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DBL%20Hendrix%20small.png College chemistry, 1983

Derek Lowe The 2002 Model

Dbl%20new%20portrait%20B%26W.png After 10 years of blogging. . .

Derek Lowe, an Arkansan by birth, got his BA from Hendrix College and his PhD in organic chemistry from Duke before spending time in Germany on a Humboldt Fellowship on his post-doc. He's worked for several major pharmaceutical companies since 1989 on drug discovery projects against schizophrenia, Alzheimer's, diabetes, osteoporosis and other diseases. To contact Derek email him directly: derekb.lowe@gmail.com Twitter: Dereklowe

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August 24, 2010

Gegen die Dummheit . . .Well, Guess Who Wins, Again

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Posted by Derek

If you haven't heard about the explosion at Texas Tech earlier this year, this piece is the place to learn about it. (More from Chemjobber and the newly re-blogging Paul Bracher). In short, two graduate students were preparing a nickel hydrazine perchlorate complex, on far more than the recommended scale, and one of them was severely injured while trying to break up the substance in a mortar and pestle.

This is, as any experienced chemist could tell you, not a surprise. Call me when something like that doesn't blow up. But these weren't experience chemists. They were grad students, and I'm just glad that they didn't pay an even higher price for not realizing what they were getting themselves into.

At the same time, I find myself lining up more with Bracher's post, although I won't express myself quite as vigorously. The entire point of this research program was to look at hazardous energetic materials. The professor involved specifically told the students not to make more than 100 mg of material; they made ten grams. The injured student then ground up this material - yep, I did say "mortar and pestle" for real back there - with no blast shield, and gave the stuff one last poke after having taken off his goggles. He now gets to learn to write with his other hand. I can't figure out how he's still alive.

It's cruel, but one thing I actually respect about the physical sciences is that they have no regard for humanity. No exceptions are made; they respect no laws save their own. In a chemistry lab, we are dealing with the world as it really is, not as we'd like it to be. And if you want to believe that you can scale up the synthesis of a violent explosive by a factor of 100, despite warnings, and poke at the material without protection - well, you'd be just as well off doing it to a tiger. Perchlorates don't care what you think you can get away with, or how invulnerable you think you are.

Comments (41) + TrackBacks (0) | Category: Graduate School | Safety Warnings


COMMENTS

1. Will on August 24, 2010 2:50 PM writes...

To add insult to injury, the article paints him as a very sloppy scientist (at best) and someone with nefarious intentions (at worst)

useless record keeping? samples of explosives in his home??!!??

I'm sure he'll be a sought after candidate in the materials industry after he completes his dissertation

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2. Chemjobber on August 24, 2010 2:54 PM writes...

Derek: More on the reasoning behind my post later, but your last paragraph reminds me of an excellent paragraph by Gaussling of "Lamentations on Chemistry":

Like the time I discharged a picture tube through my hand while trying to remove a flyback transformer from my grandparents color TV... It is nothing at all like tangling with an vicious animal who might stand there after the altercation spent and panting, wondering in its little badger brain how to tear an even bigger chunk out of your leg. A discharged electrical appliance bears the same silent affect before as afterwards. It’s wicked electrons are inanimate and unparticular in their singular drive to find ground. An unexpected jolt from a device is much like a magical experience. It comes from nowhere and everywhere and is over in the blink of an eye. Afterwards you stand there in shock and awe of the effect of even modest amounts of energy.

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3. Anonymous on August 24, 2010 3:11 PM writes...

I'm sure he'll be a sought after candidate in the materials industry after he completes his dissertation

I was actually wondering if it was wise to award him his Ph.D after this, but then I had this same thought.

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4. Anonymous on August 24, 2010 3:35 PM writes...

The instrumentation for some of those tests was in other buildings on campus. Brown transported as much as "several grams of compounds" at a time in glass vials in a backpack or coat pocket, a researcher who helped Brown told EH&S investigators. Brown "was told that a metal container would be better for the transport, but he continued to bring them in a glass vial" the researcher said.
It looks like it was inevitable that something happened, luckily nobody died.

And TATP at home is most likely illegal, but it seems they (understandably) didn't look if it was really TATP.

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5. Mark on August 24, 2010 3:59 PM writes...

Chemistry does have an inherent danger to it. I can remember when I was in grad school a student tried to dry a metal perchlorate by putting it under vacuum, then heating it with a heat gun. Not surprisingly it exploded, but luckily it was at bench level so his stomach took most of the glass. Personally, any compound with the world "perchlorate" in it gets a wide berth until otherwise proven.

However, I was guilt of something similar. I need to purify mCPBA. I did the phosphate buffer wash on 10g of material, then put it under vacuum to remove the water. It wasn't drying fast enough so I hit it with a heat gun. I'm very lucky it didn't explode. I know that it was an unstable compound, but I wasn't aware just how unstable under post-purification.

Would it be feasible to come up with a safety list? A general list of rules when working with certain classes of compounds? It shouldn't be too difficult. Unfortunately most of the education about chemical safety comes with experience and knowledge passed down from senior to junior chemists.

Mark

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6. Anonymous on August 24, 2010 4:37 PM writes...

At my institution we have a "mandatory" safety meeting for all personnel in the chem department every summer. They show a random assortment of worst case safety problems. These situations they show are, at best, comical (student has open flame and then opens oxygen tank over top of it). They in no way adequetely prepare students for safety problems other than telling them to check the MSDS for possible complications with the chemicals they're using.

I'm convinced that these safety meetings are for liability reasons only. That way if some poor graduate student messes up and hurts/kills themselves or others the institution can say "I told you so." Chemistry graduate programs are not only preparing students for jobs that aren't there or will soon be gone BUT also putting them in continuous peril.

I agree with #5. Safety information is typically only passed down from senior students to junior students. This cannot possibly cover all the "big hitters" of chemical safety. Neither can a one hour safety meeting once a year.


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7. Anonymous on August 24, 2010 4:41 PM writes...

Texas cowboy chemists and high energy materials don't mix well.

A lot of people are surprised when I tell them I have never nor plan to make any explosives. The thought of making something that could detonate in a chemistry lab with X L’s of flammable solvents and gas cylinders is scary.

I hope he still has his thumb. I wouldn’t be surprised if the chemist is demonized in an attempt to try to distance the rest of the lab /PI from him.

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8. KevinM on August 24, 2010 5:14 PM writes...

It doesn't take a rocket scientist to figure out that any compound with hydrazine _and_ perchlorate in its name is not to be trifled with.

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9. Anon on August 24, 2010 6:10 PM writes...

"It's cruel, but one thing I actually respect about the physical sciences is that they have no regard for humanity. No exceptions are made; they respect no laws save their own. In a chemistry lab, we are dealing with the world as it really is, not as we'd like it to be."

Scientific libertarianism?

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10. Anonymous on August 24, 2010 6:30 PM writes...

@ #6 - "I'm convinced that these safety meetings are for liability reasons only. That way if some poor graduate student messes up and hurts/kills themselves or others the institution can say "I told you so." Chemistry graduate programs are not only preparing students for jobs that aren't there or will soon be gone BUT also putting them in continuous peril."

This is pretty much why some professors at UCLA make their grad students sign waivers upon joining lab. Safety isn't so big a concern so long as it leads to progress... But loss of money and reputation? That'd be terrible!

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11. J. Peterson on August 24, 2010 6:33 PM writes...

What's disturbing about this, is in the name of "protecting the country", the DHS is apparently funding all sorts of research on explosive compounds. This not only increases the likelihood of accidents, but also broadly distributes bomb-making knowledge. Your tax dollars at work.

Permalink to Comment

12. RLV on August 24, 2010 7:24 PM writes...

When I was in graduate school, there was a fellow student who would spill Chromerge, and not clean it up, just let it lie in puddle inside the hood. Luckily, I worked in a different building, and didn't have to deal with the green/yellow puddles.

With the TTU incident, the professor should have been paying more attention to the conditions in the lab. It could not have been a secret that this graduate student was sloppy. Then again, when I was in school, my professors had no idea what was going on in the lab. That was the postdocs' responsibility.

Permalink to Comment

13. Anonymous on August 24, 2010 7:25 PM writes...

I'm a little surprised by some of these comments. As a graduate student, I am responsible for my own research and am paid to think for myself. No, my 2 hour safety course did not cover everything that I will deal with. However, I am smart enough to recognize that MSDS sheets are there to be looked at, and that somewhere out there, someone has worked with almost all of the chemicals that I will use, and I can find out just how dangerous they are. When I make a novel compound, I treat it as though it is toxic/reactive until proven otherwise. That's just good operating procedure. Lazy/careless people don't belong in any occupation that is potentially dangerous...I have safely heated perchlorates before because I first found out at what temperature they decompose. We need to be careful about shifting blame off of ourselves and trying to pin it on some institution.

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14. bbooooooya on August 24, 2010 7:36 PM writes...

"I am smart enough to recognize that MSDS sheets are there to be looked at"

And what a great help the MSDS sheets are! Once, as a PDF, some friends and I snuck off to the beach at lunch. I got some sand in my shoes. Luckily, the MSDS helpfully explained the hazards,and how to safely dispose of this material (may be toxic to lungs, can produce target organ damage, the MSDS said that sand should be kept locked up, but it was all over the place, I think they allowed kids at the beach). Phew....

It's easy to sit back and say that "Lazy/careless people don't belong in any occupation that is potentially dangerous", but I'd be surprised if there are more than 5 or 6 chem PhDs in the world who didn't do multiple stupid things during their PhDs/PDFs, mostly due to inexperience (worst teacher...test before lesson...). Thankfully, cases of chem students dying are rare (probably more dangerous to walkf across the campus at TTU).

Permalink to Comment

15. Anonymous on August 24, 2010 10:03 PM writes...

that's 'gegen die Dummheit'

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16. Petros on August 25, 2010 2:04 AM writes...

A failed attempt for a Darwin award

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17. processchemist on August 25, 2010 3:22 AM writes...

I hate to say it, but with the current climate this kind of episodes will be more frequent. Haste, low level of consideration for any added cost about chemistry (and safety IS a cost), no discriminations between good chemists and bad ones: all these factors have also this kind consequences.

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18. petros on August 25, 2010 4:37 AM writes...

Doesn't seem to be related to cost.

The interviews with the labworkers in the investigation report suggest the whole group was sloppily run

http://pubs.acs.org/cen/pdf/TTU_EHS_accident_report.pdf

Permalink to Comment

19. processchemist on August 25, 2010 5:38 AM writes...

@18

I don't read anything about safety shields dotation in the lab.

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20. Paddy on August 25, 2010 7:01 AM writes...

Whilst working in Germany an undergrad in the lab was told by the boss to do a LiAlH4 reduction on a compound, it was the perchlorate salt of an amine. Needless to say within 10 sec the fumehood sash was no more. Oh and he did the reaction on 100g.

Permalink to Comment

21. Donough on August 25, 2010 7:07 AM writes...

Its seems a pretty lax environment to me; safety glasses of in a lab is pretty stupid and would not be tolerated. His general apparent sloppiness seems to also indicate laxness.
While personal culpability is an issue institutional culpability should be more to the fore he. He is a student after all and must be taught. Further proper equipment not being available (storage facilities/blast shields) as well as no existent safety programs leads me to believe that this lab should be closed upon review. It is not the students who got complacent here (they did not know) but rather the staff.

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22. bbooooooya on August 25, 2010 7:13 AM writes...

"Doesn't seem to be related to cost."

This is actually an example of free market fomenting better regulation. Chemistry depts at universities don't need to worry about being sued for poor safety practices (at least as far as footing bill): private companies do. This seems to make safety enforecement more rigourous in industry. To be fair, greater level of expereicne once one gets to the "real world" contributes.

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23. Anonymous on August 25, 2010 7:40 AM writes...

@22

"This seems to make safety enforecement more rigourous in industry"

This rigorous safety enforcement in industry (again, a cost) is between the factors driving this industry to chindia (no safety costs, no environmental costs).
In my shop we used to do some "unpleasant" chemistry on pilot scale: we needed gas scrubbing (effluent to be disposed of), and we generate quite a lot of waste (cost). We've been contacted a couple of years ago by an indian company (small). "We know you make this product" they said "We will be glad to be your contract manufacturer for this one. We're really competitive and we have *no environmental costs*".
Our production was dropped one year ago. This niche product now comes from 4 or 5 companies between India and China. "No environmental costs" can be an huge competitive quality, in productions.
By the way, I don't mean that in the western world we need lower environmental regulations.

Permalink to Comment

24. El Selectride on August 25, 2010 8:27 AM writes...

"In a chemistry lab, we are dealing with the world as it really is, not as we'd like it to be."

Or as Dostoevsky put it:

"Nature does not ask your permission, she has nothing to do with your wishes, and whether you like her laws or dislike them, you are bound to accept her as she is, and consequently all her conclusions."

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25. gyges on August 25, 2010 8:41 AM writes...

Perhaps you need a culture of secrecy in your jurisdiction like we have in ours. It makes proper scrutiny so much more difficult and often helps the culpable wriggle out of manslaughter charges.

See, "MoD scientist says no safety concerns raised before fatal blast."

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26. Curt F. on August 25, 2010 9:01 AM writes...

Both TTU and the students in question deserve blame here. But for me the onus falls mainly on the student. He was told by several people that he was being unsafe. He intentionally circumvented safeguards (100 mg maximum scale) told to him by his boss. Do graduate students in chemistry really need to be "trained" to not disregard or ignore the dictates of their supervisors and the implorations of their colleagues?

If there is one single thing TTU could do to create or improve its culture of safety, it would be to dismiss this student (and possibly his anonymous colleague) loud and publicly for complete disregard for their own and others' safety. Keep dismissing people who are found to willfully disregard the safety-related dictates of their supervisor -- whether or not their insolence leads to an explosion -- and the required shift in the "culture around safety" will happen in a hurry.

I hope the local DA's office will take a serious look at this incident. It's hard to imagine behavior that would better qualify as "reckless endangerment".

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27. E on August 25, 2010 9:38 AM writes...

The C&EN article says that the research group did not have any blast shields. How can anyone have sympathy for the principal investigator here when she did not make available the most basic protection for people working with explosive materials? I get the impression that the lax attitude toward safety did not lie with just the one graduate student - the tone was broadcast from the top down.

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28. Nick K on August 25, 2010 12:16 PM writes...

The project the unfortunate grad student was working on strikes me as grossly inappropriate for an academic lab. Surely the work should have been carried out in a Government lab with the correct containment facilities for explosives?

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29. DN on August 25, 2010 1:40 PM writes...

I used to work on explosives detectors on these sorts of government contracts (albeit on the engineering side, not chemistry). Safety is provided by conscientiousness and the plan of work, not by fancy shielding. In particular:

1. Stick to small quantities. Most practical detectors work on microgram scales, and can be characterized from a milligram reservoir. (Nitrates are a general exception for practical reasons.) RESULT: Accidental detonation results in a nasty wound, not the guy behind you being impaled by your ribs.

2. Significant quantities should be dispersed in a porous medium. Most explosives become incapable of detonation when mixed 99:1 with sand. Usually they won't even burn. RESULT: Safe, and the usual vapor detectors and backscatter spectroscopy detectors work just fine.

3. Use non-fragmenting containers and tools. To pulverize a solid, put it in a plastic bag and massage it between styrofoam blocks. Preferably outdoors, to reduce blast reflection from walls. Mr. Teflon is your friend, because he is squishy and inert. Use earplugs in addition to goggles. RESULT: Injury is reduced to surface burns and blast overpressure. (A ceramic mortar and pestle, I ask you?! That would have resulted in administrative leave where I used to work.)

4. Field workers must be trained! E.g., some laser spectrometers have enough power density to ignite black powder, causing at least one tragedy when a multi-kilogram sample was tested by a poorly trained user. Ditto for flashlamp sample collectors, electrostatic particle samplers, detectors with heated tips, and so forth. If it's not safe enough for a toddler to play with unattended, don't point it into a 50 pound drum of TATP.

5. Hire and promote, or at least visit the labs of, people who blow shit up for fun and still have all their fingers. A guy who reloads his own pistol ammunition would have come down on the Cowboy Chemist like a ton of bricks.

Permalink to Comment

30. myma on August 25, 2010 2:43 PM writes...

So I had the thrill in grad school of synthesizing stuff in a wet chemistry lab, where safety was haphazard and enforcement lax, and then testing my stuff in a clean room nanofab where safety was the other extreme of safe. In the clean room, there was a healthy dose of ridiculous rules (eg: a cough drop in the mouth is considered forbidden food; any glass vial no matter how small had to be carried in a large rubber bucket). But there were the one strike rules that were followed religiously. Why? Because if some idiot engineer did something dumb like leave HF in a glass beaker (bad) unattended (getting worse) and probably unlabelled (ah jeez), that engineer's card access would be cut off without discussion, effectively ending graduate school right then and there. Safety problem solved.

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31. Anonymous on August 26, 2010 1:29 PM writes...

My experience as a graduate student was also that health and safety was just for liability reasons. for example, it was perfectly fine to work alone before 6 pm, no matter how dangerous the procedure, but God help you if you were caught working alone after 6, even if it was with something completely harmless.

@13: MSDS are laughable, if they had one for tap water it would warn you of danger of death (after all, it can kill you by drowning) - info supplied by manufacturers is the epitome of doing something to prevent litigation rather than preventing injury.
Also bear in mind that a careless/inept student can harm others, not just himself; institutional negligence puts everyone in the lab at risk.

@21 Donough: Yes, an explosives lab without blast shields seems blatantly unfit for purpose.

@17 processchemist: that too was my experience, that it was assumed everyone was equally competent, when that blatantly wasn't the case - anything else would've required somebody other than students and postdocs to take a peek at what was going on in the labs, so it obviously didn't happen. Actually there were instances in which the most inept person in a group was working on the most dangerous project.

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32. Anonymous on August 26, 2010 11:05 PM writes...

i remember watching a former colleague (grad student) empty (purge) a syringe containing t-buli in the lab sink after he was done with his rxn. Unfortunately, back in the late 80's we washed our glassware with acetone in the sink. Needless to say, he did a major Richard Prior act (but on steroids)!!! (pardon the pun). We managed to put him out with