Author Topic: Your Really STUPID Lab Mistakes....  (Read 13486 times)

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Bozakium

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Oops.
« Reply #100 on: July 30, 2004, 11:44:00 AM »
Ha cha cha I got a million of 'em!

--When really young, making oxygen with MnO2 from dry cells and H2O2. Dumped in the H2O2 too fast and whoosh! and 25 years later my mom still brings up the black shit all over the ceiling.
--One of my fave substances is NI3.'Nuff said.
--What sucks waaay more than getting hurt by forgetting theres a BIG pile of NI3 drying under too many household items to remember?(glass ashtrays, toilet seat legs, etc.) No ,not losing friends who got 'pranked', It's thinking of all the pounds of iodine crystals I bought OTC back in the day, that got wasted making fucking explosives!!
--My cousin still has metal in his elbow as a result of the equation: flash powder + steel gas can + gin --> bad things
--Someone gave a good tip not to throw out miscellaneous liquids until the rxn is complete. Who forgot to tell me to label them?
--While on that subject, one time I has a flask half-full(not half-empty) of solvent saturated(?) with pre-product that just refused to crystallize. It went away to the basement box of "extra chemicals I don't need but can't bear to throw out".Unlabeled of course. Four or so years later, while cleaning out said basement, I come across said flask, lo and behold full of nice white prismatic crystals! At least I remembered what they were. I decanted the supernatant liquid, rinsed, reacted, basified and began the product distillation. The phone rings. Need I say more? At least the burnt mess smelled nice.  :)
--In organic lab class, we used to get OJ from the vending machine to mix with the absolute ethanol. It comes in the same kind of metal can as ethyl acetate.
--Filling the house with nice yellow gas. Chlorine gas. At least it was germ free!
--(probably drinking, and hands/sleeves soaked with gasoline from indoor motorcycle maintenance), noticing the river of hexane/pentanes running 10 feet across the kitchen floor right toward the gas space heater. In one fell swoop, in slo-mo I simultaneously: 1-envisioned the entire room going whooopff, and myself engulfed in flames 2-dived for the gas shutoff valve behind heater  3-swiped towel off counter and into sink  4-in mid-air, while passing sink, slapped the faucet on full  5-coming in for a landing, whacking the gas valve to off  6-skidding into the bathroom, cracking my head on the vanity corner
  Jumping to my feet while still seeing tweety birds, I realized the pilot light was still on. As I dropped frantically to shut it off, I saw that the ceramic thingys inside the ancient heater were still orange-hot. I think it took me an extra .001 millisecond to get that wet towel on the floor just in time to blanket and intercept the hydrocarbon River Styx.

CharlieBigpotato

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fulminated silver
« Reply #101 on: August 07, 2004, 08:44:00 AM »
friends were having so much fun w/ fulminated Hg; why not Ag?
bad idea. swim's pal still has chunks of porcelin imbedded beeneath his skin. they look like blue chesse. doc didn't think thy were worth removing. he quit foolish experiments after that.

here's one that still amazes me:
in attempt to fine-tune a flask of hot HI, gassing out, swim adds a tiny pinch of fresh snow, thinking it would bee a way to deliver less than a drop of H2O; and it was, actually.
too bad it cracked the flask, instantly.

dumber-yet:
swim tosses an acetone soaked filter paper into a wood stove; flame ignites  low lying fumes that jump all the way to another table with final dream in another filter with tiny amt. of acetone still evapping. dream and paper go up in flames.

swim didn't think those vapors would bee so heavy. it was less than an ounce of acetone. such a surprise.

nautilus

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Inert
« Reply #102 on: August 08, 2004, 08:35:00 AM »
I was pretty proud of my HCL gas-generator: A suction flask with a pressure-equalized addition funnel on top of it (with a perfectly-fitting rubber ring), going to a non-improvised drying tower, with a silicon rubber tube to go into the pyridine.
I was going to gas the pyridine to get the pyridine.HCL, used for eugenol demethylation.

I forgot to use the glass gassing-tube, putting the silicone rubber hose directly into the pyridine. That day I learned that the wonderfully inert silicone rubber *dissolves*  :o  in pyridine (or pyridine.HCL, whichever).
In short: Doh!

To top it off, I actually had the glass gassing-tube in my hands a few times while preparing the drying tower  :-[ .


armageddon

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lachrymator...
« Reply #103 on: August 17, 2004, 03:34:00 PM »
Recently SWIA replaced his huge, superb double-surface condenser with a self-made one and attempted a grígnard rxn with benzyl chloride using in-situ drying. He added 1/4 of the benzyl chloride solution and everything went fine first, only that the rxn started a bit later than usual - until SWIA started to add the remainder dropwise. Unfortunately the BzCl solution wasn't absolutely dry, causing the rxn to subside upon adding the BzCl-soln. So SWIA added at a faster rate...

...and suddenly everything began to reflux *really* vigorously - the BzCl became dry and started to react, unfortunately SWIA already had added 2/3 of it...

...his homemade condenser was connected to the rxn flask with rubber stopper/glass tubing - bad idea...

Big pressure buildup, lots of boiling ether collecting in the condenser rather than flowing back into rxn vessel - and before SWIA could react, the expensive addition funnel shot to the ceiling, where it burst into myriads of little glass pieces and gave a shower of ether and benzyl chloride, while the pressure release inside rxn vessel caused the ether to boil away and spilled more BzCl/grignard complex/ether around the rxn vessel...

After 2 minutes of cleaning with EtOH-soaked paper and sealing the lab door with water-soaked towels, the effects of the BzCl caused SWIA to leave lab space with red face, tears in his eyes and coughing like a 80-year-old, heavy cigar smoker..

The laboratory was not trespassable for at least six days, not to speak of the REALLY expensive addition funnel and the picture SWIA gave when jumping out of his window (remember he sealed the lab door), while looking like having received a healthy amount of pepper spray (his thought while leaving through his window was "elvis has left the building.." BTW) - and you surely can imagine SWIAs paranoid imaginations of men in yellow pressurized protection suits with breathing apparatus, walking towards him, telling him "You're arrested" with darth vader's voice, as soon as he would return to ground zero  ;D  - but luckily nobody even noticed his accident......

(hopefully nobody did see him jumping  :) )

Benzyl chloride is GREAT fun!!! As long as it cannot exit the rxn flask...

Grignard reactions with ether are fun, too - you JUST have to use an appropriate condenser with wide inlet to avoid pressure buildups...

Best thing about it: SWIAs nostrils were cleaned up very thoroughly, and he really enjoyed how his sense of smell returned after just three days... ;)

Greetz A


Bandil

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Fun with DOB
« Reply #104 on: August 17, 2004, 09:49:00 PM »
While working in the evening before a day where I had to get up really early and be usefull the whole day, I ended up doing something incredibly stupid. The next day was full of official meetings where Bandil was called for in a suit with a big smile and a seriously functional brain. Approximately 5 grams of DOB was dissolved in 100 mL DCM in a 250 mL RBF and stood around on the floor. While working on another project I suddenly (a real DUH moment - of course you end up kicking stuff if its on the floor) kick the bottle, shattering it into a million pieces soaking the floor, my socks and everything else in a concentrated DOB/DCM mixture. I immediately removed my socks and proceeded to clean up. An hour later I was getting a little jittery and after two hours, when I attempted to sleep, I realized that that just wasn't going to happen. I'd say that I had gotten about 1 mg of DOB in my system, which didn't exactly improve my sleep that night a great deal.

The next day was only survived by ingesting some pretty efficient uppers - and getting some called for sleep in the night!

Kids - don't put DOB on your socks, because its a really dumb thing to do  8)


ChemoSabe

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Glass Cannons and Xylene Geysers
« Reply #105 on: August 26, 2004, 07:59:00 AM »
Swim has had several shocking incidences in which a certain vac adapter was used in a steam distillation setup and usually involved huge blasts of hot steam being blown into the room.
 
In one one of these incidents the great pressure created by the steam from the pressure cooker blew the 24/40 glass stopper off of the top of the vac adapter like a cannon. Luckily no one was killed and nothing was broken but the force with which it was fired was easily enough for it to have done some major damage.

I don't even recall what was being done when the xylene geyser blew like old faithful. But blow it did and it made a large splatter patten on the ceiling directly above where it occurred. The upside of it was that the hotplate used had some stains that seemingly could not be removed but this boiling xylene treatment it got made it look like it was brand new.

Also I learned in quite a dramatic fashion that when redistilling used acetone not to add boiling stones to it after you've got it heated up. Nearly a whole liter of near boiling acetone vacated a large flask almost instantly and then evaporated almost as fast.


armageddon

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kicking flasks pt. 2
« Reply #106 on: August 26, 2004, 05:56:00 PM »
Well essentially the same thing like happened to Bandil:

Some twenty grams of already purified product (not as active as DOB though  ::) ), still dissolved in a small amount of DCM in evaporating flask, SWIA placed it in a cork ring on the floor cuz he had no place left on the table (SWIA is a busy guy you know  :) ), a friend, trying to help, misunderstands SWIAs instructions on how to simply switch off the rotovap - and as SWIA is a bit impatient sometimes, he moves one step, to be able to show his friend how to switch off apparatus - and bang! Heavy-walled flask is history, - and after swearing like a sailor and wiping up everything and extracting the tissue paper followed by re-purification, SWIA still was able to isolate 4.5g of product again.  >:(
And a new property of the product SWIA didn't realize before: it is pretty good in cleaning linoleum lab floor! The place around ground zero looks like noone had ever stepped on it! (and this is not due to DCM which already was spilled several times without same cleaning effect!)

 - guess SWIA will stick to standard cleaning methods though; this one would become a bit expensive if done regularly!  ;D

Greetz A


Rasputin

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My Own Fun Times With Xylene Geysers
« Reply #107 on: August 29, 2004, 01:01:00 AM »
Hey All:

Back, quite some time ago(about a year or more), I was washing the dilluted, post-reaction fluid from an HI/RP cook with Xylene. There was about 400mls of fluid plus, 400mls of Xylene, in a 1000ml RB flask. I, at the time, was into the habbit of using boiling hot solvents to wash with. I usually heated them up in a seperate container, then added them to the post reaction fluid. This time I had the great idea of making it easier by doing it all in the same flask. I added the Xylene and, being impatient, turned the heat up to max, and waited. For about 5-10 minutes there was no bubbling, no nothing. Now, I had a friend over to keep me company and we where smoking weed(I know, this whole situation is just destined for something teribble hapening). My friend walks over to me to pass the joint, I looked over at him to take it, as I look back to the flask it suddenly erupts. Almost all of the Xylene and about half of the reaction fluid shoots straight out of the flask, six feet to the giant light on the ceilling, hitting the round/domed shaped diffuser its atached to. The susequent result was an all encompassing dome shaped shower being rained down on us.

 Aside from being covered in crap, I was all right, my friend however was not, he was not wearing any eye protection(except for just having walked over, he was on the other side of the room all night, so he figured they where not necesary, I agreed, since he wasnt near anything). He had been hit dead on, in both eyes with Xylene and post reaction fluid, not good to say the least. Now I keep a kit of emergency stuff for these kinds of occasions(baking soda,respirator,eyewash,etc), so I scrambled over to get it, only to find that the eye wash(for some reason?) was empty. I ended up having to lead him, quickly as possible up stairs to the shower, and stick his wyes into the stream for about 4-5 minutes. The burning finally stopped but, it took us about a full minute or more to get him upstairs and into the shower. Now is where the story gets kinda interesting, a few minutes after he stopped washing his eyes, they covered over with a sort of skinlike plate(like the stuff you get on contacts if you fall asleep with them in, is the best description I can give), he just reached into his eyeball and peeled it off like a sticker and every hour or so for the rest of the day it would keep re-forming. He was not blinded, or anything like that, in fact he had no vision problems at all(lucky fucker). What did happen though was(well at least he claims it did), he was spun out of his mind for about two days. I figure it could be possible from the HI eating through the outer layer of his eye, and getting absorbed through the cappilaries, Ive heard of peole dosing LSD the same way, and the HI/Xylene was in his eyes for a minute or more, maybe it was long enough to eat its way in, even in its dilluted state. Needless to say my lesson was learned, I looked up bumping and boiling stones the next day and, eyewear is mandatory for all from now on.


Lestat

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I just had a very small scale pyrotechnic...
« Reply #108 on: September 01, 2004, 08:04:00 PM »
I just had a very small scale pyrotechnic experiment (done in a table-spoon) go rather spectacularly wrong, I was fooling around, and fused some ammonium nitrate into a liquid, I have been trying to determine the product from this reaction for some time w/o disaster or success.

Anyway, I decided to pre-heat the lanthanum I was using BEEFORE adding it to the NH3NO3, and guess what! instead of oxidising fast but stably, I heated the lanthanum chunk to red heat, then added it to the spoonful of NH2NO3.

It exploded in my face, spraying molten ammonium nitrate and red hot, vigourously oxidising lanthanum all down my shirt, burning the crap out of it, and all down my hand that held the spoon, I now have painful blisters all over my hand from where the molten nitrate exploded out of the spoon, lucky I was wearing my glasses at the time otherwise I would probably have been in serious shit :(


metalgirl

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"super heated water"
« Reply #109 on: September 26, 2004, 02:45:00 PM »
Alright...after many days of work I was about half an hour away from seeing about 4 grams of meth which is alot for me. The reaction fluid had been cleaned and I thought it would be good to reduce the volume a little as to acommodate the np in the beaker so i place it in the oil bath and eagerly wait for it to start boiling...You know how it is; time slows down and the deeper parts of your brain try to warn you....the beaker sat in the rather hot oil bath for a heck of a long time without bubbling and just as my brain very slowly articulated the words "super heated water" i touched the beaker causing a volcanic expulsion of said meth all over the ceiling, walls floor and my face....strangely enough i wasnt burnt in the slightest... i was very alert for the next 30 hours though.

metalgirl

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while i'm at it
« Reply #110 on: September 26, 2004, 03:08:00 PM »
I usually have a bottle of cleaning vinegar sitting in the lab as to neutralise any caustic shit i may get on my skin...works a treat but boy does that bottle look like my distilled water bottles...can't remember exactly what i was trying to do(some step in working up a rp/i meth cook) but boy howdy, vinegar shurely wern't not supos'dta be in dare....god it took a long time to fix...
       oh yeah, my vinegar bottle now has the words "vinegar stupid" writen in BIG letters on every face of it, including the cap...