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Author: Subject: Ancient bottle of picric acid
e.liska
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Ancient bottle of picric acid

Found in my box of ancient dyes. Should I run or what? Can it be safely opened? The box survived mailing with post and other harsh movement, so it should not explode immediately, I hope.

[Edited on 20-10-2017 by e.liska]
hissingnoise
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 Quote: Should I run or what?

The conventional wisdom would suggest that you treat your find as if it were a fission bomb and first evacuate the entire area to a radius of 3 miles...?

But seriously, aged picric acid may have reacted with the metal bottle-cap to form sensitive picrates?

But if, as it appears, the cap is of glass, their formation is less likely.

Exercise extra care anyway if you want to investigate?

LearnedAmateur
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From Wikipedia:
"Picric acid was the first high explosive nitrated organic compound widely considered suitable to withstand the shock of firing in conventional artillery."
So it's not a terribly sensitive explosive, at least that concern is out of the way. I'd be more worried about the possible presence of metal picrate contaminants - do you know the origin of your sample? In any case, I wouldn't open the bottle for any reason, since some compounds can be detonated by friction, and I suggest looking for explosive disposal specialists (make sure you get that grenade, erm, bottle marked as well). As I like to live by, treat any unknown as if it will try to kill you.

In chemistry, sometimes the solution is the problem.

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SWIM
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It's hard to tell how big, and how full, that bottle is from the picture.

If you could give a better Idea how much seems to be in there it might help people here form an opinion as to what you should do.

Not that I'm saying LearnedAmateur is wrong. He obviously knows more about this material than I do, and it's great that he's here to lend a learned hand, but if the quantity in there is very small it might change matters about disposal.

For instance if it's only a gram or less it might be more reasonable to deal with it yourself than if you've got 100grams in there.

unionised
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Do not try to open it.

Picric acid is usually stored slightly damp- to make sure it's not going to explode.

However that means thee is always a little of the solution in the bottle. That gets into the gap between the stopper and the bottle- where, over the years, it dries out.

Then, when someone tries to open the bottle, that's enough to initiate the explosion in the stuff caught up in the joint.
It's not usually a big explosion, but the flying broken glass isn't a nice thing to have.

The best approach is probably to build a bonfire round it somewhere in the middle of nowhere, light it and walk away.

Another "solution" I have heard is to carefully turn it upside down and put it in a bucket of water.
Leave it for a few months so the water can soak into the joint, then very carefully open it- chainmail gloves are still recommended.

e.liska
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It contains about 40 ml of perfectly dry and loose crystals. The bottle is all glass. Exact origin unknown, found in a box of microscopy dyes.
JJay
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I know a biologist who ran into the same thing not long ago. I know he was considering calling the bomb squad but I think he disposed of it himself. I'll probably talk to him tomorrow and will ask what protocols he used.

JJay
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He said he called a chemistry professor, who picked it up placed it in some kind of steel container and took it away for disposal....

BromicAcid
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Since it's not in metal it might be worth the attempt. Take the whole bottle and submerge in water for a week then inspect. See if water wormed its way in there, if its wet and the ground glass looks wet it might be worth a go. You could also break the bottle carefully to avoid the issue with friction. Or maybe setup a deadfall to yank the stopper out remotely. The actual chance of something going bad is low, but it does exist, you just need to do what you can to minimize it further.

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Bert
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(NOTE: This is not to be taken as instructions on dealing with orphaned old trinitrophenol samples...)

From The Caseformer, Volume 4, Issue 1

 Quote: THE YELLOW PERIL “How come?” asked Leo, “It’s the best yellow dye we got.” “Supposed to be too dangerous. Damn near as bad as TNT, extremely toxic, and inhalable,” said the As- sistant Director. “OK, I’ll take care of it.” Click. Leo, a World War II vet who had shot a lot of TNT and had b een shot at by a lot of weapons ranging from 8 to 88 mm, did not hear the Assis- tant Director start to say that the Chemist would come out and take charge. Instead, Leo walked over to the cabinet, took the little brown bottle of picric acid, dumped the remaining 41 grams slowly into the toilet, and flushed the crystals into the septic tank. His thoughts flew back to the early 50's when he and some other young refuge biologists had trapped and dyed the plump drake canvasbacks on their com- munal “headquarters ponds” on the Saskatchewan breeding grounds, and then followed and recorded the movements of the yellow-backed birds for sci- ence. He had used it by the kilogram, but that was decades ago. He even dimly recalled buying small bottles of the acid at the local drugstore when he and the other 6th graders sprinkled it on their combs to dye their hair as a school prank. “H-h-h-he w-w-w-what?” said Ken the Chemist, trembling as he fondled a copy of the recent Emer- gency Safety Order (EMS) that had been entrusted to him by the Assistant Director. The EMS out- lined with terrible forebodings all the horrible prop- erties of picric acid. “My God, he could easily have been killed! Now I have to try and decontaminate the place.” “Do your best,” said the Assistant Director, his voice suitably grave. “Yes sir. By the way, I changed the locks on the chemistry laboratory again. Did you know the ter- rorists have orders to steal any chemical that can be potentially useful to their cause?” “No, but you could be right,” said the Assistant Director, rolling his eyes and already enjoying the thought of telling the Director about the latest ter- rorist plot that threatened the Federal Service out in . this remote section of Wyoming. “Evacuate the laboratory,” said the Chemist. “Leo, I want you to put on this smoke mask and face shield and this bunker gear that I got on loan from the Fire Department. Put your back to the toilet and flush it 50 times.” “Fuck you,” laughed Leo, his eyes twinkling in mirth. “The dye is gone, you dumb shit. You want me to dig open the septic tank so you can snorkel for any undissolved crystals? I’ve got some fusees in my truck that you can use to light up the bottom.” Sensing a lack of cooperation and blatant disre- gard for the strict protocols used to handle Class AAA Schedule 3.7.9.2 hyperexplosive compounds, the Chemist had to settle for five minutes by himself in the toilet with a leaky garden hose. But he took pleasure in the fact that he could now report that his concern for the safety of his fellow workers had forced him to tackle the ticklish job singlehandedly. The next day was even worse. Another 14 grams of the deadly stuff had been found in a small met- al tin in another building. But this time the Chemist’s worst fears were realized.. . container corrosion! He carefully approached the container again, making sure he did not touch it. Yes, there it was, a telltale rust spot near the lid. The Chemist immediately locked the door of the building and flagged it all around with police tape. A quick phone call to the Assis- tant Director started the process. The AD immedi- ately called the Director, explained the fearsome sit- uation and got approval. He called the State Bomb Squad. The heavy truck rolled out of the outskirts of the State Capitol. Fred, Leader of the Bomb Disposal Unit, and Charlie, the Assistant Unit Leader, had never dealt with picric acid before. In fact, this was only their third call to duty. The first had been out in the oil fields, where a rancher had found what remained of the wrapper of a quarter pound of RDX after the prairie dogs had chewed it up. The small charge had been rendered useless five years ago by the wheels of a seismic crew truck. The other inci- dent was the disposal of five 2-inch firecrackers that had been found in the glove compartment of a car full of teenagers last Fourth of July. But, after talking with the Chemist, Fred and Charlie were ap- prehensive. “Got it!” said Fred as he spoke in hushed tones into his specially grounded lapel microphone that re- layed the message to Charlie outside the building and also recorded it for later analysis by the Bomb Research Division. Despite the clumsy gloves, Fred manipulated the remotely-controlled tongs and set the deadly canister into the steel mesh bag on the radio-controlled cart. “Ready with Sandy?” “Yup.” said Charlie, standing alongside the S-ton bomb container with walls of sand that would receive the canister and its sinister contents. Everything worked with precision. Fred drove the cart out to the truck, then used the special tongs to pick up the canister and deftly set it on the bottom of Sandy Charlie peered through the bullet-proof window of the truck as he manipulated the controls and gently lowered the ponderous lid and closed Sandy for the trip ahead. The Chemist got on the phone and told Maintenance that the coast was clear and they could tear down the police tape and tell the employees to go back to work. “Now what shall we do with it?” said Fred. “Best to not let it leave Federal property,” said the Chemist. “Liability in case of an accident.” “Then let’s do it in the pit at the dumpground.” said Charlie. “Great idea, Charlie, but what about the media?” said the Assistant Director. “This is certainly worth a story.” “Yeah, give them a call.” said the Director. “You got State Radio on the line, Charlie?” “Yup.” Because of the heavy bomb suit and lead boots, Fred almost fell over the piles of slightly used type- writers, computers, microscopes, and other laborato- ry equipment that lay at the bottom of the pit await- ing burial. H e gingerly placed the canister on the back of an old Hasselblad camera that lay lens down in the mud at the bottom of the pit. “OK, place the charge.” said Fred. Now it was Charlie’s turn. He carefully placed the capped, one- ounce charge of TNT next to the little can and del- icately poured sand over both items. Then, ever so gently, he ran the lo-ft. length of dynamite fuse up to the top of the pit where Fred weighted the end down with a rock. . “Fire in the hole!” cried Fred as he pulled the ig- nitor ring and the bickford fuse bubbled to life. What seemed like hours was only 51 minutes to the Unit crew, the Chemist, the Assistant Director, the reporter, and his crew from KSMA-TV, as they watched from the top of a hill about 600 yards away from ground zero. With a SPLUT sound the charge detonated and the TV crew caught the top of the tiny puff of black smoke as it briefly rose from the pit. Fred missed it with the 1000 mm lens on his armored Nikon, but the Assistant Director thought he might have got it with his handheld wide-angle. “Wasn’t very loud.” said the Assistant Director. “Hey, these guys know what they’re doing.” said the Chemist. “They had it perfect barricaded.” “Did you get all our names?” said the Director to the reporter. On the long drive back to the Capitol, Fred said, “Always feels good to save lives, don’t it Charlie?” “YUp,” said Charlie, as he chest heaved with pride. KSMA aired the disposal project during a special feature called “The Environment.. . to Protect and Serve” that was picked up and played on some oth- er stations, some out-of-state. Several stations saved the story and were able to tie it into their anti-fire- works material scheduled to be aired during the up- coming Fourth of July. The Chemist appreciated the $500 Special Achieve- ment Award he received for his herculean efforts, but absolutely cherished the framed Certificate of Special Achievement that now hung above his desk. His chances for promotion or lateral transfer to a position of higher authority were now greatly en- hanced. The Director and Assistant Director chortled over the incident and the good publicity. “Sure it cost$17,457, but it was worth every pen- ny,” said the Director. “Really put us on the map.” “Damn right,” said the Assistant Director. “No trou- ble justifying our new budget request now!” - HORST KNALLKORPER

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3. Mention anything you have learned from your target.
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ave369
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I think making some long lever contraption to yank the stopper out remotely is the best bet.

Smells like ammonia....
phlogiston
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It would be easier to just smash the bottle remotely.

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SWIM
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I have received some second-hand information that leads me to believe the OP's problem has been resolved in a safe and cautious way.

e.liska
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Incinerated successfully.
Quaff
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In "the Chemistry of Powder and Explosives" by Tenney Davis of MIT, he wrote that dry picric acid is very dangerous, but in the wet state it is relatively safe.

When my wife and I were newlywed we went to an estate sale. Inside the garage on the floor rested several large boxes of chemicals, I'd hit the jackpot ! The first one I pulled out was a 500 gm bottle of Baker's Reagent grade picric acid, dry as a desert. I gently lowered it and instructed all persons in the house to leave immediately. They didn't believe me, so we stopped at the first fire station and explained. Turned out, they cordoned off the whole block and it was on the 6 o'clock news. If I found dry picric acid again, I'd secure the area and call the bomb squad. If I were the last man alive on earth and found it, I'd probably try to see if I could somehow get it wet. But even moving it could be the end of it all real fast.

edit: That was a good example of how knowing about such things can be of benefit to others.

[Edited on 8-11-2017 by Quaff]
Bert
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Tenney Davis was more concerned with picric acid in a production/industrial setting, COPAE was written for the new explosives engineering and chemistry students during the rapid expansion in explosives production and development from WWII. You will note that this was a quite common industrial chemical and lab reagent in many disciplines for decades before and after WWII- With not that much in the way of accidental lab explosions.

The lab storage/use explosive events that are recorded tend to be due to metal contact leading to formation of primary explosive salts. Water helps with that process... Then an institution or lab lets such a contaminated container sit around for years and dry out, or sufficient solution migrates into the closure and drys out there, to the detriment of whoever next opens that container. Of course, it notably happened in high school chemistry labs, where odd things may sit around on the back shelf forever.

I have handled dry, reasonably pure picric acid. Carefully, mind you. One of my teachers in pyrotechny kept a supply for making old fashioned Potassium picrate/Potassium nitrate pyrotechnic whistles. Interesting devices, they whistled quite shrill and loud, leaving trails of dark smoke in the air. Yes, the mixture was hydraulically dry pressed into tubes in his shop.

Some were said to have perished due to thoughtlessly using equipment on hand for making hand rammed black powder motors to make whistles, which included a heavy Lead base for the tooling... With plenty of picric dust to coat that Lead block flying out of the tubes as the drifts were hammered down.

I had read the bit in Lancaster about English fireworks production workers of old disliking the job of whistle making due to the bitter taste it left in their mouths from dust that escaped during the loading process. So I asked if I could taste a tiny crystal. He looked at me a bit askance and said I could do that, and I did. Yeach. Spat yellow for a while and can report lager did not quickly wash the taste away. Those present laughed at me a bit, then discussed the tradition of chemists tasting and smelling new compounds they made-

[Edited on 8-11-2017 by Bert]

Rapopart’s Rules for critical commentary:

1. Attempt to re-express your target’s position so clearly, vividly and fairly that your target says: “Thanks, I wish I’d thought of putting it that way.”
2. List any points of agreement (especially if they are not matters of general or widespread agreement).
3. Mention anything you have learned from your target.
4. Only then are you permitted to say so much as a word of rebuttal or criticism.

Anatol Rapoport was a Russian-born American mathematical psychologist (1911-2007).

 Sciencemadness Discussion Board » Fundamentals » Beginnings » Ancient bottle of picric acid Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues