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Author: Subject: What do you think I should do with my picric acid?
VSEPR_VOID
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[*] posted on 4-8-2018 at 15:49
What do you think I should do with my picric acid?


This was my first real energetic material (aside from hexamine diperchlorate and TAC(II)nitrate. I really want to see something detonate.

Synthesis

4g of a salycilic acid, prepared by the acid-catalyzed hydrolysis of ASA, was slowly added to a beaker containing 30 mL of 70 C (96% drain opener) sulfuric acid. The resulting solution was stirred for 45 minutes at 95 C.

After, the solution was left to cool to 30 C. To it drop wise was added 15 mL of 68% yellow nitric acid. The solution was heated to 95 C for 1 hour and 30 minutes.

The solution was dumped into 250 mL of ice cold water. A yellow precipitate appeared immediately. The solution was filtered and the product collected and stored under water in a plastic screw top conical tube.

Tests: A test samples were wet

small amount placed on hammer and smashed against brick- no result
small amount set on top of Mg turning pile and set on fire- no result
small mount placed between two coins and smashed- no result

What do you guys think I should do with this stuff? Lead picrate is off the table for now. What reactions use picric acid as a starting material?





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[*] posted on 4-8-2018 at 21:11


Tty to make DDNP
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[*] posted on 5-8-2018 at 00:51


I'd make some ammonium picrate, it's more powerful, uses inexpensive ammonia as the precursor and you get significantly more material back than you put in.

None of the metal picrate salts are very good primary explosives, I would just make some other type of primary like SADS to detonate your secondary.


[Edited on 5-8-2018 by OneEyedPyro]
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[*] posted on 5-8-2018 at 06:33


How does one detonate ammonium picrate




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[*] posted on 5-8-2018 at 08:32


Quote: Originally posted by VSEPR_VOID  
How does one detonate ammonium picrate


Ammonium picrate have low sensitivity , was used in grenades, need a primary explosive, mercury fulminate.

I prepare picric acid when I student, from nitric 65%, mercury nitrate and benzene ( OTC) in thats years. That yellow foam dont detonate, deflagrate in fire . Never more repeat .
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[*] posted on 5-8-2018 at 09:06


Turn it back into asprin
Use a nonmetal reducing agent

[Edited on 6-8-2018 by symboom]
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[*] posted on 5-8-2018 at 14:49


I would try to reduce it with zinc/iron in acetic acid but because of the obvious danger of forming metal picrates I wont



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[*] posted on 5-8-2018 at 15:34


A simple blasting cap is all you need to detonate TNP or ammonium picrate.

It seems like you've never dabbled in such things so I'd recommend doing a lot of research before attempting to assemble a cap, there are some little details which may not be obvious that if overlooked could result in missing digits or worse! That applies not only to the design of the cap and methods used to make it but also the manufacture and properties of whatever primary explosive you intend to use.
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[*] posted on 5-8-2018 at 18:40


My first batch of TNP from salicylic acid was unsuccessful.
SA have a difficult being sulfonated because the CO2 group deactivates the molecules by positively charging it, so higher temperatures (95-120 ºC) should be maintained for long periods of time (3-5 hours) in order for the 2 sulfate groups to get attached and form a bond.
The good thing about it is that once you got 3 deactivating groups attached its much more unlikely that any of your nitric acid will decompose into NOs, which is a good thing because NOs are nasty gases. I'd rather deal with Acetone Peroxide than with NOs.

The reason why my batch was unsuccessful was because probably only one sulfate group was attached, so when I added the Nitric Acid most of it decomposed into NOs and was basically wasted. So make sure that you sulfonated your SA properly and add your Nitric Acid slowly.

With TNP you can make all sorts of chemicals. You can make DDNP for your detonator, you can make a booster charge with a lithium based compound (I don't remember what it was).. You will have everything you need, TNP is the main explosive and the precursor to other explosives needed in order to detonate itself.

Attachment: Sulfonation of Salicylic Acid.pdf (606kB)
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Attachment: Nitro-sulfo-salicylic Acid.pdf (438kB)
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Attachment: Salicylic Acid Pages from Von Richter.pdf (212kB)
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Oh, hello! :)

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VSEPR_VOID
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[*] posted on 5-8-2018 at 18:43


I was thinking about making DDNP but I do not have any sodium sulfide. The synthesis I considered required it in order to reduce the TNP.



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[*] posted on 5-8-2018 at 20:57


I have synthesized and expirimented with DDNP, it is a somewhat poor and inconsistent primary explosive on its own unless confined EXTREMELY strongly, it will not detonate easily when ignited by a fuse or E match.
For example, after many failed attempts at getting it to detonate I packed some into a 6mm copper tube of substantial wall thickness and tightly crimped the ends with plyers, the result was a disappointingly small bang with no detonation.
So even if you went through the trouble of making DDNP you probably still wouldn't get the detonation you want without some other primary to kick it off.

Ammonium picrate is quite a good explosive and its formation/precipitation during synthesis is quite pleasant to observe in my opinion.

Perhaps you're more interested in the chemistry involved than the resulting explosion, but if you intend on having any kind of detonation you will likely not achieve it with any picrate based compound.

[Edited on 6-8-2018 by OneEyedPyro]
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[*] posted on 6-8-2018 at 13:11


Can you recommend any primaries? I want to make something detonate. Well I am interested in the chemistry I have never made anything so powerful and want to start somewhere



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[*] posted on 6-8-2018 at 16:01


I accidentally made molten whistle mix a while back, and it was LOUD.
It even dented a steel ruler.
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[*] posted on 7-8-2018 at 03:17


Quote: Originally posted by VSEPR_VOID  
Can you recommend any primaries? I want to make something detonate. Well I am interested in the chemistry I have never made anything so powerful and want to start somewhere


Lead Azide or Mercury Fulminate are easy to do if you have the starting materials.
You probably have the starting materials for TATP but I recommend you stay far away from that. Really.

Picric acid is interesting as an introduction to energetics. It's the kind of synthesis that needs you to understand what's going on to get good yields. Always nice to pick up good habits for later.
Plus, picric acid as an EM is interesting but it has other interesting uses, history etc.
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[*] posted on 7-8-2018 at 03:56


Lead azide is significantly more friction sensitive than MF or TATP, esp. the ß form. Like, stop spreading dangerous myths.

All three, SA.DS, MF and TATP (when fresh and done via the HCl) route are OK. Stay away from un-dextrinated azides and HMTD, though. SA.DS is about the best, though. But be sure to buy leather gloves, kevlar arm protectors (sleeves) and face shiled with glasses (single layer of plastic isn't enough), cheap 0.50 $ ear plugs can protect from about 750 mg, anything above requires ear plugs + ear muffs.

Use multiple filter papers during the filtration step, so you end up with 100 mg of primary explosive per single filter paper. Move the filtesr on large, pre-bent A4 or A3 papesr for drying (1 filter per 1 paper). Dry the SA.DS (if this is your choice) in the dark. Never let your fingers near the primary explosive, touch the corners of the paper.. not the center with the filter paper. TATP is specific in that you need to start filtering about 45 minutes after u've started the reaction (when using 30 % peroxide), otherwise u'll end up with thick slurry that is hard to divide between multiple filters).
Use cotton wrapped wooden rod for all manipulation, leave the fingers 15 cm+ away at all times.
With MF and TATP.. you'll need 1 to 2.5 g per blasting cap. SA.DS... 30 to 350 mg, depending on configuration.

you need to assemble your blasting cap like this:
https://upload.wikimedia.org/wikipedia/commons/3/3e/Blast_mi...

https://commons.wikimedia.org/wiki/File:TATP_blasting_cap_di...

this is an (hastily made) example how the bent papers look like (some have 4× as much powder as they should) and the stick has too thin layer of paper/cottton.. but you get the idea

https://upload.wikimedia.org/wikipedia/commons/3/34/Handling...

[Edited on 7-8-2018 by Rocinante]

[Edited on 7-8-2018 by Rocinante]

[Edited on 7-8-2018 by Rocinante]
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[*] posted on 7-8-2018 at 11:46


I prefer to use compound caps with ~60mg of lightly pressed SADS as the primary and a gram or so of strongly pressed ETN as the base charge. Powerful, reliable and in my opinion not nearly as unnerving to make as a peroxide based cap.

If you have a bit on HNO3, some silver nitrate and an acetylene source you can make SADS.
In my opinion it's among the best primaries for amatuer use.
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[*] posted on 8-8-2018 at 02:16


Only for the amateur with limited access to chemicals, I would say (although I agree that if you factor in the ease of production, it is quite good).

If you can get a nitrITE source (not nitrATE), it is possible to synthesize a LOT of different primaries (complex azide salts, nitrotetrazoles, etc.). Some of these combine high performance and low sensitivity.
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[*] posted on 8-8-2018 at 03:20


Quote: Originally posted by Rocinante  
Lead azide is significantly more friction sensitive than MF or TATP, esp. the ß form. Like, stop spreading dangerous myths.


All three, SA.DS, MF and TATP (when fresh and done via the HCl) route are OK.

I'd never recommend LA without dextrin or PVA. Just assumed is was obvious.
Also, "stop spreading dangerous myths" and a few lines later "TATP is ok" must be a bad joke.

Quote: Originally posted by Rocinante  

With MF and TATP.. you'll need 1 to 2.5 g per blasting cap. SA.DS... 30 to 350 mg, depending on configuration.
]

Or you could follow OneEyedPyro's advice and NOT make a blasting cap with 2.5g of primary !!!

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[*] posted on 8-8-2018 at 15:03


It is well known that TATP (HCl route) is an average primary explosive, this has been tested to death by amateurs and in laboratories. It is very dangerous to recommend lead azide to a novice, what might be obvious to you might not be obvious to him/her... Also, it is known that MF/TATP sometimes fails to DDT properly even at 2 g amounts, so it is reasonable to use 2.5 g if absolute certainity is needed. A 2.5 g MF/TATP charge has the same output as about 1.2 g of ETN/PETN so the size of accidental detonation is the same and proper handling techniques (links) can take care of that - mainly 10 cm of dumb space in your blasting cap + safety bucket. (and the PETN induced fragments will be an order of magnitude worse than the ones generated by 0.4 g/cm^3 TATP.

You're simply playing a smartass because you knew that my description is (needed to be) exhaustive (i.e. a blasting cap without any PETN/ETN) and you act like I was recommending this as a starting point, which obviously isn't true.

[Edited on 8-8-2018 by Rocinante]
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[*] posted on 8-8-2018 at 21:49


Quote: Originally posted by VSEPR_VOID  
Can you recommend any primaries? I want to make something detonate. Well I am interested in the chemistry I have never made anything so powerful and want to start somewhere


Try Rosco Bodine’s synthesis of the Lead picrate/Azide clathrate. If you have NaN3 that is. DDNP is a poor primary in my opinion. There’s a whole host of metallic pirates you could make but Picric Acid is one hell of an explosive by itself as is.
You could try Potassium picrate as part of whistle mixture.




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[*] posted on 9-8-2018 at 05:51


Quote: Originally posted by Rocinante  

It is well known that TATP (HCl route) is an average primary explosive, this has been tested to death by amateurs and in laboratories.


If it is well known why arent you citing sources ?
What IS well known is that TATP kills teens looking for a boom every year in my country. I bet in yours too. It also kills terrorists while making it which is the only thing I like about TATP. And when it doesnt, they blow up when shot at. Kinda cool.
What IS well known is the nickname of that EM: The mother of Satan. It has been known for decades. There must be a reason for that...

What is also well known is that what makes a good, bad or as you say "average" primary is it's ability to initiate a secondary. In that regard, TACP is anything but average.
MF is average / poor. But TATP certainly is not. Against some secondaries it scores pretty much like SA/DS or DLA.


Quote: Originally posted by Rocinante  

It is very dangerous to recommend lead azide to a novice, what might be obvious to you might not be obvious to him/her...


Granted, I always assume that someone interested in the field of EM's is going to spend a lot of time reading, researching, comparing etc. Reading this forum, I guess you could say I should know more. Unfortunately I cant help everyone with risk mitigation.
And this is where our disagreement truly lies: I think it is irresponsible to recommend TATP TO ANYONE. Not just novices. Who needs a primary that sublimates at RT ?
Besides, if you compare synthesis of all three primaries we're discussing here TATP is the most "complex".


Quote: Originally posted by Rocinante  

Also, it is known that MF/TATP sometimes fails to DDT properly even at 2 g amounts, so it is reasonable to use 2.5 g if absolute certainity is needed.


Next time you "it is known" me it'd better be for a Game of Thrones quote ! Because I still dont see any sources and still disagree with you.
And I think you'll find a lot of people on this forum will agree it is anything but "reasonable" to use 2.5g of primary in any device.
This is overkill even for MF based caps. If you need 2.5grams you're doing it wrong. Check how much was used in WW1 ammo on average.



Quote: Originally posted by Rocinante  

A 2.5 g MF/TATP charge has the same output as about 1.2 g of ETN/PETN so the size of accidental detonation is the same and proper handling techniques (links) can take care of that - mainly 10 cm of dumb space in your blasting cap + safety bucket. (and the PETN induced fragments will be an order of magnitude worse than the ones generated by 0.4 g/cm^3 TATP.


A detonator is not made to blow stuff up but to initiate a secondary. Again, what is important is initiating ability and not a generic term like "output".
Looking at your links, I see now where you're getting your ideas from but still see nothing backing up your theory about fragments. There are many documents a lot more interesting out there including in SM library. Most people I've seen here and on Youtube are smart enough to use casings that'll give very few fragments or with low density fragments. Plastic test tubes are fine. If you need to make a booster !
Besides, what we are discussing here are primaries: would you rather have 100mg of LA blowing up in your face (if it comes to that) or 2.5g of TATP ?


Quote: Originally posted by Rocinante  

You're simply playing a smartass because you knew that my description is (needed to be) exhaustive (i.e. a blasting cap without any PETN/ETN) and you act like I was recommending this as a starting point, which obviously isn't true.
[Edited on 8-8-2018 by Rocinante]


Even ignoring the smartass part and that YOU replied to my first post I still dont understand your sentence.

What I do understand is that you recommend using 2.5 grams of a primary in a cap ! That alone disqualifies you from making further suggestions and calling people names.
What I do recommend is that you make your detonator more efficient and not cram more boom-stuff inside !
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[*] posted on 10-8-2018 at 01:59


I'd leave this seriously OT discussion and your ego-fight that I started by pointing out the suggestion of lead azide may be dangerous. As far as the other points, I stated 1 - 2.5 g (maximum) and I already told you that the accidental explosion of 2.5 g MF (energetic equivalent to 800 mg PETN) or 2.5 g of TATP (eq. to 1.3 g of PETN) is the same, i.e. the effect of accidental explosion during loading is eactly the same as from your azide/1 g PETN blasting cap (you are loading the primary after you've loaded the PETN).

Blasting caps used about 1.6 g of MF in a serious copper tube, that's why you might need to go 2.5 g when using very thin metal tubes or plastic. The DDT proces isn't reliable. TATP data have been published for both, small and large crystals of TATP: read the book Primary Explosives by Matyáš or many of his publications http://www.wydawnictwa.ipo.waw.pl/cejem/vol-9-3-2012/Matyas.... . Furthermore, any amateur knows that TATP/MF are about the same and not that dangerous. While pure lead azide, pure silver acetylide or HMTD are obviously very sensitive. And that, for example, recrystalized TATP (large crystals) aren't that very much different from fresh TATP. That alone tells me that you haven't handled these compounds nor did you test them (to rephrase your claims). TATP accidensts happen because it's by far the most available and easiest primary to do (your claim is nonsense) and the youngsters that do it simply bend the filter papers with their fingers, detonating the dry TATP on the other side of the paper or they experience static/friction induced detonations while filling tubes that they hold in their hands. Nothing to do with the specific material. And, oh, these accidents would be 30× more common if they used pure lead azide.
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[*] posted on 10-8-2018 at 11:03


It seems a lifetime ago, but I once explored some of the energetic materials and did synthesize several. Those along with thermit type of energetics.
I have made picric acid and I have made DDNP, along with more.
My advice and this is just from a personal perspective, let it go.

Unless your focus is solely on the energetics, let it go.
If your focus is entirely on the energetics, then carry on but do use good literature to guide you.

I do realize that you may be far more advanced in chemistry than me and that is fine. Just focus and make sure that this is what you wish to do.
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[*] posted on 10-8-2018 at 12:38


@VSEPR_VOID

Picric is immensely versatile! Things possible from picric reaonably OTC are for example (in order of increasing difficulty):

1. Picrate salts and complexes
2. Trinitroaniline
3. DDNP (possibly p-DDNP as well, still planning experiments on this one)
4. Salts of dinitro azido phenols
5. Lead azide/lead picrate clathrates
6. Picrylazide, KDNBF or DATNB/TATNB (all via trinitroaniline)
7. 3-Aminopicric, styphnic/styphnates and KDNP


@joseph6355

Thanks for uploading those articles on the mono sulfonation of salicylic acid and nitration of the sulfonic acids. The exotherm during sulfonation starts noticably and pretty sharply at around 100 C, which is a good indicator. After sulfonation for 2 hours at 120 C, I usually start adding the nitric at a temp between 30-40 C like in the article for mononitration of the sulfonated salicylic and follow the exotherm and decarboxylation as indicator to increasingly higher temperatures until around 85-90 C is reached for the last addition of nitric. Even with the nitric additions starting at 30-40C instead of around 100C, most of the NOx is still produced during the final additions though (and watering down after the reaction for that matter!!!).

@Rocinante

In the book on explosives by Meyer and Kohler, TATP and lead azide are listed as being equal in friction sensitivity at 0.1 N IIRC, this is how I remembered it at least. The paper by Matyáš et al. apparently indeed shows a much lower friction sensitivity of TATP compared to lead azide. The presence of sulfuric impurities may be a big factor here, though beware...the only conclusion that can reasonably be drawn from this is that the friction sensitivity of TATP depends GREATLY on how it is synthesized. Similar to lead azide I hear you say, well yes...but these factors have been much better documented than for TATP. Friction sensitivity is often determined by crystal shape, which is a non-constant for TATP, which sublimates at room temperature. Organic peroxides like MEKP being used as radical initiators, I find it hard to believe TATP to be as chemically stable as lead azide as well. Nothing is documented on possible incompatibilities for example... the influence of transition metal impurities present in almost all hardware store available acids, compatibility with metal caps, or compatibility with secondaries. So no "in depth" documented literature available besides the one posted, yet you speak of "knowing" and reverse the argument by saying we should test it ourself. So how can you make these claims...because you gave it a loose whack with a hammer yourself?

IMO, the real danger of TATP lies in that it is easy to make in large quantities and the other being that lighting 0.5 gram of TATP without confinement will make you go " Ahhh, look at that cute little flame and little poop noise"...while the slightest hint of confinement for that same 0.5 g will ensure detonation and would be strong enough to lose some fingers. Lighting a few miligrams of lead azide will immediately demand a certain respect so to say. Anyway, dealing with 50 mg of Lead azide vs 2.5 grams of TATP is no-brainer. Pressing the primary separate from the basecharge is what I used to do and further reduces risk of premature detonation.

[Edited on 10-8-2018 by nitro-genes]
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[*] posted on 11-8-2018 at 07:25


Yes, as I have written, the sulfuric acid route is very bad - and the acid inclusions can lead to spotaneous detonation at 50°C. The only use of sulfuric acid is for terrorists to avoid the HCl odor when making kilograms of it. Hardware store impurities in acids can affect any compound, so this is not specific to TATP.
I actly saw and ~ tested (hammer induced friction, pencil) about 50 - 100 batches of several grams of TATP (since I was 8 years old :D - so many different sources of chemicals have been used) and I 've never run into problems with unexpected friction sensitivity (including various forms of large crystals). It was/is alway noticeably less sensitive to friction than HMTD, LA or simple silver acetylide. Caution is, of course, required.
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