Author Topic: Your Really STUPID Lab Mistakes....  (Read 13733 times)

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madprosr

  • Guest
got another one already...
« Reply #40 on: December 12, 2002, 06:30:00 AM »
swim setup to gas about 3g mdma by dripping HCl onto H2SO4, generated a bunch of gas, then each drop of HCl produces less and less. swim got to the point where adding HCl did not produce any new bubbling. finally he figured out that the H2SO4 was all consumed...

so he pulls off the HCl addition funnel, stops stirring, adds a few ml of h2so4, and it volcanoes. it started bubbling out of the claisen adaptor, so he dropped the addition funnel back in to plug it. bad move, in 2 seconds the addition funnel shoots up in the air, spewing acid behind it, and breaks. should have used a stopper. plugged it with a stopper and somehow enough gas comes out to finish the job.

dammit, think man, use that cerebellum.

scram

  • Guest
"he leaned over the setup and examined it.
« Reply #41 on: December 12, 2002, 11:55:00 AM »
"he leaned over the setup and examined it.  Before he knew it, the addition funnel on top of the setup shot up to the ceiling like a rocket and completely shattered.  This was followed by a geyser of mercury containing rxn mixture that subsequently landed on him and a worker standing behind him." Ha ha! Ive experience this more than once. Don't worry about the mercury... a Chemistry Head at a major University and some English grad student who brought me to him were conversing on what to do with the salt. The grad kept asking the Head if it should be reduced to make it safer (why???). The Head told me that although I was properly disposing the HgCl2 by bringing it to them that even if it got into the water system that the HgCl2 would harmlessly pass through the kidneys unreduced to elemental mercury. I almost laughed because this was completely opposite of what I learned from this sight.
   I've got all of you beat with the dumbest of all mistakes. Was cooking naked while pouring off HCL enriched acetone  off some crystals. The fucking pan was tilted too quick and a significant amount of this liquid splatered all over my genitalia. This was soon to become the absolute worst physical pain I've ever felt. I could feel myself going to into shock as I started to become dizzy and light-headed. The only thing available to somewhat neutralize it was Ajax (sodium carbonate and some other bases). But it just made it worse. I started to remember that soap is slightly basic and after 20 minutes of excruciating pain associated with rinsing balls with extrememly cold water I had genly rubbed soap on them as a cream and balls turned from hot fire and gave new meaning to "Blue balls"
...Dont cook naked.

odin

  • Guest
Water and sulphuric acid
« Reply #42 on: December 28, 2002, 12:31:00 PM »
Imagine a big flask (aprox 6 L vol) with a lot of table salt in it, Claisen adapter and addition funel full with H2SO4, gassing aparatus. When I tryed to put funel at the top, it broke and all acid was in table salt. What to do!!!, make a bigger shit from shit. Took a large container full of water and aded to the mix.
Dont do it, I lighty burned my skin, my close...

Bandil

  • Guest
During the extraction of MDP2P from hot 15%...
« Reply #43 on: January 10, 2003, 09:07:00 AM »
During the extraction of MDP2P from hot 15% sulfuric acid somthing went quite wrong... I decided that the hot 15% acid w/ some organic remains in it, was cool enough for the DCM. The DCM was added and it did not really boil, so i thought: "Hey its just below 40 dec c., cool) and put the lid in the flask and shook. The valve was a little tight, so i just removed the cork, which resulted instat volcano/overboil of superheated DCM and sulf. acid shot out all over the place. Luckily it was snowy outside, so i just had my friends clean me up :)

The lab look like a -real- lab after this... No one got really hurt, so i quess it was kind of "nice" to get a reminder not the get cocky in a lab!

Regards
Bandil

pHarmacist

  • Guest
Bandil; hahaha!
« Reply #44 on: January 10, 2003, 09:11:00 AM »
Luckily it was snowy outside, so i just had my friends clean me up :)

LOL!!!



siloxane

  • Guest
Who was it (about 2 years ago) that was vacuum
« Reply #45 on: January 10, 2003, 03:01:00 PM »
Who was it (about 2 years ago) that was vacuum distilling 6L of formic acid in with an Erlenmeyer?
Apparently it made a nice mess when the flask imploded.

yellium

  • Guest
That's just asking for a Darwin Award.
« Reply #46 on: January 10, 2003, 03:07:00 PM »
That's just asking for a Darwin Award.

Sunlight

  • Guest
Lucky
« Reply #47 on: January 10, 2003, 05:51:00 PM »
I've been very lucky too with all my stupid and hazardous mistakes in the lab. Many years ago, when I didn't know that the Ritter rxn doesn't work with safrol, I tried it with HCN. I was dropping H2SO4 over a NaCN solution to bubble the HCN inside a solution of safrol and sulfuric acid. When it was starting the gas production, I tried to correct a possible bad joint in the glassware, and the glass tube was broken, and HCN was flowing in the room. Fortunately it was in a individual country house, I went out with my dog  and a few hours later, I came in again...

Wargasm

  • Guest
Water in hot oil bath
« Reply #48 on: January 16, 2003, 10:00:00 AM »
Well swim is just having a great time.  Last night my 6L sep (a rather expensive piece of glass) mysteriously broke at the neck when I lost control of the stopcock end.  Thank god (the deity, not the bee) I can have a friend repair it.

But I just topped that for stupid.  How about disconnecting the hose to the condenser on a vac dist rig... with the cooling water pump still running?  Sprayed water all over the rig, including the oil bath... which was still hot.  Oil splattered all over when the water flashed to steam, and I was lucky to not be hurt.  I would say the lesson is to pay attention, even with something that appears to be simple.  It isn’t.
Swim's record for the highest number of open stopcocks in a single day -7.



yellium

  • Guest
>...taking hoses from cooling adaptors...
« Reply #49 on: January 16, 2003, 10:37:00 AM »
>...taking hoses from cooling adaptors...

Ah. IME, it was always the _other hose_ that you needed to take off. Because when you took the hose which you thought was the correct one, the other one annoyingly decided to suck up a last gulp of water, and throw it out the now open end of the condensor. Yup, right in the oil bath.

Wargasm

  • Guest
Other hose?
« Reply #50 on: January 16, 2003, 10:47:00 AM »
The other hose?  I don't understand.  What I normally do is stop the pump, pull the return line partially off the return condenser nipple (the higher one) to allow the water to gravity drain back to the bucket (so air is in the condenser), lift the pump out of the bucket and remove the other line from the nipple.
The problem is that I forget to shut off the pump; it was still pumping.
I'm self-taught, I may be doing this wrong, so any info you have is appreciated.



yellium

  • Guest
AFAISee you don't do anything wrong.
« Reply #51 on: January 16, 2003, 10:59:00 AM »
AFAISee you don't do anything wrong. It's only that I've had situations were hoses were unknowingly folded up, or had other reasons to 'not cooperate'.

Wargasm

  • Guest
hosed by hoses
« Reply #52 on: January 16, 2003, 11:26:00 AM »
Hehehe
Once I accidently switched my vaccum hose with my condenser inlet.  It was great, I pumped water directly into my recieving flask.  Thank god I didn't turn on my vac, I would have sucked water into my nice rotery vane pump.

I have an emergency all power shut off switch at the exit of my lab.  It came in handy this morning.  I'd recommend it to other bees, it realy can save your ass.


Rhodium

  • Guest
Hoses should be idiot-proof
« Reply #53 on: January 16, 2003, 12:49:00 PM »
I have mixed up my hoses several times, pumping water into the recieving flask, into my vacuum pump or onto the bench or floor etc.

hCiLdOdUeDn

  • Guest
stupid mistakes
« Reply #54 on: January 16, 2003, 02:23:00 PM »
Recently I had distilled off some solvent from a ketone extraction on an oil bath. I let the flask cool off and i took the flask out of the oil bath. I picked the rb flask up with my hand and it slipped out of my hand. Luckily I grabbed the top of the neck and caught it, but upside down with ketone dripping everywhere  :( . Saved my glass, but lost my ketone! >:(  >:(


yellium

  • Guest
Of course, the same thing also goes up for...
« Reply #55 on: January 16, 2003, 02:42:00 PM »
Of course, the same thing also goes up for working under nitrogen-- try filtering something through a schlenk filter and forgetting that your standing at the _other_ side of the valve, and therefore turning a valve clockwise isn't going to do what you expect it to do...

('so, this line should be nitrogen....d'ooooh!!')

And let's not forget the famous 'washing flask that decides to suck it's contents into your reaction flask.'

yellium

  • Guest
Another goodie: reactions with a tendency to...
« Reply #56 on: January 16, 2003, 02:51:00 PM »
Another goodie: reactions with a tendency to bubble. A LOT.
Those are real fun. If you stir harder, you'll break up the bubbles, but at regions of stirring speeds you also speed up the reaction, forming only _more_ bubbles. Of course, 9 out of 10 occassions this ends up with plastering your fumehood with psychoactive material.

(anyone with runaway Al/Hg adventures?)

abolt

  • Guest
Using a cheap Hydroponics inline fan as a fume
« Reply #57 on: January 16, 2003, 05:43:00 PM »
Using a cheap Hydroponics inline fan as a fume hood for dissolving Palladium in Aqua Regia. The fumes melted the fins and seized up the fan filling the garage with toxic fumes.
It was around this time that i realized that i had a bit more reading to do :-[

iloveshulgin

  • Guest
Left a ketone distillation unattended and...
« Reply #58 on: February 01, 2003, 09:58:00 PM »
Left a ketone distillation unattended and heard a loud pop, ran into the lab to see water from the condenser spraying all over the room including on the hot mantle creating lots of steam, smoke coming off of the overheated charred goo left in the distilling flask, and black chunks of charcoal type goo (still glowing red hot) imbedded in the roof above the flask. The window was open, and smoke and steam were pouring out, a car was driving by and stopped to stare, luckily the fire dept was not called. Apparently the ketone had finished distilling, and the remaining crap continued to heat up, overheated, charred and expanded shooting the adapter off of the distilling flask and breaking the condenser in the process. Found chunks of black shit for months after that. DON'T LEAVE SHIT UNATTENDED.

also, pHarmacist (and anyone else with siezed glass joints:
SWIM has got glass joints stuck together a few times and the only method SWIM has found to get them lose is to use a torch. BTW this has worked everytime for SWIM. The type of torch to use is one of those little portable torches you get from the hardware store that has the screw on thing on the top, they're about a liter in size, and are blue, I think they are propane, sorry I don't have the exact info, I don't have mine here. So you take the torch and gently heat up the outer joint for a couple of seconds, then with oven mitts or similar try to twist the joint lose, if it doesn't come yet try again a little bit longer. The trick is to get just the outside joint hot enough to expand enough to loosen, while not transferring too much heat to the inner joint thereby keeping that joint smaller. Hope this helps.

SiLiCoN7

  • Guest
Too stoned... Burned honey
« Reply #59 on: February 14, 2003, 03:58:00 AM »
Swim has done all the usual fuck-ups, sep funnels left open when pouring, dcm added to hot reaction contents, amalgamation volcanoes in small rooms. But by far the most annoying mistake was smoking way to much hydro and consuming several beers after doing several reactions in a row and deciding to evaporate about 40 g's on a hotplate instead of the usual steambath. After several hours of watching water evap swim passed out from the obove mentioned enebrients.
Only to awake to a room full of thick smoke and a small pool of bubbleing black goop in the evaporation plate.
After several minutes of intence swearing swim realised he was getting high from the smoke!!!!!

Swim has quit smoking weed since then.