Tomorrow for sure you'll have the results, and in acetone too.

Arthis
June 8th, 2003, 04:02 PM
I tested TCAP dissolution.

Results are not very precise, this is an idea.
I got:

* 0.4 gr TCAP in 700-800gr H20 @ 25oC, I stopped the experiment after having had 400mL of water, but compared to the quantity left non dissolved I think this is a good approximation.

* 15 gr TCAP in 60mL acetone @ 25oC. This is an approximation, a bit more could have been dissolved but it took way more time to dissolve, so that should be globally a reliable value.

We see that AP dissolves very well in acetone, not much in water, so the addition of acetone in your mix should be limited, even if you waste H2O2, rather than adding more acetone that will globally result in a loss of AP. I think 2-3 mL more than the stoechiometric ratios should be enough (still it will cause a more than 0.5-1 g loss).

frogfot
June 8th, 2003, 05:19 PM
What about adding lots of acetone, to increase reaction speed and then, when reaction is done add lots of water to precipitatetate AP.. how do solubility of AP vary in mix of acetone and water?
Oh, about a typo, your acetone on pic in pdf have double bondings.. :p

kingspaz
June 8th, 2003, 05:51 PM
also, for diluting concentrated H2SO4, you must add somthing to say 'always add the acid to the water never the other way around otherwise acid will spatter everywhere'.

also, have you thought how adding the acetone to the acid then adding the H2O2 would affect the reaction as opposed to adding the acetone to the H2O2 and then adding the acid or even adding the H2O2 to the acid and then adding the acetone? i think the last one would give best yields for no particular reason other than i have a hunch (not on my back).

blindreeper
June 8th, 2003, 11:09 PM
On the subject of AP. Once I have done some calculations (doing it myself even though the ammounts are out there) today or in the next week, if I can borrow a digital camera off my friend I'll be doing a controlled test changing only one variable - The Acid. I know this may have been done but I want to do it using the 3 most common inorganic acids availabe OTC. I'll be using 30% HCl, 98% H2SO4 (boiled battery acid) and 70% H3PO4 (rust remover). What do you guys think, is it worth while doing it or just wasting my time? The only real thing stopping me is that I only have 2 250ml beakers and if I use a glass jar it may have an effect on the results.

Also I have heard that sulfuric acid is stronger than hydrochloric and so on and so forth. But does anyone out there know how to have the same "strength" of acid. Eg: 1M of sulfuric acid is equal in strength to 5M of phosphoric acid. Or somthing like that. I think it has some thing to do with the ammount of H+ ions in the acid. If any of you know what I'm on about and can calculate the equivenceys (sp?) it would be helpful as I'll do that in my experiment, as it would be like have 30ml of H2SO4 in one beaker and then having 1ml in another and saying they are the same as they are the same strength.

EDIT: Another source of H2O2 in Australia is a product called "Oxyplus" which is sold in hydroponic shops. I have scanned the lable for those who want to know what to look for.

http://www.geocities.com/blindreeper_chemistry/oxypluslable.html

Arthis
June 9th, 2003, 05:15 AM
I've modified the schemes of acetone, a stupid error it was, really.

Adding the acid to h2o2 then the acetone is not the best way depending on the acid you use. I've read that H2SO4 + H2O2 -> H2SO5 + H2O,
though there should be no problem with HCl.
Last, I presented acetone+acid, then h2o2 to change a bit, for people to be aware you can do about as you want, to keep the reaction the coolest possible. I personnally quasi never use this method, but one do as he wants. Maybe I'll say a word about that.

I'm not sure filming is necessary. Instead of beakers use jam pots (empty ;)). You'll tell me if my calculations are correct, there may be some errors (I'm far from reaching a decent yield compared to theory...)

80r15
June 10th, 2003, 12:28 PM
Originally posted by ALENGOSVIG1
ALL of the above has been taken from my website WITHOUT my permission. REMOVE IT NOW. Wait, i'll do it for you. Most of it is copied word for word except a few lame instances where there has been some slight changes. You didn't even take the time to remove the parts where it says "to the left is a picture of whatever". Fucking sad.

I hate it when people plagerize from my website too. Although, maybe he was just using it to enlighten us(on acetone peroxide, which everyone has synthesized, and a great synthesis is at roguesci.org/megalomania). But if he meant to do that, why didn't he just leave a link?? Hmmmm Interesting...

kingspaz
June 10th, 2003, 12:57 PM
80r15, look up the page. its already been dealt with. no need to bring trouble back to the surface.

80r15
June 10th, 2003, 01:36 PM
Sorry. And KingSpaz, is there any way I can change this gay screen-name without re-registering???

Arthis
June 11th, 2003, 07:23 AM
In order to forget lame posts ? Maybe you should just try to be an interesting member and post interesting things about explosives and weapons.

Anyway, there have been not many appreciations about my guide, do you think it's correct ? Would I need to add anything ? How to make it accessible by newbies if they want it ?

kingspaz
June 11th, 2003, 05:09 PM
80r15, you must re-register to lose the gay name.

Arthis, try adding a reaction mechanism backed with the chemistry behind each step. and also about the differences in reaction conditions making each AP batch slightly different. thats why some is more sensative than others - variations in the trimer:dimer ratio.

Anthony
June 14th, 2003, 06:20 PM
blindreeper, using a jam jar for one reaction shouldn't make any difference, unless you can't remove all the product from the jam jar because of its shape. In that case rinse all reaction vessels out well.

Or do all the reactions in jam jars.

It would be best to do at least two reactions with each acid type and take an average score.

Probably best to use a equi-molar amounts of acid for each reaction, so you'll have different amounts of each acid.

blindreeper
June 15th, 2003, 02:45 AM
Ok thanks Anthony I'll do equimolar amounts. This is the Calculations I have done and was wondering if I made any mistakes:

--------------------------------------------------------------------------------------------------------------

STIOCHEMISTRY - ACETONE PEROXIDE (TRIMER)

Reaction

2 H2O2 + 3 C3H6O + Acid catalyst ---> C9H18O6 + H2O + H2

Reactants

Hydrogen peroxide - H2O2 - Molar weight = 34.0146 x2 = 68.0292
Acetone - C2H6O - Molar weight = 58.0798 x3 = 174.2394

Products

Acetone peroxide (trimer) - C9H18O6 = 222.1
Water - H2O - Molar weight = 18
Hydrogen - H2 - Molar weight = 2

Density of 100% H2O2 = 1.46g/ml
68.0292 / 1.46 = 46.58ml of 100% H2O2
25% H2O2 = 46.58 x 4
= 186.36ml of 25% H2O2

Density of acetone = 0.789g/ml
174.2394 / 0.789 = 220.8357 of acetone


Theoretical Yeild

186 ml of 25% H2O2
220 ml of acetone

in the presence of acid will yeild 222g of trimetric acetone peroxide.

--------------------------------------------------------------------------------------------------------------


I am new to working this stuff ouyt so can you guys please point out the stuff thats wrong. I'm not too sure I did the densities right...

Arthis
June 15th, 2003, 05:15 AM
Nope. There's no release of hydrogen in the reaction. For the trimeric reaction, the equation should be
3 H2O2 + 3 C3H6O --> C9H18O6 + 3 H2O

blindreeper
June 15th, 2003, 08:05 AM
Well other than me getting the raction wrong :rolleyes: did I do the densities and other stuff correct?

Arthis
June 15th, 2003, 12:36 PM
Take the pdf I made for the densities. I noticed that while using Windows' calculator I fucked up the calculation, because of the scientific/standard calculation mode. I should update the pdf to modify these.

You need to recalculate the weights, as you have them function of 2 H2O only. Rest seems to be ok.

vulture
June 15th, 2003, 02:57 PM
The way you calculated your amount of H2O2 is only correct if you start from 100% H2O2. Otherwise, dilution will cause density changes which are not predictable, just consult a density table for you concentration of peroxide.

blindreeper
June 16th, 2003, 03:15 AM
I thought I'd use 100% to start with as there is an assumed 100% in the reaction scheme. So how would I go about altering the density of H2O2. Would finding the density of 25% H2O2 (1.1g/mL) and finding that then x it by 4 as 25% is a quater of 100%?

Nevermore
June 17th, 2003, 04:39 PM
Some days ago i tried a possible way of storing Ap. I took around 5 grams of dry Ap and dissolved in room temp acetone, stil till completely dissolved.
The solution appeared clear after the complete dissolution of Ap, then i stored the solution in fridge for a week, a very small precipitated appeared when the acetone got cold, but was very little.
After a week i decided the experiment was over, so i fastly poured all the acetone into a large becker of icy cold water, immediately the solution turned white and precipitate appeared.
After filtration i measure the Ap, it was barely 2/3 of the one that was dissolved the week before, also the cristal where somewhat bigger.
I assume this way of storing ap could be used at price of great loss of Ap and bigger cristals..
Definitely not worth considering that is possible to make Ap right before it is needed.
I assume is not possible to detonate the Ap while dissolved in Acetone due to the large quantity of acetone needed to completely dissolve 3g Ap (200-250ml).

ALENGOSVIG1
June 17th, 2003, 06:04 PM
Dissolving AP in acetone has been discussed before. If you can only get 3g of AP to dissolve in 200+ ml of acetone, something is seriously wrong. :eek:

I suspect you lost most of you product when you attempted to precipitate the AP. If you dissolved 3g in 200+ ml of acetone you'd have to pour it into ALOT of water to dilute the acetone enough to crash out the crystals, as Ap is very soluble in acetone and even a weak water/acetone solution should dissolve quite a bit of AP. Still, you wont get it all back, becuase as Athris' experement has shown, AP is soluble in water.

Sonny Jim
June 17th, 2003, 06:09 PM
Why not just leave the acetone/AP solution in a shallow dish and allow the acetone to evaporate off, leaving the AP behind. That seems easier than cooling the acetone to precipitate out AP crystals, and should leave you with a better percentage recovery rate for the AP.

ALENGOSVIG1
June 17th, 2003, 06:14 PM
Becuase then you'd be left with big, flakey crystals, which would probably stick to whatever they're drying on. Meaning you migh have to scrape the crystals off the dish.

Scraping large, flakey crystals of AP off of anything isn't my idea of a good time. :)

Sonny Jim
June 18th, 2003, 08:11 PM
You could remove the crystals before all of the acetone had evaporated, so most of the AP had precipitated out but was still damp due to the remaining acetone. The damp AP could then be placed in safer drying conditions. This works quite well, but you will be able to recover a better amount of AP if your acetone/AP solution is saturated or near to it.

fayll
June 18th, 2003, 10:25 PM
quote:
______________________________

My AP is drying in the sun now
______________________________


Arthis, if you want a long life, you should be to avoid doing dry AP under the sunlight ;) .
Use precaution when you write your pdf file about AP guide, because newbies don't know all risk when they making AP for the first time. Last month in France, there is a teenager who had serious damage with AP. Bonn's and one of his friends too. AP is very unstable under the UV radiation.


_______________________________

blindreeper
June 19th, 2003, 04:09 AM
fayll, not meaning to be harsh or disrepectful but I think Arthis knows what he is doing and telling him about if he wants a long life is probably not good seeing as he been here since nearly the begining.

fayll
June 19th, 2003, 06:44 AM
Ok, sorry, but i written that for any beginner who haven't sufficiently knowledge for making AP safely and who may read the thread.


_________________________

vulture
June 19th, 2003, 07:35 AM
I thought I'd use 100% to start with as there is an assumed 100% in the reaction scheme. So how would I go about altering the density of H2O2. Would finding the density of 25% H2O2 (1.1g/mL) and finding that then x it by 4 as 25% is a quater of 100%?


I don't know what the problem is all you people are having with calculating amounts from densities, all it takes is some common sence.

For example, say you have a 25% H2O2 solution. This solution contains 25% H2O2 by weight, so volume calculation is NOT accurate.

So you have calculated how many moles you need and from there how many grams.

Now, assume you need 10g of H2O2. Since your solution is 25% you'll need 10 + (10/25)*75 = 40g of your H2O2 solution. You know it has a density of 1.1g/ml, so 40/1.1 = 36,36ml of your H2O2 solution.

Simple as that.

blindreeper
June 19th, 2003, 07:51 AM
Ok thanks for that vulture, I mean we all have to learn sometime.

Arthis
June 22nd, 2003, 10:44 AM
For H2O2 density, take my PDF, or go on h2o2.com and you'll get the density function of the concentration.

I let my AP dry in the sun, actually this is not very dangerous as there was only 30 g. Once is enough to change one's mind, but having never had any problems with AP, I think I will making the AP dry in the sun. Not in the sun for long btw, when it's quasi dry I remove it. It's when dry that the risks are the most important.

inFinie
June 30th, 2003, 12:06 PM
synthetise : synthesize
absord : absorb
personnal : personal
monthes : months

And i think instead of h.p you should say H2O2 because symbols are here to abbreviate:D
And catalysts should be written on the reaction-arrow

knowledgehungry
June 30th, 2003, 01:32 PM
No one likes a smart ass... especially one who is new... I'm sure you meant the best but it sounds like your being one. Also its not possible to write the catalysts below the arrows with this BB.

inFinie
June 30th, 2003, 01:56 PM
I mean catalysts blabla for the PDF and i'm trying to be helpful

EDIT: Am i doing something wrong?:confused:

kingspaz
June 30th, 2003, 02:10 PM
inFinie, you worded your post in such a fashion that it sounded like you were being a smart ass. it sounds like you're being overly picky.

whether you meant to sound like a smart ass or not that isn't the issue. try and word your posts more carefully in future.

Anthony
June 30th, 2003, 02:32 PM
synthesize = synthesise

:)

knowledgehungry
June 30th, 2003, 02:34 PM
Ahh smart ass mods whatever shall we do *runs in terror*:eek:

Halo
July 1st, 2003, 01:24 AM
I have seen sooo many diferent VoD's for Ap that I am just getting confused now. does anyone really know for sure what the VoD is? And if so, how do you know? How do they test new explosives to find the VoD for it?
Thank you

Halo
July 1st, 2003, 01:49 AM
sorry about this but i have another borring question for all you experts.
What is the storge life of Ap if kept in distilled water in a glass jar?
Also, what is the reaction (if any) with brass. I want to make detonators using spent 270win casings.
Thx again-halo

Arthis
July 1st, 2003, 06:20 AM
You should edit your posts instead of posting twice in a such short time interval.

I use 'h.p.' because when you always use the symbol H2O2 it's getting boring to read. But no real importance.

Normally your AP can be stored for long in water, I don't know exactly. You know I store it in an open container... No problems yet. (i just lose a little product, and it makes larger cristals --> no long term storage for me). In water, if you keep it away from light, as H2O2 it should not decompose a lot. The main problem you could get in my mind is a lost of product. You see.

If your AP is well washed, with no acid traces, there won't be any important reaction with copper.
I guess though, that you may get
AP + 3 Cu --> 3 CuO + 3 acetone
with the peroxyde decomposition. But this would be a very slow reaction.
Anyway I advise you to make small quantities at beginning, before trying to make several hundred grams. And use your detonator readily after confectionning them.

Halo
July 1st, 2003, 10:11 AM
Thank you for your info. It has helped. Im going to make a very small amount my first time.(use about 75ml of 3% hp)
sorry about not editing my posts. Im new here and havent yet learned how to do everything.
Im using 3% hp. obviously Ill have less Ap but will it be weaker?
I cant just stick a metal thermometer in the solution so how do I check the temp? I will be keeping it in a very cold ice/salt bath for about 4 hours during/after mixing chems. is this long enough?
and finaly, do I have to keep the Ap cold while in storage? I happy about storing a film canister amount of Ap in my bedroom in a glass jar. thats like a small claymore mine! I want to keep it outside under a tree or in a lil wooden box I have made for it.

knowledgehungry
July 1st, 2003, 01:24 PM
I believe the detonation velocity for TATP is around 5000meters per second, however you never get pure TATP so it is normally somewhat lower.

Anthony
July 1st, 2003, 03:22 PM
Don't use metals, as you will get side reactions and contaminents!

A glass thermometer is commonly available and will do for both temperature checks and stiring.

AP doesn't need to be kept cold in storage, although it will reduce sensitivity a bit and lower the rate at which the AP volitises.

Halo
July 1st, 2003, 04:47 PM
ok thanks for the info. I didnt have a stiring rod so i just stole a glass thermometer from my neihbors porch(hes on vacation)
what kind of case should i use for my detonators? (small glass ones would look so kool) :)

Arthis
July 1st, 2003, 05:22 PM
Pure AP is pure AP, and if you make it with 3% hp will not change anything. Once washed you'll get the same product than if made with 30%.

If it's your first time, use it instead of storing it, it's so great the first time, when you're not blased of it yet. ;)

When neutralized, AP can be used in any casing, as long as you don't store it. Empty shells are often used. Glass is ok, though the confinment will be lower, and it's normally harder to get, more expensive. You have the choice.

yt2095
July 28th, 2003, 10:46 AM
this may or maynot be usefull to someone.

in the persuit of alternative peroxides I`de read MANY times about Ether (di-Ethyl ether) making some rather nasty peroxides if left standing or exposed to UV light. as of yet I`ve not managed to manufacture any :(
while "fucking about" this morning I found that ether will infact dissolve quite happily in acetone :)
SO... thought I, lets add a little 30% H2O2 and see what happens.
it splits again like oil on water :(
now I have to wait until it evaporates and try salvage something usefull from it (probably more AP :( )
I figure since we learn just as much from our mistakes as sucesses that it would be worthy to post this.

I`ve tried in the past the UV method, still nothing? and ether won`t work as a cheap solvent for AP or HMTD either thus saving on acetone :(

Life`s a Bitch!

can`t wait to see if my Hexamine Borate crystalises though, will it burn green or won`t it????

knowledgehungry
July 28th, 2003, 11:08 AM
All you have to do to manufacture some di-ethyl ether peroxide is leave it in the sun for a week or so, then distill the di-ethyl ether off, or maybe just let it evaporate off, but DONT DO IT. Not very powerfull IIRC and extremely sensitive. No use for it save perhaps as a touch sensitive explosive.

Evan007
August 13th, 2003, 04:43 AM
I have 400mls of 6% H.P. and 750mls of Acetone, no acids except for citric acid, the crystals that come in little containers like salt and pepper. How much citric acid will i (fictionally) use to how much acetone and peroxide? i have no real way of having this all cooled ( its winter here and the nights are around 5 degrees) other than the winter ambiantair temp how much of a problem will this be ( will it make dimer instead of trimer ?) ?

very sorry but this is my first go at AP

DBSP
August 13th, 2003, 05:03 AM
Haven't you got any ice?? can't be to hard to get.

Citric acid will as I remember it not work, your choise of acid is HCl, run a few internet searches and you must be able to find some. Wherever you live, try pool accesory stores or hardware stores. Use the search egine (http://www.roguesci.org/theforum/search.php?s=) and your questions will be answerd as AP has been covered in all possible aspects by now.

And at last, use 6 times as much acetone as pure H2O2 and about 10% acid (10% of total ammount of reactants that is)

Arthis
August 13th, 2003, 05:27 AM
I can't find the info with a search, but I remember some tests had been done about using a low acid as citric acid in TCAP production, and I think it worked, though a little slower. I'll look for some information.

Evan007, I made a pdf for beginners, like you, and there's a table in, you have the ratios to use with 6% H2O2. I suggest you take a look.

fasa
August 13th, 2003, 09:58 AM
I don't really know if this will work, its just a theory... I'm really not experienced with this enough to know for sure...

Would it be possible to add AN while making AP to keep the reaction cool?
I'm pretty sure it will have some effects on the AP, but I have no idea which...

kingspaz
August 13th, 2003, 10:50 AM
it'll have no effect on the AP but it will dissolve and cool the solution as you said. an alternative to an ice bath i suppose.

tri-x
August 13th, 2003, 02:39 PM
Earlier in this thread ...

Originally posted by Arthis

You should try to get the trimer form, as it’s also more powerful, and for that you need to keep the reaction the coolest possible.You may have noticed that the acid is not present in the equation: it only acts as a catalyst.


Acid used

]The acid acts as a catalyst and about any acid can be used in AP synthesis. Citric acid and sulfuric acid are also commonly used but some differences can be noted, and must be taken into account.

Sulfuric acid: adding it will cause immediately a local overheating and ebullition. You must add it drop-by-drop. A good solution to avoid a temperature elevation is to dilute your acid and let it cool (e.g. from 95+ % to 30%).
Hydrochloric acid: easy to get, it may be the best suited acid in this synthesis, regarding to its low cost. It is safer too, as pouring the whole acid at once in the mix will not cause (even local) ebullition or overheating; however, the global temp of the mix will rise thus favoring the formationof the dimer, or even producing tear gas. Don’t forget that it’s easier to keep the reaction cool than cooling it down once the temperature has raised.

Citric acid: this is not a strong acid, but it works well too. The main interest, excepted the ease in keeping the reaction cool, it that it’s way easier to wash the AP and make it neutral, compared with the use of strong acids.

kingspaz
August 13th, 2003, 04:38 PM
whats your point tri-x?

about my post above. i just realised that its not the best idea because with stronger acids you'll end up with a solution of HNO3 which could react adversly with AP.

knowledgehungry
August 13th, 2003, 06:12 PM
HNO3 makes AP go boom;) . In my very beginning days I tried to nitrate AP with rather loud results:D. I'm not sure how much of a problem NH4NO3 and Citric or HCL would be, as their equilibrium favors HCl and citric rather than HNO3, but still not a good idea to be adding any more impurities to an already sensitive and impure explosive.

Blackhawk
August 13th, 2003, 06:37 PM
I didn't want to start a new thread but I am planing on an AP batch soon and I was going to convert it to putty to lessen the evapouration and stabalise it (as much as is possible with AP) but I am a little concerned about kneading AP crystals in with NC, are there any particular precautions I should take or would the acetone in the NC laquer desensetise/disolve the AP while you are mixing.

knowledgehungry
August 13th, 2003, 06:52 PM
Just dont knead it with a hammer:p. It is fairly safe to knead as long as you dont have big crystals and its just made.

Blackhawk
August 14th, 2003, 04:18 AM
Ok thanksfor that, I just didn't want to loose some fingers (who does) and there isn't much said on the net about the sensetivity during preparation.

Evan007
August 14th, 2003, 06:46 AM
OK last night i dreamed that i mixed up 150mls of 6%HP and 50mls Acetone added some citric and let be for 20 hours. no crystals of any kind. added more citric acid and is waiting for results

scarletmanuka
August 14th, 2003, 07:27 AM
I made my first batch of AP last weak, and since then I have made over a kilo of it. I can't get enough of it. I use 50%h2o2 and 100% acetone with 30%HCl. The first batch I made, I filled the beaker three quarters of the way up with reactants, and had crystals pouring out of the beaker into the icebath within half an hour. However, using the same conc. h2o2 and acetone with citric or acetic, I was unable to produce any AP at all, even after 24 hours. I used about 30ml h2o2 and 50ml acetone with up to six teaspoons citric (I started of with two). I also used the same proportions and added thirty ml vinegar, and neither gave any yield. However the solution did turn cloudy un addition of acid (some AP formed?).
PS This morning while rushing to get to school, i added the HCl before the solution had cooled down enough, and got a runaway reaction. The beaker started boiling over and HCl gas was emmited (painful on eyes) it was a disaster, and the final yeild was not as good as expected.

DBSP
August 14th, 2003, 07:56 AM
You made your first batch of AP a weak ago and since then you've made over a kg of it. If I where you I'd definately slow things down a bit, AP is simple but dangerous. You shouldn't make any greater ammounts untill you've got to know it and trust me, you don't get to know AP from dealing with it for only a weak. Lets just all hope you carefully neutralize it and keep the reaction below 10* C, which isn't very easy with the reactants you are using.

Take my advice and slow things down right now before something happens!!!

Evan007
August 14th, 2003, 09:10 AM
I am officially with Scarletmanuka - CITRIC ACID DOESNT WORK ! quite frustrating considering the waste of time, money chemicals etc being 15 makes it hard to go out and buy the required chemicals to do this sorta stuff without parents knowing.......man i have some messed up dreams :)

Arthis
August 18th, 2003, 11:04 AM
I'll do experiments again, but I'll suppress citric acid from the list for the moment.

btw, does anyone know how to edit a pdf ? The fact is I formatted my computer last week and forgot to save the sources, so I end up with only the pdf, on the website. Anyway I could modify it (and keep sources for further modifications) ?

thanks

Desmikes
August 18th, 2003, 11:56 AM
Yeah a kilo of AP is a little much, I leaarned about AP from some "magic tricks site" and I had myself some "magic" after lighting a pile ~3cm in diameter with a match and not being able to hear for the rest of the day..! Getting down to business
A while back there was a thread discussing various aspects of AP's sensitivity, and as I remember someone tried to initiate it with a spark and found it extremely difficult, well i've had the same results up untill I crushed my AP down to tiny bits (it doesn't take much pressure don't worry) and then was able to set it off with an electric spark. What's even better is that I kept on reducing the power of a spark up until I found out that a simple, tiny spark-maker thing from regular electric lighters is plenty to set it off when it is in this form. I thought of some possible applications such as impact ignition/landmine etc. My AP was prepared safely i.e. in a temperature controlled enviroment, washed throughtly and treated with baking soda so it should be relatiely stable.
So there is a possibility of a static ignition afterall...
Another strange property of AP is that unlike most white things it doesn't stick out in black light, it's just black.

scarletmanuka
August 19th, 2003, 05:26 AM
On the subject of ways to ignite AP, I had some 0.2 grams of caked AP "pebbles" and was looking at ways of igniting them, and thought that it was getting a bit boring lighting them with a lighter on the end of a knife (nice fireball, but it doesn't det). So I tried heating up a long peice of wire, and then touched it to the pebble, rather amusing except when everyone is sleeping.
EDIT: the wire was not glowing
Another idea I had to get tiny mounts to det, is to put a pile of AP about the size of a apple seed (to small to weigh) onto a piece of Alfoil, and heat from underneath with a bunsen burner. It willd et and drill aperfect hole through at least four pieces of Alfoil provided they are not loose.
PS You are all right; One kilo of AP is way to much, but at about $15 Australian per kilo, it is hard to slow down. I needed to dump about half a kilo down the drain, because i felt unsafe about soring it in the shed.

kingspaz
August 19th, 2003, 12:48 PM
half a kilo down the drain?
what the fucks wrong with you? thats the most fucking stupid thing i've heard for a LONG time!
for one, you make way too much AP to be even resonably safe.
two, you dump half a kilo of it down a drain. why the hell do you think AP mames so many people? its because they haven't a FUCKING CLUE what they are doing.

don't think you're clever because you can make AP. as you know, babies can make it. the clever bit is doing it safely. no please, for your sake and ours stop making explosives of any sort until you have atleast some idea what you are doing.

Anthony
August 19th, 2003, 03:11 PM
I agree. Your drain is now likely to be an extreme explosion hazard - AP is not water soluble.

The reason the AP you poked with a hot wire detonated, would be that the deflagerating AP the wire touched would have been confined by both the wire and the AP mass, thus allowing a deflageration to detonation transition.

T_Pyro
August 19th, 2003, 04:31 PM
From my initial experiments with AP, I found it pretty unstable when placed in heaps/mounds, or even when confined in closed places (a fusion tube, for example). Through experimentation, I came across a few ways of making ap slightly safer. Here are a few methods of doing so:

1. AP strips: AP in mounds or heaps tends to be much more sensitive, and quite unsafe, to say the least. To make matters worse, trying to remove ap crystals from dry surfaces tends to lead to er, "unpleasant" results. Therefore, just as the ap was almost dry, I poured the ap and remaining acetone "slurry" on double-layered strips of tissue paper, and left them to dry completely. This prevented the formation of any dangerously large crystals or heaps. The ap strips so formed could then be comaratively safely ignited.

2. My first few casings for ap were fashioned out of fusion tubes (the chem lab seems to have an unlimited supply of them ;-) ). Though readily available, they had one major problem, especially when using an AP + Ammonium Nitrate mixture: shrapnel formation. Thus, to limit the formation of shrapnel, I reinforced the tubes with about 4-5 layers of insulating tape. The results were pretty good: there was a definite explosion, but fewer shrapnel pieces... The glass pieces had a tendency to stick together on the tape!

3. Although I've never tried this one, but it's still a suggestion to those who feel the need to store ap. AP volatizes pretty fast at room temperatures, leading to the formation of large, dangerous crystals around the mouth of the container. Why not cover the AP crystals in the container with a layer of water, to prevent the ap from subliming? The moisture will also keep the compound cooler.

Arthis
August 19th, 2003, 04:49 PM
And this transition from deflagration to detonation can occur if you use much explosive, depending on the critical mass of the explosive.

That's why it's not recommended to handle large AP quantities. 1 kg of AP that self ignite will achieve detonation. Don't even hope to be only burnt. You could thank God if you survived.

It's fun to handle large quantities, and I like it too. But you need a little experience before.

Storing AP has been previously discussed, but AP is not soluble in water, and does not sink, therefore you can't make a layer of water over the AP.
But storing the jar upside down will do the trick.

T_Pyro
August 19th, 2003, 05:02 PM
Um... 1 kg?!? That much AP, if strategically placed, would be enough to bring down an entire building!

------------------------------
No Shit Sherlock! :rolleyes: - zaibatsu

kingspaz
August 19th, 2003, 06:33 PM
T_pyro, stop wasting forum space with garbage posts.

Efraim_barkbit
August 19th, 2003, 07:38 PM
I wanted to try making a fireball with some AP a night last week, I put a little more than ½ a teaspoon in a plastick coke bottle cap, with a couple of cm of fuse inserted through a hole in the side.
But instead of the fireball that I expected, it detonated without even the slightest flash (at least I didn´t notice any..) Probably the AP that ignited by the fuse got enough confinement by the AP on top of it, and the walls of the cap, to make d-d..
I think this is important to remember for people who stores their AP in small amounts in open containers, that just because it is only a few grams, and stored "unconfined",it still can make the d-d transition.
Of course, if the same amount AP is stored on for example a plate or in other "low walled" and wide containers, the risk of the AP making the d-d transition decreases.

T-pyro, what do you mean by that you found it extremely unstable? spontaneous iginition? more sensitive to shock/friction?
If your AP is mixed with "acetone slurry", does that means that you take it directly from the reaction jar to dry it without washing it? in that case you´d have more like a "acid, acetone and/or hydrogen peroxide slurry".(if you havent used calculated and exact amounts of acetone and HP, and let it sit until all crystals precipitated(sp?) out, in wich case you´d only have a "acid slurry").
From what I´ve read, unwashed AP is supposed to be a lot more sensitive, so thats maybee your problem (I once compared a unwashed and a washed sample from the same batch by doing the "put AP on a anvil-hit with hammer" test, but I noticed no difference in shock sensitivity. Of course, this may vary between batches)


Ohh, and IMO, it would have to be a small and shitty building if one kg of AP would be sufficient in taking it down. but I have no experience in building demolitions, so I might be wrong..
That brings a question to my mind: has anyone here tried to/succeded in taking down some kind of building with explosives?

T_Pyro
August 20th, 2003, 03:00 AM
kingspaz, I'm sorry if you didn't like my post, but my intention was not to "waste forum space with garbage posts", but to just share some ways of making ap safer, so that the rest of us can live longer.

Anyway, Efraim_barkbit, yes, I meant that the ap was more prone to shocks and higher temperatures- once I had a small batch of it go off when the fuse hadn't even completely burned out! Luckily, I was some distance away from it by then...
Regarding the "slurry" I spoke of, I had taken calculated amounts of peroxide (6% w/v) and acetone, with 40 ml of o.1 M HCl. If I'm just makin fine ap crystals, I wash it with distilled water, followed by washing soda. However, the instability of the pure ap I get always seems to be more or less the same whether or not it is washed. Dunno why... I keep the reaction mixture refrigerated during the precipitation process , so I don't think much of the dimer is formed.

In the above process, I think the peroxide and acetone reacted completely, but I had no way of making sure, though... Although the HCl, as many say, is just a catalyst, but I believe it could be more than just that. I've been working on some possible reaction mechanisms for the formation of ap, which I'll post if they're plausible enough. The H+ ions from the acid seem to be "used up" by the reaction, which could be detected by the measurement of Ph before and after the completion of the reaction.

T_Pyro
August 20th, 2003, 03:24 AM
Using the ap strips I desrcibed before, I managed to create some flame "tongues" as the ap deflagrated on the tissue paper base. There wasn't any proper "boom", but there were upto 5cm long flame tongues, and a loud "poof"! I haven't tried it yet, but the ap strips, if rolled into a tube and then ignited, could produce a "flame tube". A fireball might be more difficult, though... -Ways to experiment on my next batch of ap!

knowledgehungry
August 20th, 2003, 11:00 AM
I would use a fuse for all your tests, in case it does DDT. I have lit about .02 grams of AP with a match, it DDT and i felt like someone hit my fingers with a ruler. Always be prepared that AP WILL DETONATE AT THE MOST INOPPURTUNE TIME. Prepare for the worst and you keep most of your fingers.

T_Pyro
August 20th, 2003, 12:00 PM
Well, yeah, a fuse WOULD be a good idea. DDT takes place more easily with pure AP than with the ap strips, and the fuse would help in the controlled deflagration of the same.

Desmikes
August 20th, 2003, 02:44 PM
the safest way to store your AP is by letting it dry and remain on your piece of handkerchief or cardboard in some dark cool place. this way you never have to shit your pants when you open up the container and it doesn't recrystalize; after weeks of keeping my AP this way I haven't noticed any lowered sensitivity as far as hammering goes. Yes it does evaporate but if you care so much about that then use it up quicker ;)
T-pyro that idea of yours about rolling up AP in napkins shouldn't be followed up upon, first of all it is too likely to det 2nd what's the point? 5cm flames - please.
And for all of those who are sending your AP down the drain, next time just sprinkle it all out evenly on the concrete and run a line of AP to it and set it all off at once, you don't have to go out into the wilderness to do that.

Anthony
August 20th, 2003, 03:02 PM
Why would soaking the AP/acetone solution in tissue paper elminate the formation of large crystals? Surely the obvious thing is not to use a solvent that AP is soluble in? Then there will be no crystalisation at all (after the intial formation in the reaction vessel).

BTW, don't make posts one after the other, use the edit feature to add the information to the first post.

DBSP
August 20th, 2003, 04:59 PM
I always store my AP on a piece of paper in the open on a shef that is hard to reach by accident. Any AP that sublimes will have about 70 cubic meters to recrystalize into so there are no problems with any vessels getting AP crystalized in the threads or at any other non-good location.

If you can store it in the open and just put it away safely in a locked closet or something similar so that noone can get to it.

kingspaz
August 20th, 2003, 08:57 PM
T_Pyro, i was refering to the utterly useless post by you directly above my post warning you.

T_Pyro
August 20th, 2003, 11:33 PM
Well, leaving the reaction mixture to dry in its own vessel (or any other vessel, for that matter), I invariably ended up with clumps of crystals sometimes upto 1.5 cm long. Using the tissue paper method prevents the crystals from getting too long and sticking out of the paper. It also prevents the piling up of the ap, which would have led to detonation in case of any accident. While the ap is crystalising from the reaction mixture, there is bound to be some amount of unreacted acetone, unless of course the acid and peroxide were in excess, in which case there would be formation of bubbles of oxygen everywhere. (not a good environment for explosive materials, I think, though tell me if I'm wrong...)

I've never tried this one before, so could some one advise on this: If ap is mixed with AN, and filled into a medicinal gelatin capsule, how hard, and from what height should it be thrown in order to detonate? Should I include some inert "packing" material (talcum powder, maybe) to lower the concentration of this powder?

What is the best way to transport about 2gm of ap? Will the method I mentioned earlier (using a water layer on top of the ap) be safe enough?

Nevermore
August 21st, 2003, 05:58 AM
well you can transport it wet, or under water, that should be safe enough, or you can dissolve it in acetone and transport like that..
you can also transport under ethanol for faster drying.
is up to you, altought is not safe to go around with primaries, i dun think there should be problems if you DUN bring on yourself.

Efraim_barkbit
August 21st, 2003, 07:32 AM
If you are transporting your AP to a blast site, then it wouldnt be practical to have to wait many hours for the AP to dry, would it? if transporting such small amounts as 2g, then you shouldnt be too worried.
for transporting larger amounts, wich you are not going to use immediatley, wet it a little bit so that all of it gets a little bit moist, then it should be fine.

You should put a small amount of your AP in a container, and then go and throw it around for a while, to get a idea about the senitivity. I have put AP in 5cm lengths of a plastic pen, but I couldn´t get it to detonate. (of course, always throw up and away from you, never straight down;) )
If jou want a impact detonated fire cracker, test putting AP between two coins, and throw on a hard surface. just watch out for the flying coins.
I doubt that you can manage to get that gelatine capsule with APAN to detonate by throwing it.

why not put your wet AP between the pages in a news paper to dry? then you´d have no clumps to worry about.
I didnt think about it before, but how can your AP be more unstable if you put it in a "heap" than if you put it in a "line"? it´s properties wont change just because the shape changes.

It´s up to you if you don´t want to wash your AP, But think about it, is it worth to take that extra chance just to save a couple of minutes?

knowledgehungry
August 21st, 2003, 09:30 AM
I think he meant that his AP makes the DDT easier in a heap, which is true because when AP is in a heap it adds self confinement.

Anthony
August 21st, 2003, 02:56 PM
"leaving the reaction mixture to dry in its own vessel"

Do you mean that you mix the reactants (H2O2, acetone, catalyst), allow the AP to precipitate, and then let the liquid evaporate leaving the AP?

Desmikes
August 21st, 2003, 10:23 PM
it is simply impossible to throw a gel capsule filled with APAN hard enough to make it detonate. Don't even bother trying to use AP alone with this method. I don't know about using coins either, first of all how are you gonna keep them together and collapse at the same time, how are you gonna throw them... not very reliable. However this one works wonders: you take a piece of wide sticky tape and run a line of AP that's about 10 cm long and 1.5 cm wide on it. then you fold the tape to make the ends meet i.e. to have a 10 cm strip of AP now imbedded in your tape. All you gotta do now is take this baby and wrap it around a big ass bolt nut. (the bigger the better). Fix it in place with yet another piece of tape. Done. SAFE and reliable no shrapnel (the nut doesn't really go anywhere b/c AP is all around it). They travel very far and WILL explode if it hits a building/paved road/tree/car not ground though.

Cyclonite
August 22nd, 2003, 03:44 AM
Does the AP around the nut explode or was the AP deflagrated. I was just thinking you could modify a lawn dart by drilling the tip and putting a pin of some sort through it then having it strike a metal plate with AP on it while having the ap in the main body of the hollowed out weight in the front. You could also weld, glue or epoxy a little disc on the pin and put a spring between the disc and the metal surface with the AP. That would serve as a saftey and make sure the pin has enough distace to strike the AP. It would make an interesting game of lawn darts.

Blackhawk
August 22nd, 2003, 04:51 AM
Yeah, you could gain extra points for not getting your legs full of shrapnel :D
I thought it would be fun to try AP putty moulded into tips of darts, it wouldn't matter if your opponant scored really well because you could blow their dart off the board, you'd waste a lot of boards though. I think it was EP on another forum that said you could make AP putty more sensetive by mixing in fine sand as you are making it.

Efraim_barkbit
August 22nd, 2003, 06:19 AM
Of course the coins will be taped together... , but I think your Idea is the better(cheaper too)
AP detonates when set off by shock, and if it wouldn´t, it will still make DDT because it´s confined.

What about making "balls" with AP putty and throw them?

Arthis
August 22nd, 2003, 03:51 PM
They wouldn't detonate every time, it's not very stable but not totally unstable. Moreover in the NC laque only the cristals at the surface may detonate the whole ball because the cristals inside are protected by the laque which is pretty strong; particularly as drying a ball would so much time to get off all the acetone in the middle that the ball would be really hard. It's confinment, but also protect the cristal from rubbing together.

T_Pyro
August 23rd, 2003, 02:14 PM
If you want to make sure that the AP projectile detonates on impact no matter how hard, or what it hits, why not use 1 or 2 crystals of NI3 to set it off? OK, I know NI3's straight from hell, but if you could Prepare the NI3 just before use (when you're gonna chuck it), there'd be nothing like it!! Just carry a small flask of liquor NH3 and a few Iodine beads. About half an hour before (using the ap), just mix the two real well, tape 3 layers of tissue paper on the ap projectile, and pour the mixture on the tissue paper. Leave to dry, and as soon as it's more or less dry, chuck it at anything you want to (just be careful!! ;) ). If you tape the tissue paper strategically, then the entire ap projectile will go off on inpact. I've noticed that when the NI3 is almost dry (the paper should be just moist), it is reasonably stable, yet goes off as expected on impact.

DBSP
August 23rd, 2003, 05:16 PM
T-Pyro, get that stupid fucking idea out of your head!! NI3 and AP is really asking for trouble.

I really think you should start using your brains, just a tip as I feel your stay here might be ending soon if you don't shape up. In other words no more NI3+AP or the alike.

knowledgehungry
August 23rd, 2003, 07:37 PM
I think the idea of NI3 anything is a horribly stupid idea, also im not so much worried about your presence on this forum staying as your presence on this earth staying if you continue treating explosives like novelty items. If you want |<3\/\/!_ impact firecrakers buy some snappers from your local toy store...

T_Pyro
August 24th, 2003, 12:46 AM
OK, I guess NI3 + AP was a bad idea, going by the reaction I got! Sorry.

Anybody tried mixing AP with any other primary explosives? Does it neccesarily make the mixture more unstable? I've got a few gms of AN, but require a primary mixture to detonate it... Any suggestions as to what primary explosive I could use for that? I don't have access to, nor can I make TNT.

knowledgehungry
August 24th, 2003, 01:18 AM
Mix some AP with AN then either detonate it with an AP cap or make the mixture flame sensitive, dont ask how to mix AP and AN or what ratios to use or what to set it off with, do a search for "APAN" and you will find everything you need. I am not going to answer anymore of your questions until you search first.

T_Pyro
August 24th, 2003, 04:36 AM
Thanks for the info, but I was talking about ways to modify the basic APAN mixture, in order to provide reliable detonation. I've used a 60% ap, 40% an mixture before, but I don't think it detonated properly. My casing was fashioned out of the Zn metal casing of a dry cell, reinforced with tin strips. The AN was towards the bottom of the casing, and the AP above it. The explosion didn't seem loud enough for a true APAN mixture. Another major problem with the APAN is that the AN is extremely deliquescent, so it tends to draw moisture, reducing the efficiency. To prevent this, I had dried the AN in a silica gel dessicator, and moistened it with acetone before filling it into the casing to prevent it from absorbing moisture, Could this have been the reason for the failure?

IPN
August 24th, 2003, 04:41 AM
The AN was towards the bottom of the casing, and the AP above it.

You have to mix the AP and AN well, in order for the APAN to work..:rolleyes:

PasstheDutch
September 12th, 2003, 06:27 PM
Arthis, thnx for the Starter guide, nice .PDF.
I'm planning to make some AP soon, but i've searched this forum, and wind up with very much variations in quantities and stuff. This is probably because of the very various locations op people who synth AP. Since i live in The Netherlands, is there anyone in Holland who can tell me which chems they use and where they buy it ?

Thnx in advance,

Pass thee Dutchie

Desmikes
September 13th, 2003, 06:02 PM
T_pyro man, if you are planning on making any more posts on this topic - DON'T! The more you write the more retarded you seem. If you were to read ANY posts on APAN you would know that nobody in their right mind would ever "dry the AN in a silica gel dessicator, mix it with acetone, put some AP on top" and call it APAN. If you are using 60%AP you don't have to give a fuck about AN being hydroscopic unless you are going to store it. You don't even have to have finely-ground up AN for a mixture like that.
As far as variations in methods of making AP go, that’s just a proof that you cannot mess it up. (it is usually due to people either using different conc. of components or trying to speed up the reaction)

T_Pyro
September 14th, 2003, 01:43 AM
PasstheDutch, sorry for the "retarded" post... I'd got mixed up with some schematics of "booster stages" that I'd been looking up. Coming back to the deliquecsent bit: All the articles I've read so far state that AN is "extremely hygroscopic", but none that I've read, state how to tackle this problem, or even if the absorbed moisture is going to interfere. Either way, no matter how the AN is used, I invariably end up getting a layer of water on top the next day- quite a bother.
I know this is getting kind of off-topic, but it's a reply to a previous post...

Cyclonite
September 14th, 2003, 09:19 AM
Layer of water huh? Might there have been some rain when you left it outside? You should think about things before you say them, its just good advice. How do you dry your shirts after a wash, put them in a low humidity high heat environment ie..drier. Before you throw AN in the drier I was just using it as an example of how to think things through and put your ideas together. Booster stage? Its not a rocket, think of it as an avalanche. You cant move a tremendous amount of snow just like that, throw a snowball that collects more snow (energy) and in turn collects even more to cause the avalanche. In general the higher the sensitivity the lower the power and the lower the sensitivity the higher the power

T_Pyro
September 14th, 2003, 01:40 PM
Yes, it DID rain, but I didn't leave the AN outside, so the rain couldn't have possibly collected. It's the weather: in the monsoons, there's no such thing as a "drier" environment... Only moist, moister (if there's any such word), and downright wet.
Thanks, I got my mistake about "boosters": feelin pretty stupid now, but hey, I'm learnin, that's what I'm here for! ;)

Cyclonite
September 15th, 2003, 07:33 AM
Drier environment=Oven

bobo
September 15th, 2003, 10:50 AM
Dutch: acetone can be found everywhere, try the apothecary. HCl used to be at the Gamma. I used sulfuric since I have it in large amounts but HCl is better. you use a base to neutralize, I advise soda from the supermarket though you can use anything.

There is a brand called Tendo that has acetone and H2O2 (3%) for apothecaries, and there are online sellers. Getting 30% peroxide is not hard at all though I have only acquired this through online store and perhaps you prefer anonimity.

If you want to have additional info just send me an email. (you'll find my email in my profile).

PasstheDutch
September 15th, 2003, 05:59 PM
Desmikes : Ok thnx, i'm buying the chems this week so when i know the concentrations i'll post them here (this IS an AP-beginners-thread right :)?) and then maybe somebody here can tell me wat kind of ratio's to use based on their experiences?

Bobo: thnx vriend, i sent u an e-mail..

- another question : whats a "safe amount of AP-yield" to start with? I was thinking of about 5-10gms (not a Kg like that crazy kid i've seen :D)
Any suggestions?

dutch..

DBSP
September 15th, 2003, 06:09 PM
The ratios are all over this place. Just run a search like everyone else. The answer is out there..

It's impossible to tell you how much reactant to use for a given ammount of AP to be formed unless we know the konc of you chems, Get back when you know the koncentrations and we'll try to help you then.

PasstheDutch
September 15th, 2003, 06:16 PM
I did run multiple searches and found many different ratio's that makes it a bit confusing.
But i'll get the conc.'s asap, so ima post them here.

thnx for the goodwill :)

nbk2000
September 15th, 2003, 07:18 PM
But i'll get the conc.'s asap, so ima post them here.

thnx for the goodwill

Bobo: thnx vriend, i sent u an e-mail..


Use proper grammer or get the fuck out of here. "U" is not a substitute for "You", nor "i" for "I", got it? :mad:

And leave that "dutch" crap out of the bottom of your posts!

Did you think that maybe the reasons for all the different ratios is because they all work? AP is ridiculously easy to make, and very tolerant of varying ratios.

PasstheDutch
September 15th, 2003, 07:28 PM
Ok, I get the message. I was just trying to prevent me from blowing my fingers or something else of, this being the beginners guide, excuse me for mistaking. I'm not some punk 12 year old, not trying to annoy anyone but just asking advise.

metafractal
September 23rd, 2003, 08:22 AM
Someone said something about making fireballs with AP.
A while back I played around with AP/napthalene.
The first thing that I tried was putting a layer of napthalene on top of a layer of AP. When lit, however, the deflagrating AP simply threw off the napthalene, not igniting it at all.
Then I tried mixing the two together in a 1:1 ratio.
Only some of the napthalene ignites, but gave noticably more body than a pure AP fireball.
Very unscientific, but good, cheap, easy fun.
A video of it can be found here (http://www.angelfire.lycos.com/alt2/pyro/index.html) (sorry, large file / bad quality.). The whowle mixture was ~10-20g.


EDIT: Apologies, link fixed.

DBSP
September 23rd, 2003, 09:40 AM
I'm afraid that the video is not avalible at that adress. The adress is linked to an .AVI but there is no file at the target location. Have a look at it and see if you can correct the problem.

Nevermore
September 23rd, 2003, 02:51 PM
Originally posted by bobo
Dutch: acetone can be found everywhere, try the apothecary. HCl used to be at the Gamma. I used sulfuric since I have it in large amounts but HCl is better. you use a base to neutralize, I advise soda from the supermarket though you can use anything.
I
Well you should be able to find acetone at any hardware store, better if has a paint department, since acetone is a good paint solvant, it is cheap and you usually find in metal can around one liter (at least here). HCL could be found in the muriatic acid for toilet cleaning, however will be around 10% hcl, no problem, just use more, it is usually sold in plastic bottles at supermarket or house dept, cheap too.
Sulfuric acid can be found at home depot as disgorgant and plumbing cleaner, rather concentrated, around 90-92%, and cheap too, however most of the time is in a jello form, or black in colour, works anyway...
About the H2O2 the best source is H2O2 for hair colour, you can find at 60vol=15% in big and cheap bottles, just give a look at hair distributors or big coifeeur reseller..

bobo
September 23rd, 2003, 04:30 PM
H2O2 is sold in 100l package (30% H2O2) at a hydroponics store here. It is sold by several online shops in the Netherlands. It amazes me why people keep going on about hair whitener. Is it really that hard in some countries? I will start a mail order company if that's the case;)

Nevermore
September 23rd, 2003, 06:24 PM
Originally posted by bobo
H2O2 is sold in 100l package (30% H2O2) at a hydroponics store here. It is sold by several online shops in the Netherlands. It amazes me why people keep going on about hair whitener.
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...

bobo
October 8th, 2003, 09:01 AM
Today I dreamed about blastting a cap with ~3g of partially wet pressed AP in it to test shrapnel damage to nearby objects. Especially, I compared damage with the AP cap with damage from firecrackers. This test is still inconclusive and I will also test HMDT and dried AP. (so far, a .5mm aluminum casing glued tight on the cap was blasted ca 2 cm into furniture foam matress. It was positioned horizontally over the matress, not in a hole.)

The detonation mechanism I wanted to try out was to put in a resistor and put it on 220V. This resistor was 2200 ohm so I expected it to heat up and go boom.

Instead, the fragment of the resistor still attached to my wire was cold to the touch immediately after. The detonation took place one second after I put the AC on but I don't trust the connector. So I reasoned it could have been a spark but more likely there was moisture in the cap a few days after pressing it. What do you think could have been the cause?

How much will moisture decrease the power of AP anyway (so if it was moisture I'd have to repeat this particular charge)?

Cyclonite
October 8th, 2003, 11:37 AM
Moisture will desensitize AP, it makes it harder to achieve a full true detonation. It may lessen the brisance of the AP but in a way that would be hard to notice.

Efraim_barkbit
October 8th, 2003, 08:33 PM
I Find AP to be much less powerful/sensitive when (if only slightly) wet. I havn´t had it do the deflageration-detonation transition once when not dry. Here are some experiences of mine with damp AP:

Damp AP in a pice of plastic pen casing (~0,5x50 mm) lit with fuse failed to burn completely with half of the AP left in the partially intact casing, and damp AP wrapped in AL foil (2-3 cm^3 AP) made a fireball and a weak poff. A very clear powerdecrease compared to the dry stuff...

Damp AP lit with a flame leaves wet, unburnt AP behind, wich often doesn´t catch fire even if it is toucheed by naked flame
(Unless the flame is kept long enough for the AP to melt and detonate(a couple of secs.). a pice max 2x1x1 mm left me with ringing ears for a couple of minutes, and blasted a 3-5mm hole through a 4-5 newspaperpages)

NBK mentioned in the "Danger AP" thread, that he had accidently set off a ounce of drying AP close enough so that the fireball burnt his eyebrowns and hair. think about what would have happened if that AP had been dry...
I wanted to make a fireball once, and put half to one teaspoon of it in a coke bottle cap, and a few cm of fuse. I didn´t even see a flash of light, (could have missed it due to the unexpected BANG..) and it was almost pitch black when I set it off.

A teaspoon of loose AP, I guess thats ~2g. And NBK (accidently)set of almost fifteen times as much without d-d transition...

This is of course only my personal observations and conclusions on the subject, other people might have noticed other behaviours, as AP is quite unpredictable


EDIT:

I start with low power hammerblows, and increase till I get detonation, that time, the AP became too dispersed due to repeated blows so I didn´t bother putting it back together for more tries, and it was also directly after washing, with only a couple of hours of drying in a coffefilter. however, the force of the last blows were quite a bit more than for the dry powder. that can also have been due to the hammer not hitting "right on".
I was tired when I wrote it, I realise that it doesn´t tell that from the text so I took it away, it was only some last thoughts added after the prewiew anyway...

Yes, the ~2g "unconfined" charge had in fact some confinement from the cap walls, but I still don´t think that would make that much of a difference compared to an ounce of the stuff. maybee it does, I don´t really have the experience with unconfined AP to tell.
The only other test I have done is if I recall correctly a test with a couple of teaspoons of damp AP in a shallow plastic container( 4x4 cm, 1cm walls) were the AP burnt with a nice, big fireball.
I´ll maybee try some next week with "real" unconfined AP, I have a filmcan left from the last batch, I might take it all or varying smaller amounts.

Damn, I have quite a big load of different things that I want to try out sometime, ranging from blasting machine construction to explosive projectiles and different types of improvised SC´s, with the propellants and higher brisancy explosives involved.
I have already tested a few LSC´s (with pressed AP), but on a small scale, nothing to hang in the christmas tree as we say in Sweden, but at least it looks promising.


Off topic: If I edit a post of mine, will the time left to edit reset, or does it still count from the posting of the original message?
Oh, Anthony,what do you mean by suspicious?

Anthony
October 9th, 2003, 03:05 PM
Your AP would have been partially confined by the sides of the coke bottle cap.

I get suspicious when people say they are unable to detonate AP with a hammer. Especially when relatively insensitive secondaries can be detonated with a hammer blow.

knowledgehungry
October 9th, 2003, 05:16 PM
I've noticed that many times my AP does not go off with the first hit, but thats because i hit it wrong, not straight on, when hit correctly it always goes off.

Sir Dudalot
October 9th, 2003, 09:41 PM
I don't see how people are having problems with making a fireball. I just set a gram or two, up to three, on a coffee filter or piece of paper then light the paper/filter. When the fire gets to the AP it goes poof! and makes a neat fireball.
The first time I hit AP with a hammer I didn't use ear protection, it was about .1g. Now I always use ear protection. Compared to nitroglycerin it seemed to take a slightly harder blow from a hammer. This could easily just be me though. The NG was dropped into a cotton ball first so it'd be easier to hit.

0EZ0
October 9th, 2003, 11:28 PM
I agree that reports of insensitivity with AP are just a little bit suspicious. A while ago in the below post I made, I wrote something about the varied results of impact tests.

http://www.roguesci.org/theforum/showthread.php?s=&postid=34686#post34686

It would be very hard to get consistent results from impact tests using a hammer and any variety of surfaces to place the sample on. Crystal size of the sample, plus temperature and many other factors also influence the results. There is no universal impact test apparatus/protocol that members to use. That would explain why we get people saying that they 'hammered all day' without having the test sample go off, whilst others say that they experienced quite the opposite and had a sample of the same material detonate from a 2cm drop of a hammer.

Nothing springs to minds about how the 'professionals' determine impact sensitivity. There would have to be a set system which they use. Just saying that something detonated from a 20cm drop of a 2kg weight still leaves alot of room for inconsistency. Such as the surface area of the end of the ram that comes into contact with the sample? On what surface was the sample placed on? What was the particle size of the test sample? So on and so forth.

After a bit of googling, there seems to be a few standard tests for impact sensitivity:

Impact Sensitivity Test Equipment by SMS (http://www.sms-ink.com/products_impact.html)
Google search for 'determining impact-sensitivity' (http://www.google.com.au/search?hl=en&ie=UTF-8&oe=UTF-8&q=determining+impact-sensitivity&meta=)

Anthony
October 10th, 2003, 03:00 PM
I'd imagine that there would be a recognised standard that these machines are built and used to. It would give all the specs you'd require to construct a machine.

It's something that I've considered doing at some point in the future.

McGyver
October 15th, 2003, 05:21 PM
Does AP have a tendency to stick to everything, beakers, stiring rods... Or is this due to it still being moist?

I noticed that if you squish down the AP, it will detonate with the slight drop of a hammer on an anvil.

Nevermore
October 15th, 2003, 06:35 PM
Well, wet AP tends to stick to glass rod and beckers, but you can wash it out easily with some water when you filter it. It will stick as long as is wet, when is dry is absolutely not sticky like normal table salt, to detonate requires to be hit by an hammer when dry, but the hit shouldn't be so light as most ppl think.
If yours is very sensitive i would suspect you got the di-form, since is what you mainly get when performing the reaction at high temps (i'd perform at 5C or less).

Hang-Man
October 15th, 2003, 06:35 PM
My AP is like wet powder; wash it off with more acetone.
I noticed that if you squish down the AP, it will detonate with the slight drop of a hammer on an anvil.
Really? How fun! DON'T DO IT AGAIN. Hitting explosives with hammers is K3WL, and dangerous..

Edit: damn people posting better replies than mine while I'm typing....Sorry if that came off hostile

Sir Dudalot
October 15th, 2003, 10:17 PM
I've always found hitting various explosives with hammers to be a good thing. It gives you an idea of how sensitive it is. Example: The AP I make takes an easier blow than the nitroglycerine that I made. Picric acid takes more than either. Just take the proper precautions, ear and eye protection. Also, don't use very much at all. That's when you run into problems.

After my AP is dry it doesn't stick to anything. It acts just like any other powder except you should be gentle with it.

McGyver
October 15th, 2003, 11:22 PM
Well maybe i exagarated how sensitive it was, but before I hit it I pressed it hard with the hammer to experiment before pressing it into the 9V cap. It wasnt really a slight drop of a hammer, and the hammer istelf probally weighs 5 pounds, i guess the only way to describe the hammer motion is picking it up halfway and droping it without exerting any force on it.

Whats the big deal with the hammer test? It deosnt caus any damage, exept maybe kill your ear drums.

blindreeper
October 16th, 2003, 02:53 AM
Hammer tests are fun! I jsut did my first one with AP yesterday with out earmuffs. It was a .5g pile and my left ear is still ringing ever so faintly. So my advise USE EARMUFFS! It makes a world of difference and saves you a world of hurt ;)

Nevermore
October 16th, 2003, 02:43 PM
Originally posted by McGyver
but before I hit it I pressed it hard with the hammer to experiment before pressing it into the 9V cap. It wasnt really a slight drop of a hammer, and the hammer istelf probally weighs 5 pounds,

i think really that is not need to deal with primaries in that way, we know they are already sensitive, and AP is not one of the tamest, since it is a little bitchy is no need to use hammer when working with it. I see many people like to take unnecessary risks, pressing AP is already a risk, but doing with an hammer is a little too much crazy, isn't it?
I found out that AP makes the ear ring quite much, much more than Ng.
I wonder why.

knowledgehungry
October 16th, 2003, 04:23 PM
One drop of NG left my ears ringing for days. AP for a few seconds.

bobo
October 16th, 2003, 04:41 PM
How did you do the hammer test? What do you use to put the powder on/in? How do you whack the NG without it running?

I whacked a coffee filter with ~.5g of AP the other day, whacked again a few times and nothing happened. So I put it into a cap with a fuse ripped from a firecracker and blew it into pieces, so it was good AP allright.

McGyver
October 16th, 2003, 05:01 PM
0.5 grams i alot for a hammer test! .1g is enough to leave your ears ringing...

Hammer test works better when you put the explosive on a flat surface, like a piece of metal.

Will a 1g pressed cap detonate 20/80 APAN charge? YES it will, probably even the standard 10/90 as well....DBSP

knowledgehungry
October 16th, 2003, 05:55 PM
I dropped it on hot metal :o. And lets get this back on topic eh?

Efraim_barkbit
October 17th, 2003, 10:08 PM
I set of quite a few APAN charges in the end of this summer, I dont have a very good scale, but I used approximatley 10-15%AP.
In most of the smaller charges I made with it, I used pieces of garden hose(1,5cm inner diameter).
I first press the APAN to the wanted level into the hose, then I press ~5mm straight AP on top, before I add a little loose powder and the fuse.
Never failed me yet.

If wider charges is to be set off, I often use a 4cm piece of pen casing with AP (sometimes APAN in that too, to minimize the amount of Ap even more) 2/3 to full lenght inserted in the charge. Thats between 0,5 to 0,75 ccm inside the charge. In fact, I have never had an APAN charge fail because of too weak detcap. Sometimes the cap hasn´t made d-d transition because of damp AP, but I don´t count that.
If I scale up a bit, say >50g APAN, I use a bigger det, up to a maximum of~5ccm pressed APAN for my biggest APAN charge, wich wheighed in at 100g.

EDIT:
Ooops... That ended up more OT than I thought...but if I sum it up in this point:
You won´t need a lot of AP to detonate APAN., Now it´s at least a touch...

Efraim_barkbit
October 22nd, 2003, 12:11 PM
I just made a test with unconfined AP.
I used 2 teaspoons of AP, wich I put in a pile on top of the electric ignitor (a steel wool wire between two wires to a 9 volt battery) on top of a pice of one inch thick wooden board.
It detonated just like if it´s been in a casing, and I could feel the shock slightly 6-7meters away. and it also blew the board to pieces.

I have some AP left and I would have tried with 1 teaspoon too, but I´m in a hurry now. Maybee tomorrow

edit:
the pile was on top of the board, not the other way around.

DBSP
October 22nd, 2003, 12:58 PM
Just to clarify things a bit. the AP was not unconfined. The wooden board would have given the AP the needed confinement.

Try the same thing again but with nothing on top of it, not even a thin layer of plastic sheeting or similar.

McGyver
October 22nd, 2003, 07:08 PM
Most synthesis say to store AP you need to keep it under a layer of water. Well mine just floats on top, does anyone else have simular characteristics?

blindreeper
October 23rd, 2003, 03:14 AM
Mine floats ontop, but after about a week of storage its a nice suspension and most of the AP has been submerged

the_chemist
October 24th, 2003, 02:15 AM
My AP floars as well. I actually left a batch precipitating for a bout a week, after which the acetone had all evaporated and there was a nice amount of AP left in the bottom.
When using hydrogen peroxide in high concentrations, does anyone know if its possible to get pure stuff around 30-40%?

blindreeper
October 24th, 2003, 03:08 AM
Do you mean get pure H2O2 in 30-50% concentrations? HA you have to be kidding with that question! Of course you can. Check out the OTC survey thread to find out more details.

Cyclonite
October 24th, 2003, 05:39 AM
Chemist, this isn’t the place to post such questions. Those go in the water cooler, the next question you might ask is where to get it. Most would say search and your wanting to be spoon-fed but ill nudge you in the right direction try a hydroponics store. Only ask questions of those types in the water cooler, even then asking questions that can be answered by searching isn’t a good idea.

Efraim_barkbit
November 11th, 2003, 02:00 PM
When playing around in MS Excel with a “programme” that I wrote for calculating the amounts of Acetone and X% hydrogen peroxide needed for Yg Acetone peroxide, I saw something that caught my attention.

First, I saw that the amount of acetone, in millilitres ≈ the theoretical yield of AP in grammes. (-2,4ml @ 1000g)
Example: for 50g AP, the amount of acetone needed is ≈50ml.

Then I thought that there might be something that simple for the hydrogen peroxide amount too, so I put together some readings and made a graph.(I used 30% H2O2 in these readings) Then I got the formula:
Y≈ 1,09X ( +1,3ml @ 1000g)
Y= H2O2 amount in ml
X= AP amount in grammes

Example: for 50g AP, you need 1,09*50g= 54,5ml H2O2 (30%)

If other percentage is used, the formula can be changed easily by first dividing 30 with the percentage H2O2 you have, and then multiplying the results with 1,09.
for example, if you have 6% H2O2, Then you do as follows:
30/6= 5 and 5*1,09= 5,45
wich changes the formula to:
Y≈5,45X

Of course, you probably won´t get a 100% yield, so don´t come and complain when you get less AP from your batch than my formula said you would get.


All of the above depends on if I got my calculations correct, so if you spot something wrong, please let me know.
3 moles Acetone <-> 3 moles H2O2<-> 1 mole AP<-> 3 moles water
1mole acetone: 58g, 1mole H2O2: 34g and 1mole AP: 222g

Ammonal
November 12th, 2003, 08:22 AM
I have just aquired all of the materials for AP and I am well versed on the procedure, only problem is I dont have a fridge to put the reaction vessel in. If I get a couple of kg's of dry ice in an esky (polystyrene box only bigger with a plastic skin) would this be suitable for the reaction to occur or is the approx -60degrees too cold for the process?

knowledgehungry
November 12th, 2003, 07:07 PM
It should work, it might take longer. You would aslo probably end up with a larger percentage of trimer:)

ALENGOSVIG1
November 12th, 2003, 07:13 PM
It'll most likely freeze.

Ammonal
November 12th, 2003, 11:37 PM
Ok thanks for the advice I will try it as it should allow me to leave the reaction vessel for 24+hrs. I am thinking along the lines that it will take longer that is the reaction will be slower but the cold temp should favour more of the trimer AP.
I will also try the shorter ice methods, there are mixed insructions ;some say leave it for a couple of hours while others say put it in the fridge for 24hours.
I am going to pick up the dry ice today for the first batch. and tomorrow I am hoping to make a second batch using just normal ice.
I will post the results of both here.

McGyver
November 14th, 2003, 11:02 AM
If you can't use a fridge, :rolleyes: then use H2SO4 for the reaction, crystals will form faster then 24 hours.

Ammonal
November 15th, 2003, 09:26 AM
I am hesitant at trying H2SO4 as the acid catalyst because I read somewhere that using it favours production of the dimer form. I do not know the validity of this but I am going to test it. I currently have a batch of AP (100ml 6% H2O2, 50ml 100% acetone, 15ml 35%HCl) sitting in a beaker inside my esky with 4 litres of methylated spirits and 5kg of dry ice. It has been sitting in the dry ice now for 8 hours, with a small precipitate on the bottom and the top of the beaker. I scraped a small amount out with a plastic spoon and waved a lighter near - resulting in a rapid sp. deflagruation and a light pop. So I know that I have some AP formed.

Nevermore
November 15th, 2003, 09:59 AM
I suppose the dry ice brings the temp too low for a good reaction to occurs..0°C would be enough for forming mainly the trimer version.
H2SO4 doen't form the dimer, the acid is only a catalyst, the temperature decides if dimer or trimer should be formed. so keep your temp lower than 5°C to form mainly trimer version.
The batch of AP you are making is quite large, i've never worked with more than 25ml of acetone at time, raise the temperature to -5°C-0°C and the reaction will proceed much faster..

Ps i suggest you work with smaller batches, then seal the becker with plastic wrap after adding the acid, and bring to fridge, so doing no smell will leak out and the Ap will form at best temperatre control.

T_Pyro
November 15th, 2003, 01:27 PM
I am hesitant at trying H2SO4 as the acid catalyst because I read somewhere that using it favours production of the dimer form.

That's because H2SO4 tends to produce localised hot spots, which promote the formation of the dimer. If your reaction mixture is kept at around 10*C or lower, you shouldn't have any problems.

Ammonal
November 15th, 2003, 11:17 PM
I have just checked the reaction beaker and the cloudy solution has cleared and the is a large precipitate on the top and bottom of the solution. Is it normal for the solution to return to a clear state? I am thinking it could indicate the endpoint of the reaction.
I am about to filter and wash the AP.
NOTE: the reaction beaker was left for 25hours in very close to -60degrees C.
I will report the final yield in a couple of hours.

blindreeper
November 15th, 2003, 11:40 PM
-60 *C :eek: You probably will be disapointed with the yeild because the reactions was so cold it didn't react as much! Example hot acid will eat metal faster than room temp. acid. Then again room tempertaure acid will eat metal faster than -60 C acid. Thats jsut an example, the same goes with AP it will take far longer to react in such cold conditions.

Ammonal
November 16th, 2003, 07:56 AM
I have just finished washing and filtering the AP, I would say that because this was my first time making, collecting, filtering etc I have lost about 1 gram of AP, and my final dry yield is 8 grams. Which is 3 grams better than the estimate I was aiming for, so as far as I am concerned it has been a success. Tomorrow I am going to try the standard ice method, guess I'll have to defrost the freezer for mum after all :p
The 8 grams of AP was produced from 100ml 6% H2O2, can anyone say if this is a good or bad result?

blindreeper
November 16th, 2003, 08:29 AM
Considering I used 200ml of 6% stuff and got next to nothing I would say thats a very good result. Just wait until you get some high conc. H2O2, damn there is lots of AP! But be careful and play it safe. Make whatever you feel comfortable with. As in the first time I made AP with 25% H2O2 and I had over 60g of AP on my hands! That is not easy to get rid of safely and silently ;)

Efraim_barkbit
November 16th, 2003, 11:47 AM
Here is a formula for calculating the amount of acetone needed for for optimal ratios with Xml 30% H2O2 (note: the amount of acetone = amount of Ap with 100%yield)

Formula: (30% H2O2)
X / 1,09 = Y
Where Y is the amount of acetone in ml (= amount of AP with 100% yield in grammes)
example:
with 50ml 30%H2O2, you should use 50/1,09=45,9ml acetone (= 49,9g AP if 100% yield)

If you have another percentage of H2O2, the formula is easy to change.
Formula (Z% H2O2)
X/ (30/Z*1,09) =Y

Example: Z=6%
X/ (30/6*1,09)= Y
X/5,45=Y


If you want to calculate how good your yield was, just divide the amount of AP you got from the synth with the amount 100% yield would have got.
Example: Ammonals yield: 9/ (100/5,45)~ 0,49 =49%

________________________________________________

@Ammonal:
Thats not very good yield compared to 100%, but it is probably hard to get much better with so low concentration of the H2O2, combined with the very low temperature you used.
It will be nice to see the results from the other batch, and how much(if any) better the yield is.

do you still have the reactants?, it would be interesting to see if there is any more AP forming if you leave it in room temp for a couple of more days. and, how much acetone did you use?

How was the size of the AP crystals?

Ammonal
November 17th, 2003, 12:45 AM
Efraim_barkbit: I have been watching the reactants at room temp for ~20hours now and they have only become slightly cloudy with no definate precipitate, I am going to leave it for another 2 or 3 days and observe the results. I used 50mls acetone.
The AP crystals are like flour, very very fine. They detonate excellently; 0.5grams turned the coffee filter, after it was wrapped in masking tape into confetti :D

Efraim_barkbit
November 17th, 2003, 04:25 AM
Thats WAY too much acetone,
The optimal would have been 100ml/5,45=18ml,
If you leave it so that the acetone evaporates, or add another 150ml H2O2, you will get more AP out of it,

chemofun
November 23rd, 2003, 10:22 PM
I'm new to making explosives and I thought AP would be a good place to start (after reading as much as i can about it). I'm prepared to take every step possible to make it safely and I've gathered the ingredients except for one... I need an acid catalyst but i can't find mineral acids anywhere. Any help would be appreciated. Thanks in advance.

JBC
November 24th, 2003, 01:01 AM
chemofun, i really wouldn't bother making AP. i haven't made it myself, but i was sort of considering it at one point. after hearing about how many accidents people have with it though, i've decided it's not a good idea - it's far too unpredictable. personally i plan on trying to make MEKP instead, but don't have the time to do so yet. it's a lot more stable and is sensitized fairly easily if you want it to be that way.

in regards to acids...hydrochloric isn't all that difficult to find, it's used for cleaning cement in 30% concentrations. sulfuric is a little more difficult depending on where you live, but a few plumbing cleaners use it, and usually in high concentrations (~95%).

blindreeper
November 24th, 2003, 02:17 AM
i've decided it's not a good idea - it's far too unpredictable
How can such a statement be valid if you have not tried it yourself? As far as I am concerned it is a completely invalid point!

flash619d
November 24th, 2003, 11:37 AM
Originally posted by JBC
chemofun, i really wouldn't bother making AP. i haven't made it myself, but i was sort of considering it at one point. after hearing about how many accidents people have with it though, i've decided it's not a good idea - it's far too unpredictable. personally i plan on trying to make MEKP instead, but don't have the time to do so yet. it's a lot more stable and is sensitized fairly easily if you want it to be that way.

in regards to acids...hydrochloric isn't all that difficult to find, it's used for cleaning cement in 30% concentrations. sulfuric is a little more difficult depending on where you live, but a few plumbing cleaners use it, and usually in high concentrations (~95%).

HCl can be found at Lowes or similar as muriatic acid. H2SO4 can be found in ~%35 conc. as battery electrolyte, and IMO, is the easiest and cheapest source for a lot of acid at ~US$15 for a 5 gallon bag which you can concentrate to ~1.5gals of %95. Of course, that's a lot of boiling. AP isn't too unstable, it requires a fairly hard shock to detonate, so if you're careful, you will have no problems. Most people have accidents because they did something that they knew was dangerous, or something they should have known was bad. Nearly all accidents can be avoided, if you act logically, don't rush, and think things through. AP is one of the best HEs for beginners, as it's fairly easy to get the precursors for, and is not too difficult to make.

Ammonal
November 24th, 2003, 04:41 PM
I wont bother quoting you JBC, but unless you ACTUALLY make AP, you have no idea how stable AP is in the hands of someone who researches; reads; asks questions and then ACTUALLY makes AP. I too, only a week ago had no experience with AP whatsoever, BUT NOW I have made roughly 50grams of it and I followed the instructions here and from other sources and I have yet to have a batch that has 'gone wrong' or any that has been super sensitive and blown my fingers off.
I have made detonators by pressing dry AP into .22LR cartridges, it is not unstable when it is handled with respect.
I am too tired and sick of covering old ground to continue flaming your post so I will leave you with a final comment; next time you consider posting DO so ONLY if you have something worthwhile to add.

PS: Gee I didnt know I had that much spirit to flame someone like that, heheheheHA!

RabidGeneral
November 24th, 2003, 07:44 PM
chemofun, I hope you don't mean COMPLETELY new to pyrotechnics. If you are completely new, start with LE's such as BP and flash, and then move on to HE's. If you make AP as your first explosive ever, chances are high you're gonna hurt yourself.

chemofun
November 25th, 2003, 12:15 AM
Thanks for all the info. I've worked with things that explode before; but I've never made my own explosive compounds. Just out of curiosity (and i know it's off topic but) are high voltage electrical discharges and working with plasmas (like from Tesla coils) considered pyrotechnics?

If this is too off topic then dont answer if you dont feel like it.

Bert
November 25th, 2003, 10:48 AM
No... That would be electronics and/or physics.

nitriees
November 27th, 2003, 10:27 PM
I have make AP three times, the precusor I used was,
H2O2 50%
HCL 33%
Acetone ~99%

Place the H2O2/Acetone mix into ice water bath, add HCL slowly and
maintain the temperature below 5 degree celcius, with continuosly stir,
add excess HCL, stop adding when 30% AP already precipitate.
Just need another hour for AP to precipitate almost completely, fast and easy.
No run away reaction encounter like when I make HMTD.

chemofun
December 4th, 2003, 08:36 PM
where do you guys get your concentrated h2o2? I only have 3% so my yeild sucks.

blindreeper
December 4th, 2003, 08:52 PM
SEARCH!

Look for the Great OTC Survey thread in Chemicals, Appartus and Equipment!

Sir Dudalot
December 4th, 2003, 08:59 PM
Exactly. I don't think the yields for 3% are really THAT bad. Actually, for 300mL of H2O2 I can get about 10g-12g of AP which is right in line with some other peoples synths who use 30%. The only difference is they get 40g and use four times as much (I compared it to Alengosvig's yields). To get decent yields using 3% I use an excess of 100mL of acetone to 300mL of H2O2 and 50mL of 91% H2SO4. I let it react for a few days. I know this is exessive and wasteful but when you only have 3% it's almost worth it.

blindreeper
December 4th, 2003, 10:12 PM
Sorry to say this Dudalot, but you can't say anything about how good yeilds are from 3% untill you have had high conc, H2O2. The yeilds are amazing its like a slurpie (frozen coke) of AP. 3% hardly compares to that, I have tried both.

Sir Dudalot
December 4th, 2003, 11:12 PM
Yes, but what I was trying to say is that the yield comes out to relatively the same in the end. Alengosvig uses 120 30%, I use a quarter of that and get a quarter of his yield. High conc. H2O2 is good because you can make more at a time instead of having to deal with thousands of mL of H2O2. Higher conc. H2O2 also gives you the yield quicker with less acid and acetone to deal with. Damn, so many advantages that I'm missing out on. I've been checking all my local and not so local pool supply stores for it but they never seem to have some. Someday....

mikey
December 6th, 2003, 03:25 PM
"sir dunalot" if you do not mind mail ordering your h202 there are plenty of Hydroponics Suppliers, usually it's about 17.5%, but some is 30-35% you just gotta look for it. It is usually sold as Oxy Water Oxygenator or instant oxygen or somthing like that. Hear are links to several websites that do it in the US.


http://www.1-hydroponics.co.uk/cgi-bin/shopper.cgi?preadd=action&key=N87

or


http://www.aci-hydroponics.com/ has loads of links to suppliers in the USA

or

http://www.genhydro.com/dealerlist.html even more suppliers in the USA

or

http://www.quickgrow.com/cgi-bin/shop/search.cgi?query=H202+

or finally if none of them work and you got a spare 399 dollars you can buy 50 gallons of 35% for hear

http://www.groworganic.com/a/item_PSA860_HydrogenPeroxide3550Gal.html

thats alot of AP:D and if you still cant find anything just do a search on google for a Hydroponics Supplier, good luck finding some

Sir Dudalot
December 8th, 2003, 11:26 PM
Wow...I've never really looked for suppliers that could ship it to me. However, after trying just about every other alternative (pool supply, hydroponic, rocket fuel, etc.) I'm beginning to think that ordering it might be the way to go. Many many thanks for all the links. They look quite promising. Once again, thank you.

Evan007
December 12th, 2003, 06:55 AM
Holy S***! LIKE A SLURPIE!?!?!?! Thats Unbeleivable. I have only ever used 6% h2o2, which in my method results in a layer on the top or bottom (or both) of the beaker (depending on how long I leave it) which is easy to filter and wash.

In My opinion it might be better for begginers at AP to use the lower concentrations, in order to avoid run-aways and also excessive amounts of AP, The latter might not sound so bad, but people who arent completely familiar with the properties of AP might unwittingly do something that they didnt know would instantly and unmercifully remove fingers. I suggest familiarising yourself THOROUGHLY with AP before going for the "supa-size slurpie"

just a message for any real begginners thats all.

chemofun
December 15th, 2003, 03:23 PM
Hey thanks for all the info. I've made several batches of AP now and i was wondering if anybody knew an easy (and safe) way to start mass producing AP? I mean like a a pound or a half pound per batch.

Stubine
December 16th, 2003, 02:51 AM
I use H2SO4 in the form of Rooto Drain Cleaner, 30%H2O2, and I get instantanious results and terrific yields. It is a bit of a pain to use the H2SO4 though, you have to add the acid very very slowly, and I usually have to put the reaction mixture in the freezer a few times before I can get all of the acid in. The results are well worth it though. I have a question concerning making an ap "putty" though. I understand you can use NC and acetone as the other compound in an AP/NC mixture in a 50/50 ratio by weight. Has anyone here made ap putty?

grendel23
December 16th, 2003, 07:13 AM
There is no safe way to make large quantities of AP.
There is no safe way to store large quantities of AP.
There is no safe way to use large quantities of AP.

AP is unstable and unpredictable. You can get away with using small quantities if you are carful, but large amounts are very dangerous.

Read some of the threads on accidents, AP is the culprit in many cases.

Ammonal
December 16th, 2003, 08:06 AM
Chemofun: There is a place called 'The Water Cooler' on this forum where you can go to make statements "like i want to make a pound of AP", otherwise for things that you would make in one pound batches there is the 'High Explosives' section.

Sir Dudalot: I would suggest that you do not use excess acetone on your AP synth, because it has the nature of a powerful solvent - one of the thing it dissolves is AP. I performed a test once where a batch was filtered and weighed, result: 8.5grams, I left the filtrate for a week in the sun to drive of the excess solvent I had used and then put it into the fridge when it nolonger smelt of acetone. After it was cool more AP precipitated and I filtered and weighed this gaining another 7 grams of AP. The ratios I used were 150ml 6%H2O2, 50ml acetone, 30ml 30% HCl. This in total with the extra week of evaporating the acetone gave me 15.5grams from that batch. It was time consuming but it did establish that an excess of acetone is not an advantage. I now use 100ml 6% H2O2, 15ml acetone, 20ml 30%HCl and get a yield of 9-10 grams consistently.
Just a suggestion though, damn I want some higher concentration H2O2! :p

matjaz
December 31st, 2003, 02:03 PM
Some dream data:
It looks like we all get 20-25% yields. The final mass of AP would ideally be approx. equal to the mass of acetone used. I use 12% strength hair dye lotion (whiteish colloid thing) as H2O2, and old HCl which was once 30%. If I use 1 part HCl for 10 parts acetone, I get most of the reaction done in some 48-72 hours and a yield of 20%. Doubling the amount of acid, it only takes about 20 hours to get 25% yield. (All numbers after filtering... etc. losses).

K'Luuppo
December 31st, 2003, 04:25 PM
I red somewhere on the Forum that nitroglycerin will be nasty if it freezes and then melts.
If the acetone/hydrogen peroxide/acid mix freezes with maybe some AP in the beaker and then melts, what will happen? I just don't want blow our balcony's windows out...

bigbang
January 5th, 2004, 02:09 PM
Does any one know how AP reacts with NaOH ? If it does not react with it and the HCl does not get consumed (it is just a catalyst) Then wouldn't adding the same amount of NaOH of HCl you used after the reaction is finished, neutralize the acid? You would end up with NaCl, H2O, AP and what ever is left of the Acetone that didn't get used in the reaction. The AP should float on top of the salt water and be neutralized. After removing the AP all you would need to do is let it dry.

If this has been asked before, forgive me. I looked through the four pages of posts but diddn't see anything.

Ollie Snowie
January 5th, 2004, 04:20 PM
If you want to neutralize the HCl you might as well use bicarbonate of soda because it's not as as soluble as NaOH and you can tell when you've added enough because the mix will not fizz when you add more of it. Also, HCl is a gas when it's not in solution, so as your AP dries the HCl will float away. No need for neutralization if you're using HCl.
[EDIT - Sorry, I tried to put in a Tab and then pressed Enter by mistake. Anyway, do without the Tab]
You'd need far more than the necessary HCl and NaOH to make the AP float on the brine produced, and what's wrong with filtering it?

--------------------

newbies reading this post also read my post below - kingspaz

xyz
January 5th, 2004, 10:10 PM
Ammonal, check pool shops and hydroponics shops for some 30% to 50% H2O2. 50% H2O2 is sold as "Oxyplus" in most Australian hydro shops for about $20 per litre. I was able to buy a bulk 5L container for $75. It may sound like a lot but it works out much cheaper than the 6% stuff once you consider how much H2O2 it contains.

Sir Dudalot
January 6th, 2004, 09:14 PM
I just finished an AP synth using ~30% H202 (boiled down from 3%) and the crystal structure is very noticeably larger. I mean, it's not gigantic, but obvious. It's definitely smaller than salt crystals. Normally when it's wet and drying it's kind of creamy but this time it's grainy. I'm assuming this kind of crystal size is normal for using more concentrated H202.

I'd like to say that the yields from concentrated H202 truly are better than 3%. It really is like a slurpie. I don't think I'll ever be able to go back to 3% now. It took less time and less reagents, the two things I don't have much of. Blindreeper, I'd like to say that you are absolutely right about concentrated H202 being worlds better.

Ammonal
January 7th, 2004, 08:00 AM
Its all good now XYZ, my delivery came just 2 days ago and I've made 79grams AP and 194grams HMTD. One thing I gotta say about making HMTD is if you've got some 50%H2O2, then dilute it by at least a half strength again, otherwise unless you add solid dry ice into the acid/H2O2,hexamine it go runaway before you add your acid catalyst! What I mean is to dilute the H2O2 to at least 25% or about 15-20% concentration seems to be controllable. I paid AU$20 for 500ml oxyplus, do any fellow aussies reckon this is dear or what? I found another product called "oxyponic" in a litre bottle for $20, anybody in Aus know if this is H2O2? (it must be the only thing about online ordering that sucks; not knowing what something is until you've got it and paid for it and its the wrong stuff! :()

xyz
January 7th, 2004, 08:30 AM
That is quite an expensive price for oxyplus. See my post earlier about prices.

I use straight 50% H2O2 for my AP synths but I make sure that it is in a good salt ice bath and all the precursors have also been cooled.

kingspaz
January 8th, 2004, 09:53 AM
Ollie Snowie, nice theory, BUT is your AP ever going to be COMPLETELY dry? i think not. there will always be a residual amount of miosture in it since you can't heat it to drive the last bit off. thus, it will always be acidic since the 'water' will still contain HCl. so, you are wrong in saying you don't need to neutralise it.

T_Pyro
January 8th, 2004, 10:20 AM
Originally posted by Ollie Snowie
Also, HCl is a gas when it's not in solution, so as your AP dries the HCl will float away. No need for neutralization if you're using HCl.


Not going to happen. HCl is too soluble in water to just "float away" as the mixture dries. Even IF you were to heat some aqueous HCl (which I don't think you're going to be doing in this case), you wouldn't be able to discharge the HCl completely.

Hang-Man
January 11th, 2004, 04:22 PM
Yes, even when I let my AP react for a long time, there is sufficient HCl to make it bubble when bicarb solution is added.

PS. I have pics/ video of some AP crackers going off with various things. Should I post them here/at all?

kingspaz
January 11th, 2004, 06:31 PM
the reason there is still plenty of HCl left to make bicarb bubble is because it isn't consumed by the reaction. it is a catalyst for the reaction and catalysts are not used up. so you should still have the same amount of HCl in there that you started with.

inverse
January 12th, 2004, 08:24 AM
Chemofun,
in the field of primary explosives there's no such thing as 'mass production'.

Industrial production batches of lead azide and mercury fulminate are always kept at laboratory scale.
There's a reason for that.

lucas
January 12th, 2004, 11:06 AM
XYZ: My Oxyplus , 500ml was markred $17 but I paid $15 because thats what the local guy does. I have found that it definately should be diluted for meduim sized or larger batches. Small, ie <50ml batches are ok in full concentration, but then I base this on mainly HMTD synths. AP synths with this gear, the 50% H2O2, can be given a fraction of the acid, which is nice for neutralisation later. I also would like to remind everyone that if using H2SO4, that it should be added to water to dilute it and then cooled before it is added to the mixture of reactants. The heat released when it reacts with the available water is quite immense.

My experience with the 50% gear also shows that the acidity of the acetone, mentioned in other threads is sufficient for a slight reaction to occur between the reactants before the addition of the extra acid catalyst.

Regarding Oxyplus, my hydro shop guy sugested that I might want to try another new type of product because some growers were finding that the hydrogen peroxide sanitisers were not always preventing infection. This abvously leads me to believe that there must be other sanitisers that are not H2O2. I dont know what these products are, but it isnt H2O2. Oxyplus and similar products also refered to as oxygenators on their labels, aswell as sanitisers, so "oxyponic" is likely H2O2, since the name implies it i an oxygenator.

blindreeper
January 12th, 2004, 08:54 PM
When on I was hunting down H2O2 as oxyplus some drongo at the hydroshop tried to sell me this H2O2 with some funky silver compound in it, may be what your talking about. All I know is I didn't want to buy it :P

chemofun
January 14th, 2004, 10:52 PM
I got my h2o2 at an organic food market as a chlorine free bleach. Its great because its very concentrated ( i dont know exactly how much but i can tell from my AP synth that its very good) and it doesnt have any inhibiting ingredients. The one I got is called Ecover. It's also very cheap. Something like 4 US$ for a half gallon jug which makes quite a load of TCAP. If anyone has a method of testing concentration of H2O2 then I'm sure everyone here could benefit from it.

bigbang
January 21st, 2004, 02:54 PM
Ollie Snowie - I was just looking for a way to not need to wash/filter 18(sarcasim) times to remove the acid from the AP. I was thinking that adding NaOH to solution I could just filter the AP once and not need to wash it in water or a bicarbonate of soda solution.

Wild Catmage
January 22nd, 2004, 06:40 AM
I'd choose to add NaCO3 instead of NaOH, as NaOH can be corrosive in higher concentrations. NaCO3 will react to form CO2, H2O and NaCl, and the NaCO3 is soluble in the acid/water mix. Add it before filtering, let it react, then filter out the AP.

Cyclonite
January 22nd, 2004, 08:53 AM
I just submerge the ap in a filter into the strong bicarbonate solution for 30min then in water....Iv never had any problems

Hang-Man
January 25th, 2004, 12:54 AM
I put my raw AP in a coffee filter suspended over a beaker held there with an elastic band around the lip. Then I pour in 100 ml of water, 100ml of Bicarbonate solution, then spred it on paper and let it dry. Granted I never store it very long, but it has always been stable, never giving me the slightest problem.

If you are overcome by the urge, as I was, to fill a copper pipe with AP and set it off. For Gods sake get some cover. It sends shrapnel everywhere, peppering the coffee can I had it in with holes. If it’s your first time making some and you want an idea of what it could do, <a Href=Http://www.geocities.com/hangmangod/Pics.html?1075005843894>go here</a> to see the site I made in less time than it took to type this message.

Damn you geocities...I could post the images here, but they need to be pretty high res to get the idea.

Boomer
January 26th, 2004, 07:35 AM
I may be the last one to tell others to be careful, missing fingers myself since 3 weeks. But if you HAVE to put AP into a metal casing, for gods sake use a remote press and seal the end with tissue + epoxy so the AP cannot be pressed/moved before handling the thing. Another member lost fingertips while lightly (!) pressing some AP into a plastic straw (!).
It is a good idea to use max. ½ g AP, pressed in first, and then add a less sensitive HE. This also increases power further. Your blown copper pipes would be dust (<1mm pieces) instead of ‘peeled bananas’ if you had used PETN / MHN / ETN etc for the main charge. They generate over 200 kilo-bar (tons/square cm) compared to approx. 30 kbar (IIRC) for AP.
And: AP as a main charge is suicide! One static spark, one bigger crystal, …..

Cyclonite
January 27th, 2004, 03:36 AM
I dont think it would be quite dust but more like bird shot. Iv put military caps under coffee cans and it looks like it was hit with a shotgun afterwards and its all bowed out. You get some great height on the can also. As for AP as a general rule keep the caps away from your main charge until you place it. Pressing should be done remotely as mentioned. Its kind of strange but when I use 6% H2O2 vs. 30% I get better quality AP, allot less though.

Guerilla
January 27th, 2004, 04:56 AM
But isnt the PETN in commercial caps shaped to focus the explosion outwards from the end, thus the peeling effect? At least the caps Ive seen have only blown about an inch from the other end and looked like a trumpet after that (if detonated alone). Im sure it would make a significant difference if PETN was used instead of AP in a similar pipe..

Cyclonite
January 27th, 2004, 09:09 AM
The end of the cap is blow apart but the less powerful explosives in the blasting cap train leave a banana effect. Iv only seen this a couple of times though, most caps I use are destroyed by the main charge:D

Efraim_barkbit
January 28th, 2004, 04:37 PM
When I went out today to dry out some AP, I found that the moist AP had now frozen to a hard solid "cake"in the coffe filter it was sitting in.
I have heard about NG becoming extremely sensitive when frozen/thawing, How worried shall I be about the AP, should I dare to thaw ice in it?

The other option is to take it out in the forest and ignite it in the filter.

Since it isn´t the explosive in itself that is frozen, I figure that it could probably be thawed with out increased stresses on the crystals, I guess that the actual freezing is more stressing.
But I´ll probably go with the second option anyways.

Guerilla
January 28th, 2004, 06:19 PM
Ive once had AP in frozen liquid too, I let it thaw with some water and processed normally. I dont think the freezing would make the crystals any bigger, after all the reaction just gets slower and slower along the temperature drop and those that form are even smaller than normal. While the ice will stress some of the ap, the DDT is unlikely to happen if its all moist. In NG's case its frozen itself and thawing generates more friction between molecules..

Hang-Man
January 31st, 2004, 08:59 AM
I let my reaction run outside all night and in the morning it was a solid block, I put a few ml of water in it and the "block" disolved pretty fast. I broke it apart with a glass stirring rod and moved it around for a few miniuts and it disolved into a slurry of AP which I processed. I noticed this AP was allmost granular but that may have been because I didn't let it dry very long before useing.

Efraim_barkbit
February 1st, 2004, 07:42 AM
I have solved the problem, I just poured warm water over it.
Strange I didn´t think of that myself, so simple.

I also tried to ignite a piece of the "frozen" AP, and it wasn´t possible to keep the deflageration going, it just made a small fireball and got slightly smaller with each ignition. when in contact with a red hot wire, it made a "snapping" sound, but nothing more.
(the piece of AP was ~2x1x0,5 cm, ignition methods was fuse and electrical ignition, and some smaller pieces with open flame.)

It is drying slightly below room temperature as I write, hopefully dry before evening., Damn, I havn´t detonated anything for over a month, and I can´t even walk past a big heap of snow, without wondering about how big snow cloud 400g ANNM would make of it.

al93535
February 15th, 2004, 11:06 PM
I did my synthesis of Acetone Peroxide and got better each time I tried it, using varying amounts of reactants. The first time I tried it I did this:

100 ml 50% h2o2 (3% frozen to concentrate)
45 ml 100% acetone
21 ml 29% HCL
Acetone and H2O2 reacted and climbed about 4-5 degrees celsius to about 7 degrees. Let mixture cool back to 2 degrees, added HCL in 3 ml increments rose about 1-2 degrees per addition.
90 minutes added 2 ml HCL some nice precipitate.
3 hours, lots of AP thick layer on bottom.
6 hours looks nice! lots of AP.
Precipitate colleted after 24 hours
24 hours good yeild. Final yield of 3.568 Grams
You can view my pictures for this synthesis at www.geocities.com/al93535/index.htm

Then I tried this:
100 ml 50% h2o2 (3% frozen to concetration)
150 ml acetone
30 ml HCL
24 hours nice nice amount of precipitate, about 1/4 cup on bottom.
Precipitate collected afer 32 hours
Dry final yield 10.046 Grams

And this is the one I tend to use now:
60 ml 50% H2O2 (3% frozen to concentration)
100 ml 100% Acetone
24 ml 29% HCL
24 hours reaction time
Dry final yield - 10.7762 grams!

On a side note, I also found that using the 3% h2o2 concentrated by freezing works very well. Put it in a baggie, put it in the freezer, and watch it until it's almost totally frozen. Then pour out the liquid back into container. Tested to be about 50%.

matjaz
February 16th, 2004, 04:41 AM
al93535,

if your H2O2 really is 50%, your ratios are way off. Please read the AP section on www.roguesci.org/megalomania and recalculate for 50% peroxide. I won't tell you the right figures because I want you to read it and do it yourself. ;)

Also, are you sure you got 50% peroxide with freezing? How did you test it? Your yields seem shitty... A good harvest of AP is around 1/3 of initial acetone weight.

When you figure out the numbers, limit yourself to 10ml acetone for one batch. You should get over 3g of dry AP this way and this can still reduce everything from your wrist down into red mist. Seriously. This is a primary explosive, so it can happen for no reason. Did you remember to neutralize before drying?

al93535
February 16th, 2004, 03:49 PM
Matjaz,

I calculated only for the third batch, using the formula I read on here somewhere ago: for 30% h2o2: X ml in h2o2/1.09=Y ml of acetone. I adjusted X/(30/Z*1.09)=Y so it came to be X/.654=Y, thats 91.75 ml acetone for 60 ml 50% h2o2. Added a bit extra to use up all the h2o2. So I got 1/3 of a good yield (10 out of 33 grams), since you say good yield is 1/3 of acetone weight.

I did a small test of the H2o2 by decomposing it over silver grains, and measuring the amount of oxygen produced. However I may have to do another as I believe there were a few problems the first time. (Maybe why I got shitty yield.) I will re-test, and run a reaction with only 10 ml acetone to check as you suggest.
I know how powerful AP is, haven't had any accidents yet. Safety is most paramount in my mind, and I try to limit risk! And yes I neutralized. I washed with distilled water twice, then 10% bi-carb solution, then water agan. After that I used the coffee filter as a tea-bag and dipped it into 20% bi-carb for about 10 min until no further fizzing was heard. Then one more bi-carb rinse, and a final water rinse. I plan on using a small AP det, 1 gram or so, to set off some NG as soon as I get my nitric.

matjaz
February 17th, 2004, 07:06 AM
al93535,

don't know about this formula, I use ratios derived from the balanced formula for acetone peroxidation. It's 34g pure peroxide for 50g acetone. By volume, that's approx. 30ml/50ml.

I'm guessing you add excess acetone because your H2O2 costs more time and money. It's tempting indeed, but if you have unreacted acetone at the end, a lot of AP will be dissolved in it and lost through the filter. (Although this may be a remedy: at the end of the reaction, dump everything in twice as much water. I think dissolved AP should precipitate.)

As a comparison, try this. 10ml acetone, 60ml of 3% H2O2 - boiled to 5ml, 2ml of 30% HCl.

Be careful with boil-concentrating H2O2, it can detonate above 50% conc., and it's extremely nasty on the skin.

I like your attitude. You fear explosives. I guess it spells "longevity". :)

- Another thought: At the end of reaction, my product is as thick as yoghurt, so I actually have to add water to make it pourable enough to get it all out.

Myrol
February 17th, 2004, 08:00 AM
G'day folks! Im a new Voice here so it could be intresting for ya what i can say about AP: For the Synthesis i used everytime 100ml Acetone, 150ml 30% H2O2 and 25ml 35Vol.% Sulfuric Acid (from the Drugstore). The Acetone was very cold and the Oxiplus around zero degrees. I mixed both Chemicals and let it sit for around 2h unchilled (its good to hold the Temp. after Acidcatalysing around 15°C). After that i put the Sulfuric in the Beaker and stir or swirl it until the gentle shit is nice mixed and can react for 24h at 15°C. A too low temperatur is bad for the Quality! It form hard lumps that i dont want to broke down into fine dust, because its AP not TNT.....The solid Block of AP is ready for Washing and i do it with Bicarb.-Solution until it smells not more so strong after Camphor! Blabla...washing with huge amounts water until its NEUTRAL (on a Towel, i hate these instable Coffeefilter) and drying near my Desk to do the last step for perfect quality AP! I take the Stainless-steel sieve from my Moms kitchen and sieve the dry product to carry out bigger lumps of hard AP. The sieved AP is extremly fine and ready for our good-old APAN! My Yield: 100g Acetone form 100g AP whats around the 80% mark!

phone
February 17th, 2004, 02:35 PM
Well, I am quite a newbie, I just make some explosives and blow em up for fun, and well, if I´m going to be honest, I don´t even bother going somewhere deserted, I just blow em up in the local park.

Well, I gotta ask i couple of questions, I made some other stuff and so,
but what I need help with is this:

"What quantity aceton/peroxid shall I have?"

I don´t really know, what I do is that I take a lot of snow in a bucket, take an icecreampack on 2L and put it in the bucket in the snow, then I put 4 parts H2O2 and 3 parts aceton and 0.1-1 part acid (depending on conc., sort e.tc.) Usually like 1 part 30% HCI.. (I read this is "Swedish Infomania")
It´s colder then 5C, that´s one for sure, but I´ve heard you get some unstable shit with stuff made over 5C so I try to cool it nice. (this one I read here somewhere).

Is this seriusly wrong or? And when I distill it I just take an eternity-coffeefilter and filter it a long time so I don´t get some acid reacting lame, and all the materials I use is in plastic. And this weekend I want to make like somewhere around 700AP and take a lot of AN and do some APAN :) But well, I could get some expertise :D And well, I think I could need the help of a pro or someone who really has read on, ´cause there are some people on this forum that just doesn´t.. Seem to know what they talk about (As I don´t am like that :( :P)

al93535
February 17th, 2004, 02:50 PM
Phone,

What concentration h2o2 are you using? And yes make sure you keep it as cold as possible between 0 and 5 deg. is fine for forming the trimeric isomer of AP. You should use glass for your reaction vessel, any glass, a drinking glass will work. We can't tell you if 4 parts h2o2 to 3 parts acetone is correct unless we know your concentrations. And did you say you wanted to make 700 grams?

Matjaz,
Thanks again, I am sure a bit dissolves in the excess acetone. Good idea to pour it into the water. I think I will try 10ml acetone, 60ml of 3% H2O2 - boiled to 5ml, 2ml of 30% HCl. Will post my results.

Efraim_barkbit
February 17th, 2004, 06:07 PM
The formulas I posted in this thread some pages back, is not correct.

I thougt about uploading the excell "program" I made, to help people calculate proper ratios for AP, and when I looked at it, I saw that I had forgot an important step when changing the H2O2 amount from grammes to ml.
I had overlooked the simple fact that the density varies with the H2O2 percentage.
So, I´m sorry to say that the formulas I posted is wrong.
the first (http://roguesci.org/theforum/showpost.php?p=48345&postcount=148) and the second (http://roguesci.org/theforum/showpost.php?p=48673&postcount=161) (except for the part about acetone volume= AP wheight, if 100%yield)

BUT, I´m working on correcting it, and I will post the correct formulas, as well as a excell "program" to do the calculations, hopefully done before the end of the week. it´s just not quite as simple as I thougt it to be.

Thank you, al93535, for (unintentionally) making me notice this.

phone
February 17th, 2004, 06:52 PM
Phone,

What concentration h2o2 are you using? And yes make sure you keep it as cold as possible between 0 and 5 deg. is fine for forming the trimeric isomer of AP. You should use glass for your reaction vessel, any glass, a drinking glass will work. We can't tell you if 4 parts h2o2 to 3 parts acetone is correct unless we know your concentrations. And did you say you wanted to make 700 grams?

Matjaz,
Thanks again, I am sure a bit dissolves in the excess acetone. Good idea to pour it into the water. I think I will try 10ml acetone, 60ml of 3% H2O2 - boiled to 5ml, 2ml of 30% HCl. Will post my results.


I use 19.5% technical. How Much I need isn´t necessery, I just want a lot but not too much ´cause it is still an explosive that is known to go screw people up..

Myrol
February 18th, 2004, 07:17 AM
Could it be that small amounts of Water in the finished charge AP increase its Power? In Fact, PETN does! Why not AP? Let me say 2-5% Water makes AP 1: more safer for transportation and pressing 2: Increases the Detovelo like the PETN-way 3: the water can broke down during the Detonation into oxygen and Hydrogen because the Carbon/Carbonmonoxide can reduce Water at Temperatures around 2000°C--> Wassergasgleichgewicht! Whats your opinion? Ive heard that from some Friends who ignites AP ever in wet form with a 2g AP-cap with great Success! An example could this one here: C9H18O6+ H2O--BAAAMM--> 7CO+ 2C+ 10H2 :p

bigbang
February 23rd, 2004, 09:29 AM
Ok, I see in many places through this thread how to calculate h2o2 and acetone needed. (which is easy enough given the reaction.) What I would like to know is, How does one go about calculating the amount of acid needed in an acid catalysed reaction. Other than just tring different amounts or relying on information given. (I don't like being told to use x amount, I want to know why.)

Myrol
February 23rd, 2004, 10:12 AM
Calculating is not necessesary! I use everytime Sulfuric Acid as Catalyst! My Drugstore sell it 96% for 6,9Euro per Liter! So i thinned some to a concentration 50% by Mass (around 37% by Volume) and chill it until its cold and useful for AP-preparation! I have a Yield 80% from Acetone within 24h at 15°C with sometimes stirring! 200ml Acetone and 300ml 30% H2O2 forms with 50ml 50% Sulfuric Acid around 160g AP!

matjaz
February 23rd, 2004, 10:32 AM
Myrol, yes, but this yield isn't comparable. You use a huge excess of peroxide, which is the expensive component. So in terms of peroxide used, your yield is just the same - between 30% and 35%.

Also, that's exactly what Bigbang doesn't want. Recipes. He was trying to understand. Unfortunately, there's no easy way to tell the amount of catalyst needed. The more, the faster the reaction. On the other side, a really BIG amount of catalyst would lower the reactant concentration, so...

scarletmanuka
February 24th, 2004, 02:26 AM
A little bit OT, but in terms of AP filtration, I have just discovered that A chamois is the way to go, it absorbs all the water very quickly, or lets it soak through, and when dry it is easy to reclaim all the AP unlike when using a shirt or paper towel when half the AP gets stuck in the little pores leaving behind a residue which is unreclaimable. I have yet to use it for HMTD, but I think it would be a very succesful method for optimising the reclamation of it from the pasty mixture that forms. If any of you have had the same experience as me where the HMTD just passes straight through the filtering membrane, or just gets stuck to it. Obviously the best part about it is that it is reusable.

Mendeleev
February 25th, 2004, 01:12 AM
Weary about storing acetone peroxide, I only make it if I use it, however this gets quite tiresome and I was looking for a possible mixture of AP and a less sensitive explosive for blasting caps. Most people seemed to be using APAN as a main charge, but I was hoping to use it as blasting cap, meaning about a 50/50 ratio, something which can be detonated with a nichrome detonator. However I was looking for something a bit stronger so I was thinking maybe 25/75 or 35/65 acetone peroxide to picric acid respectively. Would anybody like to comment or predict on the success of such a blasting cap?

Efraim_barkbit
February 25th, 2004, 04:02 AM
In the blasting caps I use, I use a piece of plastic pipe in appropriate size, fill it 4/5 or more with pressed 10/90 AP/AN, and fill the rest with straight AP, works like a charm, and uses very little AP.

IRC, someone said somewhere that it wasn´t very smart to mix the peroxide with TNP, I don´t remember the reason.

blindreeper
February 25th, 2004, 04:10 AM
Because you neutralize peroxides to free them of acid and then going and using them with an acid such as trinitrophenol is idiodic.

al93535
February 29th, 2004, 04:00 AM
I really messed up my test for my h2o2 concentration. Looks like it was only about 9%!! So to confirm it I bought 27%, and measured it at about 26%. Damn, I can't believe I errored that much! Anyway, I just tried an AP synth with the 27%. 55 ml h2o2, 30 ml acetone, and 13.6 ml 29% hcl (16% of reactant volume). As soon as I stirred in the sixth ml of acid ap was beggining to form, my solution was at 5 degrees. By the time I got to 13.6 the vessel was filled with ap!! Has anyone else had AP form quite that fast? I used to have to wait at least 90 minutes to see any, this time the bulk formed within 10 minutes! I sure hope about 5 degrees will form trimeric.

Myrol
February 29th, 2004, 12:25 PM
al93535: Yes its ok that your AP forms so fast as you said! I used 50% diluted Sulfuric Acid and my Beaker creates also within 5min. so much AP that you can see how the Atoms bond to the white fluffy Crystals! Umm you use 30% Hydrochloric Acid with good success! Did you believe its better than Sulfuric? I had a shitty runaway while making AP with HCl, thats the reason why i switched to diluted Sulfuric ;) Urbanski says its better to use Sulfuric instead of HCl to form more Trimeric AP but HCl is more Cheap :cool: Yesterday i blewed my first APAN-Charge into the Air and it was GREAT!! The 400g (25% AP, 75% AN with my scale) mades not a to loud BOOOMM but the Wave felts holy good on my Head :p (I was 500m away!! IN FOREST!!) Next weekend i look after the Crater because i had no Choice to went back after the Blast! The Cops are nice alerted since my 8kg ANFO............Whats your opinion? Wich mixture APAN is one of the bests? I tend to 20-30% AP because to much AN creates a not full detonateble Charge if you're mix it not well enough (Thats often in fact so). To your Question: AP formed at 5°C is nice but 15°C are better if you want a complete Reaction! When im making AP At lower than 15°C (never higher!!!!) it forms to slowly to get a yield around 80% within 24h! It makes also hard unuseable lumps under 10°C with 30% H2O2 (my Peroxide!). I hope it helpes somewhat! Please say if the Post is to long for reading, next time i make it shorter!

Efraim_barkbit
February 29th, 2004, 05:14 PM
Your post is not too long, but I suggest you buy a new keyboard, the one you use now seems to lack the "enter" key.

Myrol
March 1st, 2004, 10:50 AM
Yes you're right! My original HP-Keyboard was splashed with lot of thick sticky Cacao and we're waiting now more than 10days for a new one! HP promised us to send a new one but they said it needs time......My Mom can't wait so long and buyed one for seven Euros! Cheap but enough for writing! :p

K'Luuppo
March 9th, 2004, 10:17 AM
At last I had a dream about small white crystals in my beaker...
In the dream I filtered them and poured ~0,25l of water on them, while they were in a coffee filter. Then they were put into a beaker with few dl water. Into that beaker I poured ~3 teaspoons of baking soda, stirred quite a lot and then filtered all the crystals out. There was probably soda in the filtration(?) so I poured about half a litre tap water in the filter, for the soda to solve and be gone with water.
Then I had approximately same amount, maybe little less, crystals in the filter than I had when crystals were first filtered. I split the crystals into eight plastic balls, leaving ~1,5-2ccm (many estimates here) into them. Those balls were let to dry for about 20 hours.
One of those balls were taken into the forest besides my house and blew up there with fuse from roman candles (I know it is lame). Results weren't really what I expected: *pop,* maybe what you get if you drop a fist-sized stone from a metre, bottom half of the ball burdened ~20cm into snow and top half never found.
Well, I would have expected at least an commercial firecracker-sized *pop,* even if it were my dream.
The point is, can anyone explain, what I dreamed wrong. My guess would be the soda, moisture and/or lack of pressing.

Cyclonite
March 9th, 2004, 11:32 AM
Im sure its moisture, you should have small piles of AP on newspaper or some other absorbent material until its a free flowing powder. Try shifting it some every once and a while. Also when its neutralized pour rubbing alcohol all over it and squeeze the rest out. This will speed up the drying process.

K'Luuppo
March 15th, 2004, 08:26 AM
I had another dream, and you were right. I put the stuff onto piece of hand towel paper(?) and let it dry for few days, dreaming an experiment each night. Each time it was about 1ccm nonpressed, and the bangs strength (?) increased every time, until I ran out of the chemical.

On friday eve I filtered rest of the AP from my beaker and did all the neutralizations and etc. This time I put it onto piece of newspaper, and the difference in drying time was incredible. First batch dried for five days, but this gave same bang after 24H. The bang was quite similar to firing of .308 rifle, maybe little weaker, but not much.

I put one cracker (~1ccm again) into a corner of a big stone, and it blew ~15cm shard of granite away. I have an crappy video and some pictures about that (isn't it funny how you can record your dreams). Another thing I dreamed was a plastic model plane with little more than 1ccm in its frame. I didn't find any shrapnels of it, it was like it just had decided to disappear leaving an loud bang and quite big crater into soft snow behind. Is this normal power of AP?

Sonny Jim
March 15th, 2004, 01:48 PM
I hope new people to AP will find this helpful:

http://angry_jack.tripod.com/apstuff.WMV

I made a little movie with two impact sensetivity tests, and a final detonation of 0.5g of AP contained in a felt pen case. It might help some people get a feel for how properly prepared, neutralised AP behaves. I will not comment on the sensetivity, but will allow you to draw your own conclusions.

Yeah, before you all ask, the 'fuse' is a sparkler. Laugh all you want, but I find them quite reliable. All you need to do is place a little barrier of tape between the sparks produced and the primary. The total retreat time there was bang on 30 seconds. The detonation blew a hole through a plastic calculator backing, so easily enough to cause some nasty damage to the hands!

Myrol
March 17th, 2004, 08:58 AM
Sonny Jim: The Vid is really cool :cool: I watched it sometimes because its a nice fun to see how your Hand-and-the-Hammer plays with the "prepared" Coin! You struck and struck and struck it and PAAMM it went off :D You must really live in America because the Hammer you have looks like solid quality! Here in Germany there often 0815......Thin Woodcylinder and an easy made Metalhead :rolleyes: Arrggh Damnit! They safe the Materials everytime at the wrong Corners :( Thats annoying! America is much better!

MightyQuinn®
April 9th, 2004, 04:44 AM
........ 3% untill you have had high conc, H2O2. The yeilds are amazing its like a slurpie (frozen coke) of AP......

Dream hell.....this is like a nightmare. :eek:

Holy Shit! You got that right! I made my first batch tonight (roughly 50ml Acetone --> 50ml 35% H2O2 and 20ml of 32% Muriatic. After less than an hour I have a thick white slurry in the vessel. I am going up stairs to take a picture of it now. I was not planning on taking any, but this is fucking amazing me.

Considering how dangerous AP is and judging by what I am going to get from this small (for a beginner) batch I can see why people get hurt.

I am more afraid now than ever......I think they call it respect. Not to mention the woody you get when you look in the fridge and see the fruits of research.

There is going to be one LOUD bang at the gun range tomorrow. I wish to get rid of it all post haste. I will document it.

I am going upstairs to be very careful right now.

**Total processing time: Approx. 4 Hours.**

Edit to add images: Here are the links to the full images. (They are full sized images ie.Large! If you have a slow connection, don't click on them.)

http://www.50caliber.net/science/
http://www.50caliber.net/science/slurry1.jpg
http://www.50caliber.net/science/pile_drying_large

Arthis
April 9th, 2004, 09:43 AM
That's cool for you MightyQuinn, but that's not a fuck lot of AP. You're right accidents come from the fact it's easy to make large quantities, and easy to use it without precautions. Though you shouldn't be too scared of the 20 gr dry AP you'll get. In your batch there are no risks, wet AP wouldn't even burn.

And maybe you could scale your pictures down, as there's no need for a 1600*1200 picture of a beaker. That is pretty common.

--------------

Hey the new PDF version is released :). This has been a long time since I had to modify it, but as I'm working far away I didn't have the internet at homr so that was just difficult. For the holidays I updated the whole stuff, better presentation and more accurate information (acids for example).

I still don't have a camera so there aren't pictures so far, but I'll try to add some soon.

Moreover, if someone has the motivation to make an article, about a precise point of AP, like plastification, or whatever, and wants to help me to complete this manual, I would be pleased to insert your article, or ideas. Feel free to give your help.
Btw, if other people got the motivation to prepare such a file on another explosive, it would start a collection of precise, easy-to-use guides everyone would enjoy.

matjaz
April 9th, 2004, 11:04 AM
Nice work.

Fix the second (trimeric) equation with a "3" in front of the water molecule.

I'd really like to believe that the H2O2 concentration just influences the reaction rate, but I really had yields seem to level off low with 12% peroxide after a few days. Couldn't it be something with chemical equilibrium (I'm getting a bit rusty on this)?

BTW, what is the yield you normally get?

Arthis
April 9th, 2004, 11:20 AM
The fact that the reaction works while greatly diluted has made people think there's no difference, compared to PETN, for example, where a little too diluted acid makes the reaction fail. But in fact of course the less water you have the better results. Even if AP is non soluble in water (less than 2 gr per liter), the reaction may not be complete; you need the complete steps of reaction, including the acid catalyst for you to know where the reaction is less efficient while diluted.

I'm making a batch of AP right now just to give an idea of the yield you can get/except, not that I'm a reference, but everyone can give his method/yield for us to compare.

The method I followed is:
100 mL 35% H2O2
80 mL acetone
30 mL 30% H2SO4
(when diluted sulfuric is easier to add)

I put the acid and the H2O2/acetone mix in the freezer, then slowly add the acid, monitoring the temperature for it not to rise.
After each addition I put the beakers back into the freezer.
The acid is added over a period of one hour approximately.
Ho shit I remember I don't have my scale, hmm mybe I'll try to weight it with another one, but it won't be so precise.
Anyway...

MightyQuinn®
April 14th, 2004, 11:46 PM
That's cool for you MightyQuinn, but that's not a fuck lot of AP. ........ Though you shouldn't be too scared of the 20 gr dry AP you'll get. In your batch there are no risks, wet AP wouldn't even burn.

....said the one handed, former pyrotechnic hobbyist.....LOL Couldn't resist! :D

I actually got 48 grams (totally dry) in 2 batches (same proportions) that time. The second batch was left over night in the fridge and had to be removed from the glass with a spatula. It would not pour. My fridge holds at around 33F

I have been busy carrying out tests of its sensitivity in the basement. I have mainly been scattering small lots (.05g to.25g roughly) and tapping repeatedly with a hammer. After a few hits (after the crystals are one layer) I get a nice *bang.* ( I advise hearing protection ;) ) I am deducing from this that I have made very fine crystals which is a good thing. I have lit a few little sprinkles and have gotten nice little fireballs. I have not progressed to anything bigger for now and my trip to the range I was to have was cut short.

I *AM* charging the camcorder for a weekend trip to some distant strip mines :D This is where I can break out the "big" toys without fear of trouble. I am going to make molded AP with smokeless pulled from some old (circa 1953) 8mm ammo and acetone. I may also mix AP with some PVC cement for kicks too…

And maybe you could scale your pictures down, as there's no need for a 1600*1200 picture of a beaker. That is pretty common.

They are that way for a couple of people I know off board....they all have high-speed internet access and like the full sized images. I re-labeled them for dialup users. ;)

As a side question…..can someone tell me if AP is in the slightest hygroscopic?

matjaz
April 15th, 2004, 04:22 AM
But in fact of course the less water you have the better results. Even if AP is non soluble in water (less than 2 gr per liter), the reaction may not be complete; you need the complete steps of reaction, including the acid catalyst for you to know where the reaction is less efficient while diluted.


Huh, it must be my english... what exactly did you mean (from the semicolon on)?

Efraim_barkbit
April 15th, 2004, 06:15 AM
AP is not hygroscopic, not even slightly.

MightyQuinn®
April 18th, 2004, 08:59 PM
I thought I would share the results of me disposing of the AP I made above. I know it’s been covered, but I am trying to contribute information that I gain in my travels.

Yesterday I hit the range with 90 odd grams of very dry AP. I divided it up in the following tests: 6 grams in a film container, then 5 grams in pile struck with shovel and 75+ grams in a 1LB ricotta cheese plastic tub w/ lid. I also had a couple of “crackers” I made from DBSP + AP + acetone to get it all gooey….filled 2 pen caps (Approx. 1g each) and inserted fuses, dried for 4 days then wrapped in electrical tape I left the remaining mixture in a blob on a coffee filter on my work bench to dry….once dry I taped some visco to it and completely coated with tape to avoid premature detonation from fuse sparks.

I will make no excuses, but my dreams could not be documented (audio/visually) yesterday. I will have a couple of basic pictures to add to the report later.

First tests were the little crackers…….all worked…all were kind of uneventful….won’t bother repeating the trouble of dissolving DBSP again, but for party favors in the name of science, they work. I used a fuse for the film vial and got a fairly sharp crack for a report but not really loud.

So then my buddy starts giving me shit about the ‘tiny’ crackers and tells me to give him a pile on the concrete to smack with a hammer…..well he picks up my “spade” handle shovel and I dole him out about a pea-sized amount of AP. He smacks it, but not square, nada….hits it a few more times then just starts to scrape it in to the concrete making small sparks. Well, this causes uproarious laughter as I have been warning my buddies about the amount of danger you are in when handling, transferring, etc.

Newbs reading this pay CLOSE attention to the following. Hindsight dictates that repeating the following would be considered k3vvL

After the laugh-fest, I doled him out a “manly” sized pile I would guess was between 3-5 grams. My buddy hit it with ONE love tap (seemingly) and it went BOOM. My buddy forgot to put his plugs back in after giving me shit and got the full monty of sound. :eek: We were only about 4 feet away.

We all agreed that the detonation was similar in loudness to the .50CAL BMG we had been shooting all day minus the pressure wave you get 30 degrees behind a .50 with a muzzle brake (200+ grains of slow powder). My buddy took a surprising amount of shock to the forward (right) hand holding the shovel and reported tingling and numbness. Upon closer inspection (pictures forthcoming), I noticed that my formerly new (sans lite oxide coating) shovel felt like a 20 year old shovel!! It dented the underside of the shovel blade and was powerful enough to actually loosen the metal on the shovel. The split up the back of a typical shovel had been widened and considerable amount and the rivet is totally loose!! He will NOT be repeating it needles to say.

I walked the 75g tub out to the rail track at 100 yards and set it off the ground with a small chunk of 1.5” cast steel. I placed a 5X7” chunk of the same 1.5” cast steel between the tub and the rail to make a nice solid target to shoot at I hit it with an 8mm bullet and it went BOOM! WAY more powerful that I could have hoped! It was dark out (we were packing up to go) and I saw a slight flash and a few sparks (reminded me of embers floating up from a fire pit)

I walked out to survey the site and my jaw dropped…….the cast steel behind the tub was gone…..I looked all over and all I found was one little piece. You could tell by the clean metal exposed that the 1.5” thick piece of metal SHATTERED! I KNOW the bullet didn’t shatter the steel as it’s MADE to be a target….the AP did it. I am in awe of the power of energetic materials……I WILL be taking more forays to the range as the nicer weather will permit and I will have the cameras rolling.

sevin
August 26th, 2004, 01:01 AM
Question:

Is HCl faster or slower than H2SO4 in making the AP precipitate?

Arthis
August 31st, 2004, 09:00 AM
Sulfuric acid makes a local boiling when a drop falls in the acetone/h2o2 mix, while hydrochloric acid doesn't, so I guess H2SO4 makes the reaction faster...
Guess though, just try by yourself and tell us !

freaky_frank
August 31st, 2004, 06:21 PM
it depends on the concentration.
But in general H2SO4 is a stronger acid, so it will react more heavily...

Cyclonite
September 1st, 2004, 07:34 AM
You really should not add concentrated H2SO4, its causes heat which is undesirable to AP production. I always use HCL as its easier to get, costs less and does not cause as much heat.