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The Old School

I enjoyed this piece on “The Changing Culture of Chemistry”. The author, Bruce Gibb of Tulane, has in mind the changes that are apparent when you read old papers that describe (say) a couple of unidentified people associated with the project ingesting one of the sulfur-containing components of asparagus (asparagusic acid, newly isolated from 40 kilos of thick, syrupy “asparagus concentrate”, which must have been a joy) to see if that was the source of the smell that it imparts to human urine. That happened in 1948, and you can definitely say that it was a different era. I know that your curiosity is up, so I’ll mention that they concluded that asparagusic acid wasn’t the cause, although current research suggests that it is (via metabolism to volatile thiols – the earlier volunteers may well have not eaten enough of the stuff).

But that got me to thinking about what sorts of things were more common when I started out in chemistry that would seem odd now. The immediate example is from my college chemistry: in my freshman year we did a freezing-point-depression lab with benzene, as it had been done since anyone could remember. I was immediately struck by its distinctive odor, which makes me wonder just how much of that odor I was exposed to. But I was part of the last class that did it that way; benzene dropped off the list, never again to be seen in the undergrad labs. Even at the time, we heard stories from the older professors about how they used to clean the vacuum pump parts in deep baths of the stuff, so at least I missed out on that.

The oldest faculty member in the department was Prof. Shideler, whose pedigree went back to Roger Williams of folic acid fame. He would drop mentions of things that would curl your hair, such as the use of hydrogen sulfide gas as a laboratory reducing agent (“We used to fog the air with the stuff; only later did we realize that it was roughly as toxic as cyanide”). So I’m glad I missed that one, too. I took Shideler’s last biochemistry course in 1982 (he was an emeritus professor by then), and as twenty-year-olds, we regarded him as the personification of The Old School, a sort of coelacanth who would throw questions at you on the last page of an exam about bacterial variations of the Krebs cycle. (“If this class were a democracy, the answer that most of you got would be the correct one. Unfortunately, this is a dictatorship. . .”) He was a link to the “Here, eat some of this and see if your urine smells funny” era.

So for this Friday, I’ll throw out the question: are there things that were done in your early chemistry years that would raise eyebrows now? Just how long did some of the less-approved practices hang on in some areas? I look forward to the comments. . .

139 comments on “The Old School”

  1. myma says:

    Back in my day, they would always warn us to never ever mouth pipette. By junior/senior year when we got the old school professors in the advanced lab classes, we realized that they all still did, maybe because those enormous rubber bulbs were never any good.
    Every hood also seemed to have a small plastic bottle in the back filled with waste mercury.

    1. Derek Lowe says:

      Mouth pipetting is an excellent example. When I took a bacteriology course my junior year of undergrad, the professor encouraged it, because that’s how it had always been done. The three of us chemistry majors in the class were so revolted by the thought that we brought bulbs over to the lab because we wouldn’t do it.

      1. GutDecipher says:

        Seems like the warnings we got in every syllabi for every lab class (“NEVER PIPETTE BY MOUTH!”) were more for the instructors than the students, who don’t immediately look at a pipette and think ‘straw’.

      2. Imperialist says:

        The problem is that pipettes are designed to be used by mouth but have been retrofitted with useless pumps and perished rubber bulbs. It took decades before a decent pipette pump made it into undergraduate labs and there surely has to be a better way to dispense liquids with precision.

      3. Philip King says:

        I took a module on industrial microbiology during my undergrad. One of the lecturers, rapidly approaching retirement, taught the uses of extremophilic bacteria for leaching metals out of ores that otherwise had too little metal content to be economic to process.

        ‘These bacterial can survive at an environmental pH which is similar to that of stomach acid,’ he said, before pausing and looking thoughtful. ‘And I’ve been mouth pipetting cultures of them for years.’

        He shrugged, and carried on with the lecture.

  2. Anne Glenn says:

    We did a lab in ’82 from Pavia and Kriz that was the isolation of nicotine from tobacco. Being in NC, we all brought in different tobacco sources, and one friend brought in a giant tobacco leaf from the family farm. I’m sure we weren’t wearing gloves, and we weren’t working in hoods (I hope we were wearing safety glasses, but I’m not sure). Knowing what I do now about the toxicity of nicotine, I can’t believe we did that. I don’t think that lab is in the current edition of Pavia! 😳

  3. Andy says:

    Teaching lab steam baths, it was like a bloody sauna!

    1. Anon says:

      Oh, man – trying dry down sodium ethoxide using a water-aspirated rotovap and heating over a steam bath in Chem 62L. Nary a fluffy white powder was seen that day. RIP, Venable Hall!

      1. anon the II says:

        Venable Hall! What a cool old building! The labs had glass ceilings that you could open up by pulling on chains, like a greenhouse. I wonder how much mercury had seeped down into the crevices of that old building before they finally took it away. I noticed that when it was removed, many feet of dirt below it were also taken away.

    2. AlphaGamma says:

      Still in use in the UK for first-year undergrads who can’t be trusted with heating mandles or hotplates…

  4. MP says:

    I’ve heard stories of people smoking cigarettes in the lab…

    1. Rod says:

      Oh, yeah. I often witnessed people pouring solvent from a 4L bottle into the reservoir atop a column while a cigarette dangled from their lips.

    2. A Nonny Mouse says:

      We had one of the inorganic profs who would stub out his cigarettes in a basin of ether for a joke (during his supervision of an undergraduate lab- Imperial, but most of them were usually intoxicated from a lunchtime in The Queens).

      1. Imperialist says:

        Prof Evans FRS was an all round genuis though. He pointed out that smoking was banned not because of the fire hazard, but because you were putting your fingers to your mouth. He also taught all his group to gargle with liquid nitrogen (“it’s ok if you keep it on the move”), and ate glasses in the pub to intimidate disruptive drunks. He used to pass pressurised benzene oxygen complexes around lectures so we could see the colours. He ran a sideline in expert witness for the defence in drugs trials and gave sound legal advice that you should always insist on a jury trial “south of the river” as there was sure to be a villain on the jury who would acquit on principle.

    3. MattH says:

      well, actually I saw people smoking in the lab …
      … and, heating ethanol in a beaker using a Bunsen burner, is not always the best idea

    4. Jonathan says:

      When I was an undergrad in the UK in the mid-1990s and doing an extramural year at a very prestigious research institute there were cigarette burns on the inside of the fume cupboard in my lab, left there by one of my supervisors a few years earlier (before she quit smoking).

    5. MTK says:

      I once saw someone smoking in the lab and was shocked.

      This person assured me he was doing it as a safety measure since he was working with cyanide and claimed that smoking was an early cyanide detection method since cigarette smoke tastes changes dramatically if there’s any cyanide around.

      I have no idea if that’s true or not, but I’m pretty sure it still wasn’t safer to be smoking than not in the lab.

      1. Hap says:

        It’s previously given advice:
        http://www.orgsyn.org/orgsyn/prep.asp?prep=cv1p0314

        It’s probably not a good idea to start smoking for HCN detection (I imagine the cumulative risk of being addicted to smoking is bigger than the risk from HCN exposure) but if he’s a smoker anyway, it might make sense.

        1. GutDecipher says:

          That is a gem of a note. Thank you.

    6. Larry says:

      At UCSB many years ago, Bruce Rickborn (a real character and the “old schoolest” of the old school chemists) used to smoke in the lab. One day he flicked a cigarette ash into a wastebasket, and a whoosh of flames shot up. Turns out, one of his students had just dumped his used silica gel column into the can, wet with solvent. I almost pooped in my pants, he simply found a cover to put over the can. This guy also used to clean off his hands with benzene when he was a student with Donald Cram.

      1. a. nonymaus says:

        Ah yes, Rickborn was a character, and very educational. I remember rinsing out our glasses with a squirt of acetone after we finished with the Tuesday post-seminar wine tasting group.

        1. Larry says:

          Yes, the afternoon wine tasting group. He was quite the connoisseur.

    7. Dr. Z says:

      We used to smoke in the buildings but not in the labs except Physical Chemistry lab where the professor was a chain smoker and we got permission. Can you imagine 20 people lighting up in about 50 m2 lab at the same time (well 21, including the Prof 🙂 ). Oh, an there was an old mercury manometer in that lab without any protective oil above the mercury to keep it from evaporating… Fun times.

  5. Survivor says:

    The hanging drop electrochem apparatus we used in an undergraduate lab always seemed to have half a pint of elemental mercury rolling around in the catch pan under it. We still used a bit of benzene in some experiments then, but it was on the way out for undergrad use by the late 70s.

    I rarely saw gloves worn during grad school in org chem, but they were available, usually. We’d started using CHCl3 to wash the salt plates used for IR, because carbon tet was thought to be too toxic by the early 80’s The fume hoods were largely non-functional, which became apparent when one of the group was working to isolate natural products from milkweed seeds, those nearly-weightless bits of white fluff. You could drop a handful in the hood and they’d fall to the bench; not enough airflow to move them. Once, to complete some plumbing work, they had to shut off water to all of the safety showers on our floor. Not to worry, we were admonished to be extra careful while working during the shutdown.

    1. NQ says:

      On announcing the discovery of my non-functional fume hood to my grad school advisor, he replied “just keep working; you’re not doing anything that dangerous”. In 2015…

      1. UIUC says:

        You know you can say his name right? Scott Denmark. Scott Denmark ignored safety and demanded you continue your work in a non-functional fine hood.

  6. anon says:

    In Austria it’s still common practice to use hydrogen sulfide gas in undergrad inorganic chemistry lab courses..

    1. Peter Kenny says:

      We used a Kipp’s apparatus for generating H2S when I was at high school in Trinidad in the 70s and we used it for qualitative inorganic analysis. I recall that bubbling H2S through solutions containing Zn++, Hg++ or Pb++ gave black precipitates.

  7. Peter Kenny says:

    Here is one of my favorite Gaussian Quotes (I have linked the article as the URL for the comment):

    EVANS BOLDLY PUT 50 ATM. OF ETHYLENE IN A CELL WITH 25 ATM. OF OXYGEN. THE APPARATUS SUBSEQUENTLY BLEW UP, BUT LUCKILY NOT BEFORE HE OBTAINED THE SPECTRA SHOWN IN FIGURE 8.
    A.J.MERER AND R.S.MULLIKEN, CHEM.REV. 69, 645 (1969)

    1. John Wayne says:

      Outstanding

    2. anon says:

      This one is my favorite. And it’s from Mulliken!

  8. bacillus says:

    Sorry bacteriology not chemistry. Mouth pipetting homogenates of mouse livers and spleens laden with Listeria or Salmonella and occassionally getting a mouthful of the stuff. Squirt 70% EtOH from nearest wash bottle into mouth, rinse, spit, repeat, carry on working. Even further back, biocontainment level 3 lab working with Legionella. Containment was the glove ported biohoods in the room, everything else was considered safe. Smoking and drinking tea whilst shaking litres of Legionella right next to my desk. Worked with a lot of old-school chemists at the start of my current job. Tales of changing hydrogen cylinders with cigarette dangling from mouth. Paper chromatography in open vats of highly volatile solvents followed by drying by lifting paer up and down in front of an open heat source. When HF was needed, cylinder was simply turned upside down and valve slowly opened to allow a few drops of the condensate to drip into a glass beaker. At least this was done under a fume hood, but all glass apparatus, not so much. Everyone lived to a ripe old age though. Nowadays, newly minted microbiologists are scared of their own shadows. Little do they realize that the average supermarket chicken carcass contains more Campylobacter than found in the average micro lab.

  9. MattF says:

    I’m a physicist, so my main memory from Chem Lab is the taste of acetone.

  10. PD says:

    Benzene can be a fantastic non-polar eluent for silica gel chromatography in certain situations where a separation is problematic. In grad school, our group (focused on carbohydrate chemistry) used benzene for columns well into the late 90’s for difficult separations when nothing else would work. You’d think toluene would be a simple replacement, but it just doesn’t quite behave the same.

  11. January 1991, older French molecular biology professor who had known Jacob & Monod: ‘Don’t do this!” – takes cigarette out, mouth pipets phenol and returns cigarette to mouth.

    Environmental Health & Safety had given up on him long before that.

    1. MrRogers says:

      Same experience, 1992, no cigarette, somewhat younger American professor.

  12. Thomas McEntee says:

    Ahh, The Old School… I remember an analytical course in 1961 and the lab sessions with the dropping mercury electrode, a beast of that course and a technique that I failed to understand or use through the rest of my career. In 1963, I took a year off and worked as a lab tech in a small NJ chemical company. Environmental consciousness consisted of dumping waste solvents into the proper unlined pit out in the back 40…one for water-solubles, one for hydrocarbons, and one for chlorinated solvents…and whatever was dissolved in each. Asbestos gloves were common but no one used rubber gloves except for the most corrosive materials. Stubborn materials on glassware was cleaned with the open 20-gallon bath of conc sulfuric and sodium dichromate and all glassware was dried after washing with acetone in big Nalgene squeeze botttles. Everyone smoked at the bench and hoods except when working with ether or ligroine… Benzene, toluene, and xylene were the workhorse aromatics, MDC, chloroform, and carbon tet were the workhorse halogenateds. When I returned to school in 1964, my undergrad advisor, one of Gilbert Stork’s PhD students whose research was in indole alkaloid total synthesis, would tell us about the old days…stuff like the array of colorimetric tests the really old chemists used to employ, like the Fischer pine splinter test for indoles. Things have changed!

  13. PD says:

    I haven’t been able to corroborate that this is true yet, but when we were discussing mercury at lunch one day someone mentioned that some of the very first glove boxes involved inserting your hands THROUGH a pool of mercury. Anyone ever hear of that one?

    1. Petros says:

      Not directly but our school physics teacher used a large bowel of mercury, a glass tube and bare hands to demonstrate the principals of a mercury barometer on the open bench

  14. A Nonny Mouse says:

    I was let loose with a large cylinder of phosgene as one of the first experiments of my PhD. Fume hoods were basically useless and then I had all this liquid in the liquid nitrogen traps after distilling the product – had a smell to see what it was…

  15. gretchen says:

    Dishes of mercury. All waste, including radioactive, was just poured down the drain. Pipetting by mouth; I once swallowed a solution of 2,4-D and waited to see if I’d sprout leaves. I was using a 6-foot by 3-inch Sephadex column, and first I cleaned it with conc sulfuric acid. But the plug at the bottom came out. Cleaning the floor was fun, but I learned the acid didn’t hurt as long as your hands were dry.

    All my dresses (women weren’t allowed to wear trousers outside the dorms) had tiny acid holes in them. Only technicians wore lab coats.

  16. A Nonny Mouse says:

    I also used to do the cooking (pasta/rice) before Friday evening group meetings ( a prelude to the pub) on the hot plate that was used for developing tlc plates. The pre-cooked chilli/curry/etc was put in one of the glassware drying ovens to heat up.

  17. drsnowboard says:

    Not dangerous exactly, except to your hearing and the floor covering but running water pumps to create vacuum for filtrations. In fact, running water for anything – circulating chillers and diaphragm pumps thankfully pretty universal now.
    Although I have seen someone mop out a lab recently after a water connection failed…..

  18. Ed says:

    When I took an undergraduate organic chemistry lab class in the 1980s, we did an experiment using diethyl ether as solvent which needed to be removed to isolate the reaction product. There weren’t enough rotovaps or hoods to go around, so we all evaporated them down by heating them on the benchtop. All 25 of us. At the same time. Nobody passed out, but I think I was close.

    1. oldnuke says:

      Had a similar experience in high school biology, used ethyl ether to anesthetize fruit flies (remember the genetics experiments with eye color?).

      No fume hoods in the bio labs in my school — the only hoods were one each in the chem labs and the prep room.

      The entire class was ready to fall over by the end of the period.

  19. Red Agent says:

    Fun stuff. Donning asbestos gloves so I could rapidly hand-brake the centrifuge. And speaking of hydrogen sulfide, how about putting a match to a tube coming from the gas generating bottle, to demonstrate its flammability. So you get the place choking with both hydrogen sulfide and sulfur dioxide. The fume hoods may or may not have worked. Who knew? They were for sissies.

  20. Bob says:

    In grad school (circa 1977-1982) nothing gave the lab benches the great shine that Benzene did. By then it was already frowned upon, but I still used it until common sense got the better of me 🙂

    1. Colintd says:

      UK school in mid-80. In a uncharacteristic involvement with the science department, the headmaster who was an arts major had read an article on the dangers of benzene and told the chem department they couldn’t use it any more. The teachers reluctantly said okay….. and relabeled lots of bottles nor-toluene.

  21. BA says:

    I can think of a few things that raised eyebrows at the time:

    – getting powdered LiAlH4 all over one’s bare hands before a casual quench in the sink
    – using a portable vacuum pump attached to a poorly-sealed Buchner flask filled with years-old mercury… as a mercury cleanup kit
    – according to a current post-doc colleague, at their undergrad department, a post-lab hand wash in DMF was routine

  22. Anonymous says:

    I always rather liked the undergraduate lab for extracting cholesterol from human gallstones via the dibromide. The best part was wrapping the gallstones in a towel and repeatedly smashing them with a hammer. Quite a satisfying crunch. Pity gallstones are no longer easily available.

  23. Another Guy named Dan says:

    Mercury barometer experiment in 9th grade science. 500 ml beaker of liquid mercury in every lab station. My brother is a high school teacher, and they had to call in the fire department HAZMAT team because someone found some old thermometers in a store room two years ago.

    1. Marie says:

      Yes, high-school chem in the early ’80’s. Mercury thermometer; someone in my lab group dropped it and it broke. Little beads of mercury all over the lab top. I grabbed two pieces of notebook paper, one to collect it on and one to push them around. Everything then went…into the standard classroom wastebasket.

      The best lab of the year was making pulled taffy over the burners.

      1. Jonathan says:

        Back in high school chemistry my lab partner and I also managed to spill mercury all over the lab bench. Fun times!

  24. Isidore says:

    Undergraduate chemistry lab, refluxing something or other in 100s of mLs chloroform on the benchtop using a heating mantle (or maybe a Bunsen burner, we did use those as well) . Students and instructor inhaled a lot of chloroform that day, although no one passed out. We also used benzene quite liberally as I recall. The year after I graduated the organic chemistry lab went microscale.

  25. myma says:

    OK, not chemistry school, but still old school. I was cleaning out my grandfather’s old back shed a few years ago. There was a nice jar of DDT and bottle of Chlordane on a shelf in it, with material still in them. Since I didn’t know if the town regular hazardous waste days would/could/should take it, I just left them there.

    1. RUSSELL W STYLES says:

      DDT is said to be quit safe for mammals. Birds, not so much.

  26. luysii says:

    It wasn’t so much what my 20 students in orgo lab in 1960 were asked to do, as what one of them was always doing. They were good kids (all of 2 years younger than me), and I’ve subsequently read papers by a few and one has her own lab at NIH. So 19 of them were easy to deal with but the 20th took 90% of my time, because he insisted on knowing what the stuff we were using TASTED LIKE. Over the years, I’ve tried to Google him but to no avail (probably because he’s dead). Since there is no confidentiality agreement between lab instructor and instructee (I hope), does anyone out there know what happened to Jim Bundy (possibly Harvard ’62).

    1. Colintd says:

      I remember the teacher getting us to find out why lead acetate is called sugar of lead…

  27. tt says:

    My favorite way to quench solid sodium or potassium waste is a method taught to me by a fearless Russian chemist I shared a lab with: Fill a large beaker half with water and half with diethylether. Add solid Na or K waste. Watch the bouncing ball…The metal hits the interface and bounces into the ether layer on a jet of hydrogen. It then calms down a bit and sinks back to the interface where it once again jumps back into the ether…fun, scary, and a great way to quench. My Russian friend assured me that this was by far the safest way to get rid of Na or K and standard protocol at Moscow State.

  28. Ursa Major says:

    The asparagusic acid story reminded me of the literature prep of phenyacetyl glutamine followed in this paper from 1922, http://www.jbc.org/content/53/2/463:

    “This substance was prepared according to the method of Thierfelder and Sherwin. A man of 62.5 kilos body weight ingested 5 gm. of phenylacetic acid on each of 3 consecutive days…”

    The Thierfelder paper from 1914 (http://onlinelibrary.wiley.com/doi/10.1002/cber.19140470341/abstract) has its own interesting comment:

    “Leider verhindern uns die politischen Ereignisse zur Zeit den entscheidenden Versuch auszufuehren.” [Unfortunately, political events are currently preventing us from making the decisive experiment.]

  29. Tony says:

    I recall reading an article many years ago about the mean lifespans for various professions. Overall, academics scored pretty well, since proving theorems or studying Chaucer typically isn’t anywhere near as risky as, say, being a commercial fisherman in Alaskan waters. The sole exception was chemists. Chemists had a significantly lower lifespan than the general population.

    1. MoMo says:

      Been watching the C and E obits lately? I follow these things and we geezers live pretty long compared to other professions- 80-90 years! So get back to work and the secret to longevity is staying engaged, retirement will kill you!

      1. doc says:

        Damn right. I’ve heard that “chemists die young” stuff for years. Nuts. My undergrad advisor (Harry Day, of Crest fame) died at 102. My major professors- those that aren’t still alive- all made it to their 90’s. Every single one of ’em.

        Now, fluorine chemists have it tough. But the rest of us? Chemistry either weeds you out early, or you’re good for the best part of a century.

        1. Pennpenn says:

          It’s that “I’m old ’cause I’m ‘ard” kind of concept, yes?

  30. MoMo says:

    Those who don’t have fun/danger in the chemistry lab shouldn’t be there, and Old Schoolers know this well and were well trained in such mayhem. No smoking/ drinking in labs anymore, no access to explosive fun with sodium because of Dry seal bottles of solvents, no more joining the “Sunken Gardens Club” when your condenser hose pops off, flooding the lower floors of your building. The fun and mystique is replaced by stern safety officers, liability waivers and students glued to their cellphones, narcissistically seeking attention.

    Those were the days!

  31. In physics labs, we stopped moving lead bricks bare-handed and used gloves instead.

    In the very old-school days, so I’ve heard, people tuned cyclotron beams by placing their heads into the beam, closing their eyes, and tracking the beam size by looking at the Cerenkov radiation as the electrons passed through their eyeballs.

  32. imarx says:

    My uncle worked as a student hired hand in a chemistry lab at the University of Chicago in the 60s. Apparently they used carbon tet as a glassware rinsing solvent the way we use acetone today. No gloves of course.

    1. Isidore says:

      Carbon tet was used extensively in dry cleaning until the late 70s or possibly early 80s, I am not sure when it was abandoned.

      1. milkshake says:

        our old lab manual had recommendation to use CCl4 + dry ice cooling bath as excellent alternative to salt/ice for -20C….

        Preparation of nitrosomethyl urea (starts with Br2/NaOH Hoffman degradation of acetamide) in the freshman labs.

        Of course our old teaching lab had half-liko bottles of dry picric acid and few kilos of anhydrous magnesium perchlorate on the shared shelves, for anyone to peruse

        1. J n says:

          Carbon tet was a great film cleaner. Wish I still had some!

    2. Emjeff says:

      we used carbon tet as a solvent in freshman chemistry in the early 80s. We were warned that is was dangerous, though

      1. dave w says:

        The hazards of carbon tetrachloride were apparently known a long time ago… I once saw a technical manual for the WW2-era diesel-electric submarines: it included the comment that carbon tet was an excellent solvent for degreasing electrical equipment, but was toxic enough that it should “never be taken to sea in the closed environment of a submarine”…

  33. Barry says:

    A classic in the field was published just 32 yrs ago by Repke, Grotjahn, and Shulgin in which they report the synthesis, ingestion, and psychotropic effects of a series of substituted tryptamines. The experimental section explains that the three authors, and two of their girlfriends, and the wife of the third dosed each other by a double-blind protocol, they wrote up their subjective experiences of each “drug”

    Psychotomimetic N-methyl-N-isopropyltryptamines. Effects of variation of aromatic oxygen substituents

    David B. Repke, Douglas B. Grotjahn, Alexander T. Shulgin
    J. Med. Chem., 1985, 28 (7), pp 892–896
    DOI: 10.1021/jm00145a007
    Publication Date: July 1985

    1. NJBiologist says:

      Shulgin wasn’t alone–I’ve read papers from a couple other scientists active from the 60s to the 80s who believed you didn’t fully understand a CNS-active compound until you’d ingested a bit of it.

      1. MoMo says:

        True that. Met a prominent academic hallucinogen researcher once who told me he tested his products on himself stating ” How else are you going to know what the rats are thinking?”

        1. Derek Freyberg says:

          Shulgin, and his wife if I recall correctly, wrote the book on the subject: “PIHKAL: Phenethylamines I have known and loved”, complete with recipes and tasting notes. I believe my local library still has a copy.

  34. Uncle Al says:

    Late 1970s, petroleum company (outsourced): Benzene in an armored optical cell with huge oxygen pressure, looking for a pi-complex including “nose of the camel” (oxygen threading through the “hole” in the ring). Late 1980s, medical device manufacturer, spinning band vacuum distillation of a monomer by the liter (!) to “remove” a fatal impurity. It was a reversible oxygen pi-complex, then irreversible peroxide formation, then crosslinked mess.

    One chemist vacuum distilling pot-to-pot then breaking to *argon* royally pissed off an entire engineering section. “Best efforts will not substitute for knowledge.” W. Edwards Deming

  35. Chris Phoenix says:

    High school chem, mid 80’s, small town in New York State, I remember us using carbon tet for cleanup.

  36. AndyM says:

    When I was at UNC in the 80s, there was an old-school synthetic chemist that haunted the corridors of Venable Hall who reeked of aromatic heterocycles – I don’t know if it was because he never wore a lab coat, never changed his clothes, he actually sweated aromatics due to exposure, or all the above. He was known to indulge in departmental stocks of absolute ethanol and so colleagues had to take to either denaturing their stocks or putting them under lock-and-key. He was a great guy and if you engaged him in a conversation you soon came to realize that old-school synthetic chemistry was a hazardous art form and that a shot of EtOH at the end of the day probably helped calm the nerves.

    From that era, Burroughs Wellcome alumni also have stories of senior medicinal chemists self-dosing their creations. Those were the days literal bench-to-clinic drug discovery.

    1. anon the II says:

      I’m guessing that was Dr. Robert McKee, the very essence of an old school chemist and a great teacher.

    2. doc says:

      That was Bob McKee, one of my committee. Yep, a real organic chemist.

      He kept a ruptured high pressure hydrogenation bomb as a paperweight. Said that when it went one corner of Venable came out of the pit.

  37. a says:

    ITT: Survivorship bias

  38. Summer of '69 says:

    Dizzy Jones the woodwork master popping in to the Grammar School chemistry lab one lunchtime, “I need some conc nitric to clean out this metal bucket…”

    …And then disappearing down the corridor to the woodwork room complete with bucket held aloft giving off copious brown fumes.

  39. Wile E. Coyote, Genius says:

    Not chemistry, but making dinner in the autoclave. Does a wonderful job on pot roast, potatoes, onion, carrots, etc in about 20 minutes.

  40. Steve says:

    Freshman inorganic chemistry 1971 – semimicro qualitative analysis lab which involved identification of metallic cations via precipitation and flame tests .

    Many sulfide salts are insoluble, so of course everybody had their own little bottle for hydrogen sulfide generation. The lab stunk but at least no one died that I am aware of.

  41. F says:

    When in graduate school for biochemistry in the 60s my mother dropped a bottle of mercaptans which necessitated evacuating the building. Shes always been annoyed that if the building had to be evacuated it wasnt for something actually toxic.

  42. Bruce Hamilton says:

    High School chemistry class in brand new science laboratory, and students putting hot deflagrating spoons right through new plastic sinks because our teacher was used to porcelain sinks.

    First Job ( Industrial Lab ). Making polyurethane foam insulation test blocks by quickly pouring isocyanates and polyols, along with amine catalysts and surfactants, into a bucket on the laboratory floor, mixing with a propellor on a Black and Decker hand drill for 20 secs, quickly pouring contents into a heavy wooden jig and slamming it shut as the foam rose. Then pouring a litre of trichloroethylene into bucket to rinse all the polyurethane out before it set.

    Second Job ( Contract Manufacturer ). Tasting strychnine as part of formal pharmaceutical identification test. Yes, it is very bitter.

    Third Job ( Petroleum Company ). Noise and visual flame of total consumption burner on Varian AA4 atomic absorption spectrometer. At least we didn’t have a Turner-Burrell Adsorption Fractionator which used boiling mercury vapour to separate natural gas components on a charcoal column. Making test gasoline blends by standing on the back of a road tanker and dispensing pure tetraethyl lead and ethylene dibromide into compartments, and then driving down a bumpy road to mix the blends.

    Fourth Job ( government research ), watching two hundred litres of Freon 11 boil out a cooling bath for a 25 litre QVF reactor as the exotherm was much greater than predicted.

    Fifth Job ( current ) – by now I had access to fume hoods. Trying to open an old corroded-shut phosgene cylinder with a 1/2″ pneumatic impact driver, shattering the valve spindle instead. Cylinder subsequently disposed of by the military with 4x mass of explosive.

    Destroying contents of a large cylinder of silane, creating impressive rings of fire above the 20 litre pail if flows were too high.

    Breaking all of the Hg thermometers and manometers found on site, producing 177 kg for disposal.

  43. Young Padawan says:

    I did an internship at a major pharmaceutical company. There I met a technician who had been trained probably in the late 90s. She told me about the coffee machine they had on the shelf above the bench. In addition, the senior technicians were avid smokers. Only for extractions would they lay down their cigarettes. And indeed, I went to check out said lab, and all along the bench were the stains that the cigarettes had left.

    During a reunion event, I talked to an alumni of my university who had done his studies in the fifties. I recall they were around 40-50 students. During their introductory lab course, one person died, and two suffered permanent damage to their eyesight. The good old time? I’ll pass…

  44. Ben Zene says:

    Had one of the last undergraduate intro chemistry classes taught be Prof. John Gryder at Johns Hopkins in Remsen Hall. Prof. Gryder smoked when he lectured to the class and would put down his cigarette on the side of the lab bench at the front of the class and pick up the chalk to write on the board. He would then put down the chalk, pick up the cigarette (Pall Malls) and continue to smoke. Someone once complained about the smoking and he told the young woman to go sit at the back of the lecture hall. To wit, he then proceeded to say that despite rumors to the contrary, he had never mistakenly picked up a piece of chalk from the bench and smoked it.

    1. eyesoars says:

      Heh. My grandfather was an organic chemist (Ph.D., 1927?) who got his degree at JHU, I believe before the Homewood Campus (and Remsen Hall) came into being. Died in 1979 at the age of 84 from liver cancer. Specialized in viscose rayon, but did a lot of things for the gov’t during WWII, some of it for duPont, and some of it at ORNL.

  45. Ted says:

    I have plenty of chemistry stuff to look back at (borax bead tests, eugenol from cloves, quenching grignards with dry ice, the stills, etc..), but I am still traumatized by the 50’s era powder diffractometer from P-chem lab. I remember rolling the compound onto the wax coated spindle, loading up the film, then using a broomstick to turn on the machine from the door of the room, mid flight.. . We had a dinky little phosphor plate on the end of a wand that we were supposed to use to check for ‘stray’ x-rays, but I had little confidence in my ability to find them before they found me. The bank of tubes on that thing would fire up in a fashion that would bring a smile to Dr. Frankenstein himself. And then, my God, the measuring…

    -t

  46. exGlaxoid says:

    Boy these bring back memories… Running benzene columns with gallons of solvent. People smoking in the chemical stockroom while pouring solvents. A “hood” being a plywood box with a window box fan behind it. 45-60 students in a lab with two or three hoods running Grignard reactions at one time. People washing their hands in acetone. People heating food on a hotplate/bunsen burner/drying oven. Dripping mercury electrodes in undergrad Analytical Labs. Metal cans of ether for anesthesia used in the lab (some where 10 years old at least).

    Still remember a safety person finding someones Snickers Bars in the biological refrigerator. One guy got in trouble at BW for drying his cannabis in the drying oven. Prep HPLC with ether/hexanes in the middle of a lab with no ventilation (caught fire one day when a leak occured). More prep HPLC in an un-ventilated storage room converted to lab space with acetonitrile, causing several people’s liver enzymes to sky rocket. I have seen cylinders of HF, phosgene, H2, etc sitting in the middle of labs. Solvent stills with pounds of old sodium in them.

    But I know many chemists who did this and are doing well in their 80’s and 90’s, one guy made large quantities of most of the top 10 known carcinogens in his prime years, and is still sharper than many people half his age. So I don’t think chemicals are as bad as some people seem to think now. But the right level of caution should be somewhere between the 1960’s (spray people with Chlordane and DDT to avoid mosquitoes) and now (call hazmat team for a spill of nail polish remover).

  47. David Edwards says:

    Here’s a little snippet that will make some people prolapse …

    Back in my teenage days, one of my chemistry classes involved dissolving elemental sulphur in carbon disulphide. No, not in a fume cupboard (or fume hood as Americans here seem to call it), but out on the lab benches.

    The physics lab just up the corridor had a linear induction motor that was wheeled out for various experiments. Some bright spark decided to use a step up transformer to give it a bit more oomph, and turned it into an impromptu railgun. I think parts of the projectile are still embedded in the wall 40 years on.

    When I was 15, my physics teacher let us all handle radioactive sources for geiger counter work. We got to handle real live plutonium. Admittedly only milligrams of the stuff, and in sealed containers, but it was still real plutonium. Today’s health & safety people here in the UK would pop an artery if this was tried in a present day classroom.

    Let’s see, what goodies were in the chemistry lab back in my teenage days? Sulphur trioxide, potassium dichromate (in litre bottles, no less), a couple of perchlorates, 30 vol peroxide, a couple of small acetylene cylinders, yellow phosphorus, enough concentrated acids to strip the flesh off a bull elephant, though my particular favourites were the various cyanides. Yes, this was the UK equivalent of a US high school I’m talking about here, not a university undergraduate lab.

  48. ST says:

    people used to smoke in my old lab. I still remember my prof using he burner to lit up his cigarette and then make capillaries

  49. nowhere man says:

    I was a chemistry major, but my favorite was from a physics lab class I had to take. We had to set up a thermocouple and use it as a thermometer, sticking it in various boiling solvents. If I remember right, I was supposed to stick it in my mouth after it was in boiling dichlorobenzene or something like that. I let my lab partner make that measurement!

  50. Chris says:

    I did a work experience placement in about ’95 as a student at a small fine chemical plant. On my first day on the job, my boss threw a glass jar for me to catch. It held about half a kilo of picric acid. I also remember using aqua regia there to dissolve samples and asking for safety glasses only to be told “oh, we don’t use those.” I couldn’t get out of there fast enough and the company is fortunately no longer in business as far as I know.

    The ICI site where I worked used to have mercury cell chlorine plants, all long gone now. They had a very old movie of someone climbing into an open vat of mercury – it is so dense you hardly sink.

    My mum was an analytical chemist in the 60’s and 70’s. Lots of tales of washing benches with benzene, acid burns being part of the job… She had a colleague who was badly hurt when she sucked too hard pipetting 880 ammonia by mouth, and a couple of other colleagues who were killed, one of them in an ether fire. A large beaker of ether on a steam bath in a fume cupboard bumped very badly and produced a large vapour cloud. It came out of the hood and hit a lit bunsen on the bench behind.

    Before my time, the old phys chem lab at my university had traditional solid wooden benches and cupboards. One of the experiments used dilute perchloric acid. Over the preceeding decades huge amounts of it had been spilled, slowly soaking into the wood. The consequences became clear when a plumber went to braze a leaking joint under a sink and the whole lab went up in a cloud of smoke. When I studied there they had turned it into a tea room.

    One of my old profs (a wonderful old gent, sadly now departed) had only one eye as a result of an ether peroxide explosion in the 60’s.

    We have come a very long way indeed in terms of lab and plant safety, although we should not use that as an excuse to be complacent…

  51. zenboy99 says:

    Not Chemistry related, but I know of a handful of mechanics in their 60’s who still use Brake Cleaner (methylene chloride) to wash their hands at the end of the day.

  52. OldLabRat says:

    Maybe I missed it in previous comments. How about the lead bench tops that were common in labs built in the ’40s to 60’s? Very low glass breakage rate, easy to clean with a bit of concentrated acid or sandpaper…One didn’t need cork rings for flasks, as a few minutes with a heat gun and one had a nice customized bench.

  53. Wavefunction says:

    Back from my old days:

    Phosphate removal using acid
    Kipps’s apparatus
    Mouth pipetting
    Acid-base titration using phenophthaelin etc.
    Charcoal test for detecting metals

  54. tlp says:

    Second many things mentioned here: mouth-pipetting, absence of gloves (forget about goggles!), pouring whatever down the drain, smoking in the lab (not me, my supervisor), hanging-mercury-drop voltammetry for analytical chemistry, also routinely doing workup out of the hood – all these were reality of my undergrad education.

    Also, routine way of thorough glassware cleaning was (and maybe still is) bathing it in “Chrompik” – a dark-brown solution of chromic acid – which was made by heating a 1-2 L jar of 98% H2SO4 with solid potassium bichromate at ca. 100 C (because otherwise chromic acid isn’t formed, as everyone was saying). Witnessed once 1-L round-bottom flask being used as a replacement for thick-walled jar. Thin glass cracked right over the sizzling-hot heating element producing a mushroom cloud of sulfuric acid vapors and then acidic fog creeping down the hallway as everyone was running away in panic.
    One old PhysChem professor once told a story about his friends from Physics department who were asking for help. They’d got barrels of ethanol denatured with benzene for optics cleaning or whatever. So naturally they were curious if it’s possible to somehow separate pure ethanol out of the mixture (a never-ending research problem in post-Soviet countries). Professor – certainly of that old-school type – suggested to add water just enough to form triple azeotrope and distill it out. I don’t remember how the story ended but supposedly nobody died and professor looked very proud of that idea.
    There was also a legend – or not – circulating at the department about badass old-school stuff scientists chilling absolute ethanol in liquid nitrogen and then spreading the syrupy stuff over a piece of bread and eating that refreshing sandwich. I never had a chance to verify that – just didn’t stay long enough to join those wild parties.

    1. J n says:

      That viscous, sticky phase of barely melted ethyl alcohol is amazing to behold, although I doubt it would stay that way long enough at room temperature to make a viable appetizer spread.

      1. tlp says:

        I think the idea was to have alcohol as cold as possible so that vapors don’t immediately burn the respiratory system; and spreading was more of a ritual.

  55. Rhenium says:

    I won’t speak for any of my own chemistry, but in preparation for a paper discussion I noted that Ralph Pearson (of Hard Soft Acid Base fame) was still with us. Born in 1919, Ph.D. in 1943 he might be one of the last with links that far back.

  56. Eastern Europe says:

    In the undergrad orgchem lab, to this date, we use bunsen burners as our primary heat source. (not those newfangled hotplates!)
    You need to set up a reflux? Bunsen burner. You need to recrystallize? Bunsen burner. You need to heat something gently? Bunsen burner heating your water bath.

    We take safety precautions mind you, it is forbidden for anyone in the lab to light a flame, until all containers of ether are sealed. (RBFs with a reflux condenser attached count as sealed)
    The condensers are cooled by a steady flow of tap water, no water chillers.

    The orgchem lab does not have a supply of DI water, we use tap water for everything that needs water. Washing glassware usually means a combination of tap water, dishwashing detergent and elbow grease, acetone is usually reserved for stuff that does not want to come off, or if you need something to dry quickly.

    We do not use sintered glass filters, filtration either meany gravity filtration or cutting a disc out of filter paper and using a Buchner funnel for vacuum filtration. As a source of vacuum we use water jet aspirators connected to a water tap, no vacuum pumps.

    We still use Kipp’s apparatus for generating gases, including H2S. We do not have cylinders of Cl2, HCl or H2S.

    Since we practice the tradition of “bring your own PPE”, usually a lab coat is all the PPE you see on most people in the labs. (no boxes of disposable gloves laying around, you have gloves if you buy them for yourself, and the standard-issue goggles are typically scratched to oblivion)

    We make our own dry ice, by putting a heavy duty bag over a pipe coming out of an upside down CO2 cylinder, and carefully opening the valve to spray the liquid CO2 into the bag.

    We wash and reuse pipette tips. The chemical waste usually gets dumped into the sewer system, except heavy metals and large quantities of organic solvents.
    Just a quick reminder: all of the above so far is happening to this day.

    I have heard rumors of people cooking food in the fume hood, about half a meter away from reactions in progress, some guy is still using benzene to this day and using all manner of non-halogenated solvent waste to fuel their cars. (eluent mixes from column chrom. etc.)

  57. Rhodium says:

    In some of my Orgo labs class at U MI we had to use cork stoppers, 1967 era. There were sets of cork borers, hollow rods with sharp ends that nested together, and a cork roller to make the corks tapered. I still have a nice scar on my palm from a tube breaking during insertion.

    1. GladToMoveToProcess says:

      In the late ’30s, my father had a tube break while putting it through a cork or rubber stopper; the broken tube went straight through the palm of his hand. Off to the clinic. To add insult, he got a zero for that day’s lab.

      1. CR says:

        I remember having to use the borers to make holes in the large rubber stoppers and then try and get a glass tube through. A little bit of grease helped, but not sure how many were broken – nor how many scars from trying to get that borer through the rubber stoppers (this was ca. early 90’s).

  58. Noni Mausa says:

    Not chem labs, but

    — our biology lab tech kept a half opened bag of sugar under the counter. It was to catch cockroaches (!) to feed to the leopard frogs. I believe that was all the feed they needed.(!)
    — our electrical wiring teacher in college used to test whether a circuit was 115 or 220 volts by touching his thumb and forefinger across the circuit.

  59. Patrick Sweetman says:

    Jack Johansen, if you are still out there, I still remember mouth-pipetting pyridine for our nonaqueous titrations lab, but I confess to being the rogue who surreptitiously prepared iodoacenone and poured it into the long bench central drainage trough, sending the whole class into tears.

    1. Patrick Sweetman says:

      iodoacetone … saturated iodine in acetone, add a few % conc nitric acid, warm until efforvescence & colourless. Warning … lacremator. Procedure discovered by accident just messing around. Those were the days.

  60. Anonymous says:

    Another cigarette in the trash can pfoooof! : R B Woodward was a chain smoker. When he visited the lab, he would flick the still smoldering butts into the trash can. (He was a good shot, they say.) One day, the guys laid down some ether in the trash can (heavier than air; sits there waiting … waiting … waiting) and when RBW flicked the next butt, pfoooof!

    Another mercury comment: liquid mercury isn’t toxic when ingested because it is not absorbed. There are many case reports in the medical literature. I forget the record amount. Probably 1 liter or more. They like to include X-rays in their case reports. (I can’t find a single one at the moment. Damn paywalls!) The treatment was usually to let it pass. I don’t think that touching mercury in a bowl with your bare hands is a big risk. But why tempt fate? Breathing Hg vapor is a different matter. Here’s a video of mercury ingestion. If you think this guy is crazy, do you think he was crazy BEFORE being exposed to the Hg or became crazy afterwards?
    https://www.reddit.com/r/videos/comments/3uxvez/this_guy_is_drinking_mercuryrip/?st=j9upi61u&sh=7ddbf516

    Quenching metals: (The safest quench of excess hydrides LAH, DIBAL, etc, and organometallics BuLi, PhMgBr, etc. in my opinion is EtOAc (or EtOAc diluted with hexanes). You get ADDITION rather than the formation of H2 or BuH or PhH). Reactive metals also react with EtOAc to form the acyloin (faster with heat). Since large amounts of Na and K are or were often used in stills, you are all set up to add small amounts diluted EtOAc to your still and continue refluxing until done. Same deal: no formation of H2.

    There’s another one for the history books: solvent stills with Na, K, LAH, etc. have been replaced by Grubbs Columns in many labs. Boring.

    Almost anything from “Excuse me, Sir. Would you like to buy a bottle of isopropyl bromide?” and “Ageless Gergel” by Max Gergel. (“Send Preacher!”) And other exciting chemistry from “Ignition!” and “The Green Flame.” All gone.

    I used to keep a small nalgene bottle of dilute (~1%) HF at my sink to clean the dirtiest glassware. Worked great!! And I never had a problem of any sort with it.

    An old school bio experiment by Nobelist George Wald:
    AN EXPERIMENT IN HUMAN VITAMIN A-DEFICIENCY
    By GEORGE WALD AND D… S….
    “The first observable symptom of vitamin A-deficiency in man and other
    mammals is a rise of visual threshold known as night-blindness. […] The present paper describes the results of a second experiment in which identical observational methods were employed. The subject D. S. is 22 years of age, 5 feet and 10 1/2 inches in height and weighs 155 pounds. […]” Good old volunteer “D. S.” went on a Vitamin A deficient diet until, “On the 34th day of the deficiency the cone plateau had risen 3.4 times, the rod plateau 9.1 times above their average normal levels. […]” (D.S. survived and his vision was restored with Vitamin A.) Any current volunteers to test your latest drug concoction?

    1. J n says:

      Had an elementary school science teacher who coated his wedding band with mercury one day. Then he wore it around, playing with it till school let out.

  61. Christophe Verlinde says:

    In my third year of pharmacy studies a few of my class mates decided to use the muffle oven, normally used for calcination of samples at 800 degrees Celsius, to bake a pizza. They said it was tasty – I politely declined.

  62. TJ says:

    Warming pies in the glass drying ovens… The wall of stills with plenty of Na, wooden cupboards full of 2.5L solvent bottles. Cleaning the stainless steel fume hoods with Nitric acid. University Chemistry dept. parties with punch made with copious amount of absolute EtOH and a dash of orange juice.

    Organic chemistry seminars with wine tasting using glass beakers…

    Happy days.

  63. physbio says:

    Late ’70’s lab tech in phys biochem lab – old analytical ultracentrifuge would balance in cup of mercury as a sensor. Would run for hours. Any jolt to building, or lack of balance, would drip mercury all over the floor. Much tin foil was used.

    Same lab, fixatives for electron microscopy. Osmium Tetroxide on a lab bench. Lots of black spots everywhere (including on some fingers I knew – but not mine as I always gloved for the event).

  64. J n says:

    Back in science and math boarding school, a friend of mine and I engaged in dorm room “windowsill chemistry’ with the great outdoors doubling as our fume hood, generating clouds of nitrogen tetroxide and creating long lasting multicolored stains on the sidewalk below. Like other folks over the years I learned that you just wipe conc H2SO4 off your hand, and nitric acid stains your fingers. My buddy had a plastic dropper bottle of HF as part of the “chemistry set.” During summer break he mailed me a box of somewhat carefully packaged reagents. Obviously there was HF in that too.

  65. Wheels17 says:

    With regards to David Edwards comment:
    “When I was 15, my physics teacher let us all handle radioactive sources for geiger counter work. We got to handle real live plutonium. ”

    No plutonium for me, but between 8th grade and High School(1968), I took a summer course called “Radiation Biology”. They’d ordered radioisotopes for us and we fed them to frogs. After a few days, we pithed the frogs, dissected them to obtain their internal organs, digested the organs in fuming nitric acid, and used a Geiger counter to count the digested samples vs. controls to determine which organ accumulated which radioisotope and at what level. Really cool.

    Not a single step that could be done today.

  66. Scott says:

    late 1990s, working as an aircraft mechanic. We used lots of Methyl Ethyl Ketone (MEK) for cleaning parts and otherwise removing polyurethane epoxy paint. With latex gloves for PPE. For those that haven’t had the pleasure, MEK dissolves latex gloves in seconds, and is detectable on your breath in less than 30 seconds after it hits your hands. Big surprise, I am now latex-sensitive, break out in hives if I wear latex gloves. At least I made out better than one of my co-workers. Poor dude actually went straight-up anaphylactic to latex. Made multiple trips to the hospital before the shop finally got rid of all the latex gloves.

    I still use brake cleaner to clean gun parts, works great at getting all the old oils and powder buildup off. You do need to oil more heavily than usual after using brake cleaner, though.

  67. Dave_N says:

    Brings back “happy memories” of distilling phosphines in a standard Liebeg watercooled condenser with a nitrogen bleed. You knew when the phosphines were coming off by the delicate violet flame at the edge of the nitrogen/air interface. We collected in 10 ml soda glass vials and then flame sealed them. Ah for those carefree days of yesteryear!!

    Or since I had an UK firearms licence (early 1960s) staying back 20 metres and blowing up Winchester quart bottles filled with organometallic residues with repeated 0.22 LR or 9 mm bullets. In place of lab assistants hurling stones at them. The local police knew what I was doing as they were some of the people I target shot against, and suggested that I should do the job!

  68. David Edwards says:

    In reply to Wheels above … I have to admit that dissecting radioactive frogs was one thing missing from my curriculum, but among the other weird things that *did* form a part thereof, was dumping a nice conical pile of Potassium Dichromate on an asbestos mat, sticking a magnesium ribbon in the top and igniting the ribbon, thence watching the thermal decomposition of Potassium Dichromate produce a nice volcano turning from orange to green. A version of the same experiment with Ammonium Dichromate can be seen here:

    https://www.youtube.com/watch?v=Ula2NWi3Q34

  69. SSG says:

    If you would look up – there is a Org Synth procedure for the generation of HCN. If you think that’s scary, one of the Notes recommend that the person generating HCN (glad I never had a need of it and wasn’t tortured enough during my PhD days to have explored the idea) should smoke. Apparently nicotine and HCN makes a peculiar taste. Wonder who found that out! The submitters or the checkers!

  70. SSG says:

    Should also mention what (late) Merle Battiste [the first PhD of (late) Breslow and post-doc of Saul Winstein] told me during my grad days at UF: dicyclopentadiene, which he used to regularly crack in his laboratories since he was working on norbornanes, caused a divorce like situation at home.

    1. ddd says:

      That’s easy the believe. If my spouse came home every day stinking of dycyclopentadiene, it would take all of a week maximum for him to get kicked out.

  71. Biotechtoreador says:

    Stills with blue (or, better, purple) benzl ketyl going 24/7…..really just pretty.

    1. Anonymous says:

      Since replaced by Grubbs columns or commercial Dry-Seal bottles. ;-(

  72. dearieme says:

    In one of my undergraduate lab classes I didn’t like the instructions much so I redesigned it so that the toxic stuff went into the burette and the merely nasty stuff into the mouth-operated pipette. The lab supervisor strolled by and told me I was doing it wrong. I explained that, on the contrary, I was doing it better. He said I was a coward. I said I preferred that to being a bloody fool. A couple of the postgrads who helped him in the lab watched and listened with fascination.

    I may have taken a pace towards him, or perhaps I’d raised my voice; at any rate he scuttled away. The next lab afternoon the same postgrads were present but a different professor showed up to supervise. I was rather pleased. I had seen a change of lecturer in physics when a class’s bombardment of insults and thrown objects had driven a dud out. Now I’d seen a single undergraduate change the supervision of a lab. Excellent: it makes no sense to waste your youth being subjected to bad or dangerous teaching.

    I prefer that sort of thing to the wind and piss tradition of student protest.

  73. peptoid says:

    Only a few years ago, but anything remotely dangerous is being progressively phased out of our undergraduate labs. Hydrogenations are out, even though we had a purpose-built manifold for students to come and fill their own bombs. Up until 5 years ago we were doing refluxes in toluene on the bench (which becomes quite stifling on a 40 °C Melbourne day).

    There was one prac that involved a reflux in glacial acetic acid, and one of my fellow students forgot to put anti-bumping granules in (he insists to this day that he did). The brown gunge ended up on the ceiling, three and a half metres above the bench and we cleared out the lab until it stopped smelling like fish and chips. The best part was that the ceilings had just been painted the previous week, the first time in about 30 years.

    We’ve also been threatened with the loss of TFA from our peptide synthesis prac sessions. First a lab manager spilled some on her leg, then a student spilled a drop on her finger. Lab demonstrator notifies supervisor, supervisor notifies lab manager, lab manager notifies campus nurse, campus nurse calls fire department. Fire department are not impressed. Supervisor drives student to hospital where, five hours later, attending doctor can’t even see which hand was burned as it was so minor.

    1. kriggy says:

      Thats quite interesting actualy. We had few 50%TFA in DCM burns in our department and those are quite nasty. Not realy huge amounts but just few drops on elbow or finger

  74. BJK says:

    My undergrad advisor did his PhD in organophosphorus chemistry. He said they used to spray themselves with ozone every day to oxidize any phosphorus-based crap stuck on/in their clothes.

  75. metals wrangler says:

    Chromerge…dropping mercury electrodes…Open bench Grignard. That was quite enough.

  76. Piero P says:

    Analytical chemistry lab, CCl4 in test tubes on the benches to test for halogens and H2S from an open-access valve on the wall or cylinder to precipitate cations
    Common sodium “spaghetti-machine” in a common corridor, nobody’s responsibility and left unclean after each use…

  77. Design Monkey says:

    Chem department in sparsely populated university campus about 30 years ago. Solvent waste disposal procedure. Given: shallow iron box approx 3 by 3 foots behind the building. Pour your waste there, throw a match in. What did not burn, just leave it there to evaporate on it’s own.

  78. HGMoot says:

    All the above just makes me feel better… and, BTW, my colleague who during the 1980s worked for 6 years with steroids that were only soluble in PhH and he washed his glassware in that stuff on a daily basis… he is alive and well, in fact better than many others his junior.
    I also know very well (…) a person who evacuated entire chemistry department by generating MeSeH when the exhaust system there happened to be malfunctioning..
    Now, MeSeH, that is really nasty stuff. Avoid, short it…

  79. Roy S says:

    Dad used to bring home benzene from the lab and chuck it in the lawnmower gas tank to get rid of it. I remember being surprised as a youngster when a glass bottle of it froze in the garage and didn’t burst. Dad laughed and said that was because it was a ‘normal’ liquid.

  80. Chris Kirk Speaks says:

    Only once did I mouth pipette, and the chemistry gods struck hard. One summer in the 90s I did analytical work for an environmental lab connected to a university in west Michigan. Only a couple of weeks after starting we moved to gleaming new digs. One morning I came in early to perform a simple nitrite test. But I cannot find a bulb anywhere. Impatient, I mouth pipette. Unhappily, the gleaming new lab had gleaming large windows looking out into the hallway – and who should walk by but the Dean of Arts and Sciences. (My colleagues had a sense of humor about it: at the end of the summer they presented me with my own pipette bulb, with big paper lips attached!)

    Adding insult to injury, the nitrite test never came out right, and it came to me – I had eaten sausages for breakfast, stuffed with sodium nitrite. Never will I color outside the lines again!

  81. dave w says:

    Freshman chem lab, 1975, preparation of CrAcAc (chromium acetyl-acetone complex, we pronounced it “crack-ack”)… the workup involved dissolving the crude product in the minimum quantity of hot benzene, then adding pet. ether which would cause the CrAcAc to crystallize out: we were told that it was important to have the benzene as hot as possible, or the solution wouldn’t be concentrated enough to yield the desired crystals. So there you have the fume hoods full of first-term freshmen, boiling benzene in beakers on hot plates…

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