Tuesday, October 25, 2016

Dickinson State professor was making and grinding acetone peroxide?

A couple of days ago, there was a brief conversation on Twitter (started by Daniel Horowitz) about a reported explosion at Dickinson State University on October 4. Here's a brief report by Kalsey Stults in the West Fargo Pioneer:
DICKINSON, N.D.—Students at Dickinson State University were back to an unceremonious Wednesday, Oct. 5, 24 hours after Murphy Hall was evacuated and a faculty member was injured in a classroom explosion Tuesday afternoon. 
Chemistry professor Ken Pierce was preparing a classroom demonstration around 3:30 p.m. when an incident occurred resulting in a small explosion. [snip] 
Jack Schulz, DSU's director of security and emergency management, said the classroom showed visible signs of an explosion with parts of the counter being damaged, and blood and debris around the room. Schulz said the second floor of the building was evacuated within minutes and someone aided in helping Pierce with his injuries and giving first aid until paramedics arrived on scene. 
"There was a young lady that had some type of medical training either in the room or in the area, and she provided a little bit of first aid on him (Pierce)," Schulz said.
The professor's hands were bandaged before he was taken by ambulance. 
Schulz said the head of the chemistry department notified him immediately that there was no dangerous airborne chemicals to be concerned about in the lab and there was no fire from the explosion. Schulz said knowing that there was no immediate danger, it was about making sure students didn't panic, and said the evacuation was calm and orderly.
Yesterday, Ms. Stults (published here in the Grand Forks Herald) mentions this set of details about the incident (emphasis CJ's):
On Oct. 4 at 3:25 p.m. Pierce was conducting a chemistry demonstration in room 206 of Murphy Hall when the demonstration went awry. 
He was demonstrating flash powder—a compound made from hydrogen peroxide and acetone—for five students. After the two compounds were mixed and sat for a couple of hours to dry they then become a powder. 
During the first experiment Pierce noticed a small amount of powder in the mixture, and when he ignited the powder it flashed but the clump of powder combusted—which he thought was unusual but continued. 
He then conducted two more experiments without incident, but before the fourth experiment Pierce noted small clumps of powder in the mixture. 
Pierce then poured in mortar and pestle to grind them up, but when he started to grind the mixture, it exploded. 
Pierce suffered non-life threatening injuries and was transported to CHI St. Alexius Hospital in Dickinson before being transferred to Bismarck for surgery... 
...Pierce was wearing personal protective equipment including goggles and students had been tested on safety protocol at the beginning of the semester.
So I am open to the possibility that the details of this experiment were incorrectly reported by university officials. However, if the details are accurate (and I have no reason to doubt that they were), here's what we know:
  • Professor Pierce was preparing something that sounds awfully like acetone peroxide. Couple of things:  
    • Acetone peroxide is famously touchy stuff. 
    • I was under the impression that acetone peroxide preparations included some acid? Apparently not needed. 
  • Professor Pierce was wearing some amount of PPE. 
  • The acetone peroxide mixture exploded when ground in a mortar and pestle. (Not a surprise there.) 
A few questions remain: 
  • Was there an appropriate risk assessment done in regards to Professor Pierce's PPE? 
  • How close or far away were the students from the bench when this happened? 
  • What was the scale of the acetone peroxide experiment? 
  • Were there any records of the amounts used for the experiment? 
In general, I think that pops and bangs are an integral part of chemistry demonstrations. That said, the intentional (or unintentional?) preparation of a primary explosive seems unusual at best. 

16 comments:

  1. Grinding the solid indicates that he probably did no risk assessment at all. Hopefully he at least kept a notebook while preparing, but being someone in a similar position, I can't say I'm optimistic.

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  2. And apparently he is a full professor. Scary.

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  3. Not heard it called flash powder before, Wikipedia suggests these are usually Al+perchlorate. Any proper risk assessment would have said no. He should have kept the powder and washed the clumps away.Burnt his fingers in more ways than one.

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  4. This has some echoes of the Texas Tech incident. Acetone peroxide synthesis does use a mineral acid as catalyst, and the product (dimeric, trimeric) depends on the reaction conditions (rate of addition, temperature). So visible heterogeneity in his product could indicate poor reaction control. The different acetone peroxide structures have different sensitivities to shock and foul language; but none of them would take being ground in a mortar and pestle. Wishing Prof. Pierce a speedy recovery. I hope his students are both inspired and cautioned as a result of this demonstration.

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  5. acetonperoxide in powder form produces impressive flashes of cold yellow flame, gasoline fireball like (they used benzoyl peroxide in Hollywood for gasoline exploding car effects) . In clumpy form or in larger crystals the deflagration turns to detonation. Any space constraint, or moderate friction/impact and goes boom too.

    I think calling it "flash powder" is little coy, they don't want newspapers to print that the prof was making TATP, substance used by islamists in suicide wests. Also, little acid is need to catalyze the reaction, but just because they don't mention it in newspaper it does not mean they did not add few drops of acid.

    I think the professor just ended his career, will serve time, and the school will get sued for considerable damages. The thing with acetonperoxide is that unlike nitrogen triiodide it looks so innocuous it lulls you into a false sense of confidence - it even smells nice, and most of the times it behaves nicely except when it suddenly does not (i.e. when it starts decomposing on storage by traces of acid or recrystallizes by sublimation into large needles (over few days), if the material turn out as clumps rather than powder, or if Mars aligns with Jupiter on Tuesday afternoon.

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    1. I agree calling it "flash powder" was hiding the football.

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    2. Jesus, you sound like you know and hate the dude. How is this a crime? There was exactly one injury and it was him. I don't think an instructor should be drawn and quartered every time they get singed doing a demo. It happens. I'd never make TATP just as I'd never do the Rainbow, but it's not a crime to get injured doing a demo. I burned some holes in a shirt the other week when a clay dish of powdered zinc and sulfur reignited. Is there a safer way to demo 2 elements forming a compound? Not really. Shit happens so let's all wear PPE, use blast shields, but not get chemophobic here!

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    3. I think the current laws are excessive (post 9/11) but the dude was not authorized to make and teach how to make a primary explosive and he lacked the right kind of equipment.

      I heard of a senior grad student kicked out of a PhD program because he "borrowed" some really old sodium metal (that was too crusty to use for solvent stills), and with a couple of junior chemistry students he was quenching it in a bucket of water, in a garage of his house. There was no mishap but unfortunately a video of this educational experiment was uploaded to Youtube. He ended up arrested for theft & other charges, had to post bail, the university decided to make an example of him, zero tolerance stuff (because the university was afraid someone might sue university in a similar incident in the future). Eventually his old advisor got him spot at another research group at another university, but it cost the guy several years of total synthesis research counted towards his PhD.

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    4. I'm not even sure what the laws are, I'm no lawyer, just a humble teacher. Basically, if I want to blow something up (like, say, sodium in water), I tell the school cop before I do it. Sometimes he'll come outside to watch. As far as I can tell, he is the 'law' - I wouldn't know who else to report to.

      I refuse to accept that I need 'authorization' to teach about anything - we do have free speech in this country. And as far as authorization to acquire and use dangerous explosives, I'm pretty sure this is something that varies by jurisdiction and changes all the time. My home state, a couple years ago, managed to somehow legalize ALL recreational explosives - the 4th of July was very interesting when I last visited. It was a night to calm the dogs and keep running a hose onto the roof. Maybe next time the authorities will have managed to put a lid on it. I doubt it.

      I would expect that stealing sodium is always a crime as well as a violation of University policy. Misuse of Federal grant money too! As far as liability, I did a bit of research on it some time back and I do see where this grad student's university was coming from. If I fail to secure my chemicals and some kid steals them and blows them up and gets hurt, there IS precedent for me being liable. Bad cases make bad law, but I do padlock my flammables and my oxidizers.

      I'd bet you, though, that if I wanted I could get sodium delivered to my door. I mail ordered magnesium ribbon last year when I couldn't get a department order in on time for my annual 'chemical and physical properties of matter' lesson. Did Amazon deliver? They did! Was it packaged safely? Nope! Was it cheap and fast? Certainly!

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    5. That being said, of COURSE making TATP in front of students is pretty fucking stupid. They don't call it 'mother of Satan' for no reason, do they? And I've never heard a story about grinding explosives in a mortar that didn't end gruesomely. If someone even has enough of a primary explosive to actually put in a mortar, they're doing the demo wrong. I'm not saying that unsafe demonstrations are great. Honestly I hate doing the sodium in water thing but it is kind of a traditional procedure and I follow it. Blast shields, goggles for everybody, stand at a safe distance, and do it outside.

      Just saying I'm not sure the guy is a criminal. Probably he'll be wiping his ass with a hook in the future. But that doesn't mean he necessarily committed a crime.

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  6. PPE for explosives? Unless you buy something specially designed for that there is no such thing. The only protection is to run at as small a scale as possible, max a few hundred mg. See: http://www.sciencedirect.com/science/article/pii/S1871553214000954 and http://www.sciencedirect.com/science/article/pii/S1871553214001285

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    1. there are common blast shields that can stop glass fragments from a small explosion. You could also wear extra-rated heavy duty protective glasses and kevlar helmet, apron. There are also metal mesh gloves but those are quite clumsy to work in.

      I think it is reckless to knowingly synthesize a known explosive in a lab without extensive precautions, and some kind of SOP and contingency plans for dealing with mishaps

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  7. And, he is a fully tenured Professor? In the words of Voldemort, "when will they learn?" The students can be excused if professor is "dumb as door knob mentality! I just cannot believe that the professor was making "terrorists" popular chemical.

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  8. Maybe he should try a sabbatical in the Klapƶtke lab in Munich to learn something about energetic materials in a safe way.

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    1. This ain't no research but demonstration to some innocent dudes!

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  9. Amateur! http://blogs.sciencemag.org/pipeline/archives/2016/09/27/what-this-here-compound-needs-is-some-hydrogen-peroxide

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