Sciencemadness Discussion Board

Where does one begin ?

aga - 24-11-2015 at 12:17

Naturally as a teenager i made gunpowder and substituted KMnO4 for KNO3 once (lost an eyebrow whilst grinding) but that's about it.

Being aware that there is a Vast array of EMs, is there a 'standard' place to start that is relatively safe ?

Without experience of EMs it seems safest to Not just jump in and make some TNT hoping for the best.

Suggestions would be most welcome, along with disposal routes for any products/side products.

[Edited on 24-11-2015 by aga]

underground - 24-11-2015 at 14:33

I started with TATP but you had better to start in my opinion with HMTD. Make only 1 - 2 gr at begining and try to understand its behavour. Then you can move on.

aga - 24-11-2015 at 14:40

Small quantities sounds like an excellent idea.

Thank you.

I'll google TATP using the search term :-

site:sciencemadness.org TATP

No doubt there will be a result or two.

Dornier 335A - 24-11-2015 at 14:41

How can you suggest organic peroxides as a suitable starting point for someone who asks about "relatively safe" energetics?

Pyrotechnic mixtures on the other hand are much more forgiving and involve no side products or dangerous reactions. I can't tell if you are asking about compounds Aga, because in that case, TNT would be a pretty good place to start. The synthesis is a bit complicated but the product is safe to handle at least...

aga - 24-11-2015 at 14:48

Hold on a sec.

One of the docs says they're First adding peroxide to acetone, then adding acid.

I thought acetone and peroxide was pretty much Bad on it's own.

Sounds Advanced to me (i.e. NOT a noob synth).

aga - 24-11-2015 at 14:54

Quote: Originally posted by Dornier 335A  
TNT would be a pretty good place to start. The synthesis is a bit complicated but the product is safe to handle at least...

Really ?

TNT has such a bad rep (in my mind) i imagined it would be a Nasty thing to synth, or dispose of.

Bert - 24-11-2015 at 15:46

Start with making black powder. It's the original propellant, an excellent "first fire" for priming harder to light mixtures- and will be useful for many "follow on" projects. It is more of an engineering and technology/craft project than pure chemistry, but worth your time if you are going to work with EM.

If you go there, perhaps begin with a search on Antoine Lavoisier and his contributions to the manufacture of Potassium nitrate and subsequently black powder... Your description of the sanitary arrangements at your home suggests that you may have to hand materials appropriate to recreate the original saltpeter extraction and purification process.


After that, the road splits. Follow the pyrotechnist's path, learn rocketry, propellants, generation of sound, color and smoke- And build some fireworks. If you're in the Iberian peninsula, fireworks should not be a terrible antagonism to the neighbors, which is always something to keep in mind!

Or: Learn high explosive chemistry and related engineering. Realize that any testing done here may be taken VERY amiss by authorities used to having Basque separatists blowing up their bosses?!

To follow on historically (and to my mind, appropriately for a beginner), learn about Ascani Sobrero and the discovery of nitrocellulose, Alfred Nobel and his work on technology of producing and safely employing nitroglycerin. Research Edward Charles Howard, (the original chemical engineer) and take a side trip into the synthesis of Mercury fulminate, then combine all 3 projects by shooting a batch of gelignite with a traditional Hg fulminate or 80:20 Hg fulminate:KClO3 blasting cap.

If you are still interested, more or less whole in body and not in jail after those beginnings, I can suggest further projects.

underground - 24-11-2015 at 16:52

He said that he has already made some gunpowder so i guess he would like to move on HE. Nitration proccess is not that easy. Peroxides are much easier to make but he must be careful because are primary explosives. You can start with HMTD with only few grams (NO TATP, it is much more sensitive!!). Never burn more than 0,05gr unless you know what you are doing. You need also a digital scale than can weights even the 0.01 of a gram. This is the way i started. Only hexamine, 30%H2O2 and citric acid are needed to make HMTD

[Edited on 25-11-2015 by underground]

KesterDraconis - 24-11-2015 at 17:14

Quote: Originally posted by Bert  

Or: Learn high explosive chemistry and related engineering. Realize that any testing done here may be taken VERY amiss by authorities used to having Basque separatists blowing up their bosses?!

To follow on historically (and to my mind, appropriately for a beginner), learn about Ascani Sobrero and the discovery of nitrocellulose, Alfred Nobel and his work on technology of producing and safely employing nitroglycerin. Research Edward Charles Howard, (the original chemical engineer) and take a side trip into the synthesis of Mercury fulminate, then combine all 3 projects by shooting a batch of gelignite with a traditional Hg fulminate or 80:20 Hg fulminate:KClO3 blasting cap.

If you are still interested, more or less whole in body and not in jail after those beginnings, I can suggest further projects.


This is what I did, and to some degree I am not sure if it was the right choice, but every body is different.

My first chemistry experiment was distilling ethyl alcohol from cheap hand sanitizer which I could not get to burn like all the videos online said it should. A few months later I made very simple R-candy (when I realized I could use stoichiometry in real life, everything took off from there). I made gunpowder, flash powder, nitrocellulose, etc.

I read a lot more during the winter months (I could barely be in my lab), learning about the very chemists you mentioned above,

I don't know how I got to high explosives rather than pyrotechnics honestly. I did try a bunch of stuff with it (making my own fountains for my little sisters birthday for example), but it never became my focus for some reason. I think I just found the reactions and physics behind explosions more interesting than those behind sound and color.

Bert - 24-11-2015 at 17:23

I don't suggest organic peroxides to anyone for a learner project, regardless of the ease of obtaining the chemicals and minimal equipment required. I do know that many kids start there these days, and a few of them END right there too. But if you must-

In the sciencemadness library, see Tenney Davis: Chemistry of Powder and Explosives

http://library.sciencemadness.org/library/books/the_chemistr...

Has a lab procedure for HMTD. Be aware, it is incompatible with metals.

Then look through the rest of the book, plenty of lab scale synthesis for EM.

OneEyedPyro - 24-11-2015 at 17:30

In my experience HMTD is less chemically stable and more friction sensitive than TATP.
With that said they're both accidents waiting to happen.

If you're looking to get into HEs you're going to need a primary explosive of some sort, lead azide is probably the best combination of power, safety and ease of synthesis with the main drawbacks being high toxicity and the problem of obtaining NaN₃/PbNO₃.

Nearly all nitro explosives are a good place to start in terms of power and safety, RDX, PETN, ETN, TNP and EGDN are insensitive enough to handle without much worry, the question is what chemicals you have available to you and how involved you want to get.

ETN is very powerful and the synthesis is practically idiot proof. ETN and lead azide would be my two suggestions :D

KesterDraconis - 24-11-2015 at 18:28

Quote: Originally posted by OneEyedPyro  
In my experience HMTD is less chemically stable and more friction sensitive than TATP.
With that said they're both accidents waiting to happen.

If you're looking to get into HEs you're going to need a primary explosive of some sort, lead azide is probably the best combination of power, safety and ease of synthesis with the main drawbacks being high toxicity and the problem of obtaining NaN₃/PbNO₃.

Nearly all nitro explosives are a good place to start in terms of power and safety, RDX, PETN, ETN, TNP and EGDN are insensitive enough to handle without much worry, the question is what chemicals you have available to you and how involved you want to get.

ETN is very powerful and the synthesis is practically idiot proof. ETN and lead azide would be my two suggestions :D


I would almost suggest silver acetylide DS, and definitely ETN or PETN to go along with it, but I would be afraid the lower power of silver acetylide DS and near lack of friction and impact sensitivity would cause people to be less careful around other primaries they encounter.

TheAlchemistPirate - 24-11-2015 at 20:26

I started with nitrocellulose, which was successful. Soon after I attempted to distill nitric acid, but wasn't at all an experienced chemist and failed miserably. After that I attempted to make nitroglycerin, failed (without any explosions, just foaming), then gave up on that. I then successfully made erythritol tetranitrate, but couldn't replicate my success and gave up. This was all around 2 years ago when I was more kewl-ish and didn't understand chemistry much at all.
Over this summer I experimented with black powder and rocketry, and I started a chemistry class this semester. Now I'm restarting my whole journey with EMs with a better mindset. Last week I synthesized nitrocellulose and ETN, though I got nervous and destroyed the ETN because I wasn't completely certain of it's sensitivity :) . I will probably attempt the synthesis again after reading this thread http://www.sciencemadness.org/talk/viewthread.php?tid=13502

[Edited on 25-11-2015 by TheAlchemistPirate]

aga - 25-11-2015 at 00:32

Quote: Originally posted by Bert  
Start with making black powder. It's the original propellant, an excellent "first fire" for priming harder to light mixtures- and will be useful for many "follow on" projects. It is more of an engineering and technology/craft project than pure chemistry, but worth your time if you are going to work with EM.

Having made 'gunpowder' before, that sounds like a great plan.

We used to make small rockets, of which a very small number actually flew.

It would be good to learn how to do it properly.
Quote: Originally posted by Bert  
If you go there, perhaps begin with a search on Antoine Lavoisier and his contributions to the manufacture of Potassium nitrate and subsequently black powder... Your description of the sanitary arrangements at your home suggests that you may have to hand materials appropriate to recreate the original saltpeter extraction and purification process.

Unsavoury Shed Zone.

Home is somewhat different ! (it not being my domain)

Funnily enough there is a bit of an ammonia whiff round the back of the shed ...
Quote: Originally posted by Bert  
After that, the road splits. Follow the pyrotechnist's path, learn rocketry, propellants, generation of sound, color and smoke- And build some fireworks. If you're in the Iberian peninsula, fireworks should not be a terrible antagonism to the neighbors, which is always something to keep in mind!

Or: Learn high explosive chemistry and related engineering. Realize that any testing done here may be taken VERY amiss by authorities used to having Basque separatists blowing up their bosses?!

To follow on historically (and to my mind, appropriately for a beginner), learn about Ascani Sobrero and the discovery of nitrocellulose, Alfred Nobel and his work on technology of producing and safely employing nitroglycerin. Research Edward Charles Howard, (the original chemical engineer) and take a side trip into the synthesis of Mercury fulminate, then combine all 3 projects by shooting a batch of gelignite with a traditional Hg fulminate or 80:20 Hg fulminate:KClO3 blasting cap.

Excellent suggestions Bert.

That sounds like a plan.

I'd rather study and understand the chemistry and processes than just follow a recipe to make something that goes bang.
Quote: Originally posted by Bert  
If you are still interested, more or less whole in body and not in jail after those beginnings, I can suggest further projects.

Losing bodily parts and Jail do seem to be something of a hazard in EM.

Do friendly fireworks-display people allow/assist amateurs by letting them test out their products using a proper display for cover ?

mario840 - 25-11-2015 at 00:54

One advice : HMTD better use citric acid instead sulfuric in reaction and the KEY is to very good wash with NaHCO3 (VERY GOOD !) , if compound is wash from acid is stable (it's always risk but we should always minimizing the risk)

Bert - 25-11-2015 at 02:29
Quote:

Do friendly fireworks-display people allow/assist amateurs by letting them test out their products using a proper display for cover ?


It has happened- I was allowed to do so, a long while back. There are also events for amateurs where everyone brings their own products and shoots them.

http://www.pgi.org/competition/

In USA, there are some aspects of our insurance policy and the department of transportation regulations that make doing so inadvisable now. More likely to have a test fire on our own business property for someone learning shell building.

NeonPulse - 25-11-2015 at 04:21

I began by doing a lot of reading long before I even did my first synthesis, which was NC, with ETN was next and worth the time to get the precursors for it. Reading about Knowing what to expect was helpful but nothing beat the hands on experience....avoid the peroxides though, they have bad reputations for good reasons.

arkoma - 25-11-2015 at 07:05

I got this book from the Florida State Library as a teenager. It's an excellent book.

Attachment: [George_W._Weingart]_Pyrotechnics(BookZZ.org).pdf (1.1MB)
This file has been downloaded 1401 times

*edit* Weingarts "Dictionary and Manual" is excellent, too, but too big to attach

[Edited on 11-25-2015 by arkoma]

deltaH - 25-11-2015 at 11:40

Please do not work with organic peroxides. Black powder, then nitrocellulose, as a basic introduction to carrying out a nitration, is a good start.

DubaiAmateurRocketry - 25-11-2015 at 11:50

The post above me sounds good. Organic peroxides are not to play with at all, its just too irresponsible for yourself, future self, and your family, if something goes wrong.

aga - 25-11-2015 at 12:10

Thanks for the peroxide advice.

I had read that they are relatively easy to prepare, however i am not interested in a quick Bang.

I'd much rather get acquainted with the chemistry by spending some time with it before diving for the Bang.

Wow !

There are some Big Names in the history of this 'blowing things up' game.

Roger Bacon
Marcus Graecus
Albertus Magnus
Antoine Lavoisier
Andrew Noble
ICI
Lammot du Pont

And that's just the wiki page on gunpowder !

Tseng Kung-Liang
Hasan al-Rammah

are possibly Bigger names, although i had never heard about them before.

deltaH - 26-11-2015 at 02:27

I have a personal soft spot for black powder, if you want to delve into it deeply, there is immense scope and it's such a classic.

I very much enjoyed reading Ulrich Bretscher's pages on it... every syllable! It so riveted me, just look at the loving care and depth he put into the research, fantastic!

http://www.musketeer.ch/blackpowder/bp_menu.html



[Edited on 26-11-2015 by deltaH]

nitro-genes - 28-11-2015 at 03:35

Here too, BP continues to fascinate. :) Nice link you posted there, surprised though blackthorn alder isn't listed there for charcoal, makes one of the fastest I've tried when ballmilled, pressed and finely granulated.

A simple and relatively safe way of getting a feel for what a pressure wave feels like is to add 2 coffeespoons of a fast blackpowder to a 2 L soda bottle, with a fuse through the bottlecap. When really fast blackpowder is used, the effect is similar to an equivalent of flashpowder. Don't use the cheap soda bottles, which are thinner, there is no substitute for the real coke. :D

[Edited on 28-11-2015 by nitro-genes]

Darkstar - 28-11-2015 at 21:38

Quote: Originally posted by aga  
Hold on a sec.

One of the docs says they're First adding peroxide to acetone, then adding acid.

I thought acetone and peroxide was pretty much Bad on it's own.


The reaction is very slow without the acid. Adding the acid catalyzes the reaction by protonating the oxygen on acetone and activating the carbonyl carbon for nucleophilic attack by H2O2.
Quote:
Sounds Advanced to me (i.e. NOT a noob synth).


TATP is just about the least advanced EM synth there is. But like others have said, I wouldn't recommend organic peroxides. If you blow your fingers off, how are we to continue our discourse in the QM thread?

aga - 29-11-2015 at 15:00

TATP is basically too dangerous Darkstar.

Also there is no real Point making it, as i have no immediate need to blow anything up.

I'll start by having a go at making black powder, then try to form 'grains' with an Al machined plate and Al press, mostly to finish off what was started over a quarter of a century ago.

Continuing in the QM/OC thread is Paramount, hence making a 12v ball mill so i can stick it way out in the countryside, in a hole, with a 12v car battery.

Hopefully the soil and sandbags will catch all of the lead balls if it decides to explode, as is it's wont.

OneEyedPyro - 29-11-2015 at 15:45

Typically the milling balls aren't launched with much velocity when ball mills explode.

Besides, you can mill the charcoal/sulfur separately from the KNO₃ then diaper it together if you're really worried about it.

aga - 29-11-2015 at 15:53

It's One tiny (3L ?) mill
https://www.sciencemadness.org/whisper/viewthread.php?tid=61...

I'm not overly keen on Cleaning, so the charcoal will get milled first, then the S and KNO3 will be added, so all milled together.

With water at some point.

Not sure When that should be.

[Edited on 29-11-2015 by aga]

NedsHead - 29-11-2015 at 17:52

Personally I would mill the Sulphur first unless you purchase it already very finely powdered, my Sulphur comes in the form of sugar sized grains and is always the most difficult to mix intimately, Are there benefits to milling black powder wet? I'm guessing it would be a lot safer while milling but does it have any affect on the end product?

TheAlchemistPirate - 29-11-2015 at 19:34

I believe a small amount of water(VERY SMALL!) is tolerable when ball milling, the advantage being that it is somewhat safer. With too much water, I think the powder starts clumping together and doesn't mix well at all. Of course there are many different methods of making BP so to say whether water is detrimental (in whatever part of the process) or not depends on the method.

OneEyedPyro - 29-11-2015 at 22:08

Quote: Originally posted by TheAlchemistPirate  
I believe a small amount of water(VERY SMALL!) is tolerable when ball milling, the advantage being that it is somewhat safer. With too much water, I think the powder starts clumping together and doesn't mix well at all. Of course there are many different methods of making BP so to say whether water is detrimental (in whatever part of the process) or not depends on the method.


In my experience it mills down to an even consistancy almost regardless of how much water is added, the real problem with adding water is that upon drying crystals form changing the burn characteristics for the worse.

As far as I'm concerned adding water is unnecessarry assuming you're using non-sparking media, a liquid that doesn't dissolve the KNO₃ would be much better than water.

aga - 30-11-2015 at 08:01

From what i;ve read, producing 'grains' seems to be the objective, so once milled & mixed with a tiny amount of water sprayed in, i think i'll try to squeeze it through an aluminium plate with lots of holes drilled in it, a bit like a potato 'ricer'.

After drying (?) these strings, the process appears to be to tumble them together to get them to break into bits and rub together to get a more 'round' shape.

The water should get some of the KNO3 to dissolve slightly and coat the S and C particles, helping keep the grain in shape.

KesterDraconis - 30-11-2015 at 09:48

Quote: Originally posted by aga  
From what i;ve read, producing 'grains' seems to be the objective, so once milled & mixed with a tiny amount of water sprayed in, i think i'll try to squeeze it through an aluminium plate with lots of holes drilled in it, a bit like a potato 'ricer'.

After drying (?) these strings, the process appears to be to tumble them together to get them to break into bits and rub together to get a more 'round' shape.

The water should get some of the KNO3 to dissolve slightly and coat the S and C particles, helping keep the grain in shape.


I personally mix all of my sulfur and charcoal together in a ball mill. I make a solution of KNO3 that is very saturated, then mix in the sulfur and charcoal. I then add a little alcohol and cool the mix.

I can then dry it or add more alcohol to get the mixture to a consistency at which I can press/rub it over a mesh of wires (I use an old window screen actually) and this creates little grains of black powder. I catch them in a big plastic bucket under the screen, and then dry it in the sun.

I find it burns rather well, vanishing quite quickly in a puff of smoke.

[Edited on 30-11-2015 by KesterDraconis]

[Edited on 30-11-2015 by KesterDraconis]

aga - 30-11-2015 at 11:21

Quote: Originally posted by KesterDraconis  
consistency at which I can press/rub it over a mesh of wires (I use an old window screen actually) and this creates little grains of black powder. I catch them in a big plastic bucket under the screen, and then dry it in the sun.

I find it burns rather well, vanishing quite quickly in a puff of smoke.

That sounds like an excellent plan.

Saves a lot of drilling, and my original notion of pressing the 'paste' through the holy Al sheet using a hydraulic car jack was too worrying to attempt : the sheer pressure could cause localised heating, possibly sufficiently strong to cause ignition.

Plastic mesh is a great idea.

Can easily get different mesh sizes too, so cheap and versatile.

I like it.

TheAlchemistPirate - 30-11-2015 at 12:38

Remember that adding binders like dextrin make Corning easier and makes the grains much stronger

aga - 30-11-2015 at 12:41

Binders ?

Sounds like i need to complete step #1 first before i'll even know what difference a binder makes to shape/burn rate.

Presumably the addition of a 4th (or more) ingredient alters the chemistry ?

TheAlchemistPirate - 30-11-2015 at 16:14

The more fuels you add, the more oxidizer you should add. Usually, only 1-2% of the mixture should be dextrin. IIRC if you include dextrin add 2-3% more oxidizer.

PHILOU Zrealone - 3-12-2015 at 12:36

I used 11000 rpm electric coffee grinder for my KNO3 (or KClO3) one one side and C, S (and CaCO3 in the case of KClO3 black powder) on the other side; then I mix oxydiser and fuel (+ stabilizer).

You can have plenty of fun with the following, it is good to go that way chronologically:
-Nitrate suggar
-Black powder
-Chlorate suggar
-Chlorate black powder
-Silver acetylide nitrate complex
-Mercury fulminate
-Nickel nitrate hydrazinate
-Alkyl Amine nitrates and perchlorates
-Ammonals
-Nitronaphtalenes and nitroaromatics alone or with chlorates
-TNB, TNT and TNP
-Nitrocellulose
-Nitric esters (methyl, ethyl, glycol, glycerol, erythritol, nitroisobutan-triol, xylitol, mannitol, sorbitol, ...)

aga - 3-12-2015 at 15:24

Nitrocellulose looks simple.

Then again, i have not made any, so do not know.

An esy way to fix that is readily available !