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Author: Subject: Picric acid: different instructions
S.C. Wack
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[*] posted on 23-6-2012 at 08:25


Doesn't sulfuric acid sulfonate and hydrolyze aspirin? I'd just as soon hydrolyze aspirin with base, acidify, and get nice crunchy salicylic acid, to avoid guessing games, but I'm just a clown on the internet.



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chem77
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[*] posted on 2-7-2012 at 11:26


Well, I tried it again with cool ASA, and I got the exact same results.

I'm pretty sure the trouble is that I'm letting the sulfonation get way too hot. Both times I tried to bring the temperature to 120C and then hold it there, but due to residual warming, it ended up going to about 145C. I figured more heat would be better, but it may have broken something.

Eventually I'll have to try this again without ever letting the temperature climb over 100C. Hopefully then I'll get some nice yellow crystals.
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[*] posted on 2-7-2012 at 14:31


Quote: Originally posted by S.C. Wack  
Doesn't sulfuric acid sulfonate and hydrolyze aspirin? I'd just as soon hydrolyze aspirin with base, acidify, and get nice crunchy salicylic acid, to avoid guessing games, but I'm just a clown on the internet.



Actually I had heard the same thing for some time.




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caterpillar
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[*] posted on 2-7-2012 at 14:37


Is phenol a problem to you? When I was young, this compound could be obtained in a special shop without problems. I never tried to make picric acid from ASA, but the route from phenol is clean and convenient.



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chem77
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[*] posted on 7-7-2012 at 19:37


At this point, I've never found phenol, but I'm a little tired of making this stuff. My only chance to really test it without suspicion (July 4th) has already passed, so I'm not quite as motivated to make it. Someday I'll definitely try this again with lower temperatures, but I'm going to wait a while before finally attempt to defeat this reaction.

In the mean time, I'll try to extract some gold from an old computer in my basement.
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Kalium
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[*] posted on 7-7-2012 at 20:18


Quote: Originally posted by caterpillar  
Is phenol a problem to you? When I was young, this compound could be obtained in a special shop without problems. I never tried to make picric acid from ASA, but the route from phenol is clean and convenient.

It isn't as easy as it used to be. Watch this:
http://www.youtube.com/watch?v=HVFo44JPbMM
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chem77
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[*] posted on 25-6-2013 at 09:20


1 year update:

I finally managed to make picric acid. It turns out that the brown sludge I talked about in my previous posts was the filler in the aspirin pills. I was heating my iso up to make the ASA more soluble and since I didn't want it all to crystallize out in my filter, I just quickly decanted it. This apparently didn't do a good job of separating it because as I later saw, it just turned into a brown sludge ruining everything.

I just wanted to leave my solution here in case anyone else ever runs into this same problem. But, here's my bright yellow picric acid in the step that had gone wrong every time before.

picric _yellow.jpg - 42kB
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Ral123
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[*] posted on 25-6-2013 at 11:36


Great, now detonate it and upload it in YT. Make sure to record well, not just the burning of the fuze, the boom and done.
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chem77
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[*] posted on 30-6-2013 at 12:45


I would, but logic tells me I shouldn't upload videos that might get me labeled as a terrorist.
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Ral123
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[*] posted on 30-6-2013 at 13:47


Haha and what are you doing in this site? You've just publicly announced you're into energetics. You even uploaded a picture. Google gives you 10gb of space for free, how much do you think it would cost the NSA to store some of your data like ip and some pictures and messages? If you would worry about being known with energetics, you better start working like a real T, as stealthy as possible. You can start here:
http://www.businessinsider.com/nsa-prism-keywords-for-domest...
otherwise video, or it didn't happen
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papaya
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[*] posted on 24-11-2013 at 15:37


A question to those here, who intimately knows the subject : is this procedure here
http://www.sciencemadness.org/talk/viewthread.php?tid=4457&a...

the "best" one known here (derived during these years) in terms of yields, quality and economy of reagents, or some else writing exists?
Because I see it uses too much sulfuric acid compared to the double excess of what is theoretically needed, or there are other things that don't let to use any less? Same about the nitrate quantity...
Multiple picric acid threads (though this is longest) make it difficult to differentiate initial experimental results from the final "recipe" (I even think the final optimized version deserves an article in prepublications, from author of course :D ), so I wanted someone to confirm that what I found is what is thought to be the best so far. Thanks.
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papaya
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[*] posted on 25-11-2013 at 09:03


Great, now nobody is going to confess that ever made this compound.. Then I will show you one small trick on picric acid purity testing: I went through this thread and people offer to blow with hammer and listen carefully for echo, or to look at color and guess - not against it, but to my opinion the best test would be melting point determination (pure picric acid melts at 122.5 °C according to wiki). Only problem for amateur here is that this must be done accurately and with precision thermometer use... unless you know how to overcome that part! A possible solution that came to my mind I wanted to share is to use another PURE substance side by side with the sample under question which melts at nearly the same temperature and which is easy to come by - meet benzoic acid with m.p. of 122.41 °C. Seems easy, isn't it?
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plante1999
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[*] posted on 25-11-2013 at 09:08


Lambdasyn got some good preparation for it.

Many, many people mde some, not many will tell tough.




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papaya
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[*] posted on 25-11-2013 at 09:19


I saw lambdasyn - waste of acids, as well as strange differences in quantities if different precursors are use - compare ASA / H2SO4 with others (sooo much sulfuric) - it seems these "recipes" are collected from different origins there. The problem is that one anyway will obtain SOME picric even with wide variations of reagent quantities, but this has no value unless the synthesis gets "optimized" in some sense (quality, safety, economy, etc.). I even think that if one comes with a good polished procedure where only dilute nitric acid is used it will be substantial contribution (I read industry loves strong acids mostly beacuse they are less corrosive to equipment, not that it's impossible).
I think there are people here with enough (first hand) experience who could answer my original question, I hope so.
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[*] posted on 28-11-2013 at 03:22


I made TNP many times. Procedure is described at this very tread. Phenol, KNO3 (or NaNO3) and H2SO4. Simple and convenient (if you can get phenol). Very few NOx was generated. I suspect, that preparation, based on diluted HNO3, gives very dirty product.



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papaya
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[*] posted on 28-11-2013 at 11:41


Quote: Originally posted by caterpillar  
Procedure is described at this very tread.

Could you point out which one exactly gave best results for you (among many pages)? Also phenol or ASA ? Cannot ASA replace the phenol ONLY by recalculating for different molecular weight?
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[*] posted on 28-11-2013 at 12:17


IIRC, Rosco Bodine's TNP from ASA in this thread used to be regarded as optimized and easily reproducable. Moniter temps well with additions. Using KNO<sub>3</sub> make the workup harder so stick with sodium nitrate.



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[*] posted on 28-11-2013 at 12:35


Quote: Originally posted by Bot0nist  
IIRC, Rosco Bodine's TNP from ASA in this thread used to be regarded as optimized and easily reproducable. Moniter temps well with additions. Using KNO<sub>3</sub> make the workup harder so stick with sodium nitrate.

Agree on NaNO3, but do you speak about Rosco's procedure I pointed out above (actually it's in other thread) or to which one you refer ? (put the link). Sorry, this type of asking questions (myself) appears stupid already.
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[*] posted on 28-11-2013 at 14:58


Im on a phone so i cant do the legwork for you right now. If your interested in TNP, please read this whole thread. In it rosco posts a very detialed writeup using ASA. You will know it when you see it. And then go find his and hennigs work on BASIC lead picrate. Read read read. No spoonfeeding or lazyness for you, since your into EM its a good habit to learn.

[Edited on 28-11-2013 by Bot0nist]

http://www.sciencemadness.org/talk/viewthread.php?tid=4457&a...

If that link doesnt work, UTFSE, like this. :p
http://www.sciencemadness.org/talk/search.php?token=&src...

That writeup needs desperatly to be in the new compendium. Best I have found. That and the work on basic lead picrate...

[Edited on 28-11-2013 by Bot0nist]




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[*] posted on 29-11-2013 at 01:15


Quote: Originally posted by papaya  
Quote: Originally posted by caterpillar  
Procedure is described at this very tread.

Could you point out which one exactly gave best results for you (among many pages)? Also phenol or ASA ? Cannot ASA replace the phenol ONLY by recalculating for different molecular weight?


As BotOnist wrote to you, read, read and read. Page 23 at this very tread. There are two methods- from ASA and from phenol. During conversion of ASA to TNP some parts of ASA will be most likely destroyed, therefore this way will require more HNO3 (KNO3, NaNO3) than the route, starting with phenol. You may read Ledgard's famous book as well.




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papaya
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[*] posted on 29-11-2013 at 07:59


Thanks for the answers, and yes, I've read whole thread before asking.
In Rosco's method when you calculate molar ratios, result is ASA:H2SO4:NaNO3 = 1 : 12.37 : 3.815 !
Well some excess of nitrate I understand, but more than 12 moles of sulfuric to ASA ? No doubt it will work well, but what if for example it can be done equally well just with 6-7 moles only, any experience ?
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[*] posted on 29-11-2013 at 09:24


I'm seriously deceived by papaya attitude. There is reasons to use more sulphuric acid, we don't waste reagent for fun. If we don't the decarboxilation and acetate group degradation will not go well, and will become an hard, impossible to stir mass.

It seams to me that if you want to have a perfect "receipe" that work for all substrate using the less reagents possible without changing anything with different substrate, you want to make very large quantity of it, which is both agains the law mostly everywhere and has not link with amateur chemistry what so ever.

I'm definetly not agreeing on the way the last few posts worked.




I never asked for this.
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[*] posted on 29-11-2013 at 11:25


According to dear Jared Ledgard (procedure 18-04B) ASA 50 gr, H2SO4 350, KNO3 115 (or NaNO3 95). Now I think, that I could take less H2SO4 than I did.



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Ral123
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[*] posted on 29-11-2013 at 11:52


Does anyone know if not separating the isomers will effect the storage stability? I feel like TNP is the most storage stable EM one can make readily. May be more stable would be DNB, but DNB is invalid by itself.
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[*] posted on 29-11-2013 at 12:50


Quote: Originally posted by plante1999  

It seams to me that if you want to have a perfect "receipe" that work for all substrate using the less reagents possible without changing anything with different substrate, you want to make very large quantity of it, which is both agains the law mostly everywhere and has not link with amateur chemistry what so ever.

I'm definetly not agreeing on the way the last few posts worked.


Not really, it's my habit to check procedures myself on paper before I even consider to experiment(or not) and the question I raised is related to chemistry, so please don't speak for me next time or make incorrect deductions. If I ever test this synthesis I will start from salicylic acid instead of ASA, so quantities must be recalculated somehow, I guess equimolar salicylic instead of ASA must be correct amount, unless you take into account that... hydrolysis of ASA CONSUMES water (this may be beneficial), ever thought about it?
Also, where is that Ledgard book, link please ?
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