Author Topic: Your Really STUPID Lab Mistakes....  (Read 13502 times)

0 Members and 1 Guest are viewing this topic.

yellium

  • Guest
What's wrong with blowing air (or nitrogen)...
« Reply #80 on: July 06, 2003, 01:43:00 PM »
What's wrong with blowing air (or nitrogen) over it, instead of using an open flame?

del72

  • Guest
Fuck ups 101
« Reply #81 on: July 07, 2003, 08:55:00 PM »
Heh ok not to be redundant but the pouring shit in the sep funnel with the stop cock open is my biggest fucking problem too. 

One that was retarded as hell, a few months ago my friend was doing a mescaline extraction using DCM. He set his four liter sep funnel on the ground and balanced it as he poured a bunck of shit in it, well there was to much weight on it and it broke up above the stopcock!  

So he lost a bit of the stuff he was extracting but he still had plenty, and all he had for like 2 gallons of solution to extract was a 500ml sep funnel!

The sep funnel had no stopper for the top and that is the intro to the next fucking mistake.  So he has a sep funnel full of goods and DCM and then realizes that this little used sep funnel had no stopper. So he looks for something to plug the hole and finally(duh) puts a balloon around the top and tightens it on there with a rubber band. next morning he wakes up to find the oddest thing he has ever seen. The balloon started kind of melting I guess, but what it looked like was that somebody put a balloon in the sep funnel and then inflated it. It melted into the funnel but expanded to fit the shape of the inside of the sep funnel!  More goods gone.


aragorn

  • Guest
i vaporated
« Reply #82 on: July 16, 2003, 06:06:00 PM »
the h20 solution with 2ounces MA in it, i took a quick lab-break and forgot that the hotplate was way too hot so beside the water my whole meth disapperead in a cloud of smoke ;-(

pooky

  • Guest
O.D
« Reply #83 on: July 29, 2003, 05:30:00 PM »
This is not really a lab mistake, but may serve to educate others on what not to do.P gave a gram of mdma to a neighbour,told him someone gave it to P, for testing and fun with the explicit instructions to be used for ten people.Dipshit thought that was a little weak, and decided that three people sharing would be better.I'm not sure exactly what happened, but Dipshit looked very haggard and didn't stray too far from home for a few days.I still see him sitting on the porch,staring into the distance....

25dimeo

  • Guest
Chlorine gas
« Reply #84 on: August 02, 2003, 03:38:00 PM »
This is for anyone who wants chlorine gas home made. A long time back when SWIM wanted some chlorine gas he place about 200ml of calcium hypochlorite in a 500 ml flask. SWIM then attaches all tubing including an outlet tube for unreacted gas, setup looks great this should be pretty easy. He then begins dripping concentrated HCL into the hypochlorite.....a nice yellow gas begins to fill the flask....nice this is so easy he thinks (and everyone complains about what a pain chlorine is). After a little time has passed he notices that this setup is slow and and thinks hmmm maybe a little sulfuric acid would make this quicker. A quick switch of acid from HCL to Sulfuric and begins dripping it in....nice MUCH FASTER.....hmmmmm a lot of heat is being generated tho...oh well shit happens....so SWIM pumps more sulfuric in....LOTS of fizzing....TONS of heat but hey look how much gas there is.....after anougher quick shot of acid and a little shaking SWIMS decides to let it react and check back later....SWIM just turns his head to the side when BOOOM!!! The flask with the hypochlorite bursts into flames then quickly goes out with short flameing bursts still erupting a about 3 sec. intervals room fills with chlorine gas and NASTY black smoke SWIM can't breathe and thinks FUCK!!! grabs a towel throws the flask in a bucket of water outside runs back in and ventalates nice black burns all over the workbench and himself, he grabs wet towels and trys to wipe as much acid of as possible off himself. SWIM thinks NOTHING burns skin worse then flaming hot sulfuric acid with chunks of calcium hypochlorite clinging to the skin!!!! The acid had got the side of his face and neck and SMIM thanks god for looking away just as it happened otherwise he would be blind now! Also a good thing he left the stopper only tight enough to seal otherwise he would be picking glass shards from his face and neck...the stopper had blown off instead. The room smelled like it had been fully sanitized even a few months later!! Now SWIM ALWAYS wears glasses, gloves, and anything thing else that may be needed. As a side note FUCK cl2 gas and if he never sees calcium hypochlorite again it will still be to soon. Lesson...DON'T RUSH THINGS......WEAR SAFETY EQUIPMENT...AND FOLLOW THE DAMN DIRECTIONS!!! SWIMS reason for posting this is to prevent others from getting injured like this...if your new leave cl2 gas alone find anougther way, and if you think safety equip. is for stupid geeks then your gonna get burned....sometimes literally. :P


CSIdet

  • Guest
lye! It burns like fire
« Reply #85 on: August 16, 2003, 10:30:00 PM »
That stuff realy burns,and of corse it doesn'thelp when you keep spilling it on yourself. The table,fan,tool's,everything that your going to have to touch to finish the mess that you started. Gloves! that would have been a good idea ,but did I metion that the mess,and then panic started when my bestfriend and lab companion (when it's safe) started barking. A quick check of the monitor,three camra feed's revealed 6 police car's parked across the street.Parking lights on engine's running and this is my first go at it all on my own.
Two small scar's on my leg and a new pair of pants ,couldnt wear them again after I soiled them.
The cop's scared the crap out of me,and for no reason they where looking for the wife beater that lives across the street and not their to take  me away. Who said a little pairanoia is good for you, I was stupid for not beeing prepaired for anything and everything, man its hard beeing a newbee.  Did I metion that this all just happened a couple of week's ago


bio

  • Guest
introduction to microwave chemistry
« Reply #86 on: September 01, 2003, 09:52:00 PM »
Was making a  solution of a crystalline compound in alcohol in the sep funnel. It wouldn't all quite dissolve so I thought ahhhh the micro will speed things up a lot. Just 5 seconds should be safe. So I put it in and set 10 seconds and when it was 5 I turned it off and very carefully opened the door with my head turned the other way. Somehow I knew this really wasn't the right thing to do. Anyway I reach in with one hand and the door is cracked. Funnel is hardly warm. So I take it out and vent, hardly any pressure. Now I'm building confidence and thinking another 5 seconds will  finish it off. So I put it back in set 10 seconds watching carefully thru the door window. It hit 5 seconds , I pushed the stop button and BLAMMY, WOOSH, minor heart attack.

That was my first and last micro reaction.

jervis

  • Guest
drying nitric acid on a gas stove.
« Reply #87 on: September 12, 2003, 08:57:00 AM »
drying nitric acid on a gas stove. (I was really young and dumb.) After about two minutes of heating, my entire kitchen was filled with brownish yellow gas. I think I had about three heart attacks that day.

Confuto

  • Guest
oops
« Reply #88 on: November 06, 2003, 06:02:00 PM »
Had a mixture of Magnessium and KClO3. Layed it out on a rail road tie and was going to set up a cool display with white phosphorus but forgot the KClO3 mix was there. WP stick fell out of toluene and contacted KClO3 and BOOM. The 28 grams went up and blew wood and varius chems all over me. One the near by chems was Potassium Permaganate... that felt nice in the eyes.   LESSON : Use safety equipment and never play with strong oxidizers around any type of P.

TranceMe

  • Guest
About Bromine
« Reply #89 on: November 14, 2003, 06:05:00 AM »
While following

THIS

(https://www.thevespiary.org/rhodium/Rhodium/pdf/thf2gbl.pdf) procedure SWIM read you have to take care of the excess bromine form in situ. Fine by me said SWIM, left the contents stirring, plugged a hose for driving fumes out the window and went to watch some TV. Some hours later he came back to his tiny turned-into-a-lab bathroom to find out it was filled with bromine gas. Damn...opened the window and turned on a fan to vent the place AND stayed in to clean up the mess on the working table. Bad idea. It wasn't immediately but some 30sec. later, SWIM could barely open his eyes and had this burning sensation in his mouth. Run away and put his head under the faucet with cold water running at full throttle on his eyes and face. That's when the telephone rang. It was SWIM's friend to chat up a while. Bad, bad moment for chatting.
Took almost 2 hours for that burning sensation to clear from SWIM's eyes and mouth.


endo1

  • Guest
Yay! Another stop cock left open, bu this time...
« Reply #90 on: December 12, 2003, 01:02:00 PM »
OK how bout the old stop cock accidently left open... on the 22 liter sep funnel... beggining an extraction of about 1.5 kg raw mda base... can't see the bottom of the sep funnel w the liquid pouring out as the stand is made of wood... nor can the liquid hitting the table underneath be heard due to a noisy exhaust fan... lost well over half of it before he finally felt something wet splashing on his legs! Usually the stop cock is always closed all the time but this time a new helper was hired who left it open to drain the water after cleaning. This will make for some grumpy investors!
-always double check the sep funnel stop cocks before pouring! And also a flask underneath to catch any spilling liquid should be preplaced.

When making bromosafrole if there is too much "black tar" in your batch u will end up with a siezed vaac pump once the pump is cooled down and the pump oil solidifies! Or, if your vac source does not move enough cfm (ie a water spirator) you will slowly lose your vacuum as the black tar decomposes faster than your vac source can remove the arising "tar smoke" which leads to more decomposition which leads to further loss of vac which swiftly changes in to pressure build up and then of course the so called "bromo-volcano" and at the 2.5 kg bromo scale this is much more like an explosion than a volcano! This has happened many many times! One really bad time when it was thought "Hey, while we are distilling this bromo why don't we turn the exaust fan off and dismantle the exaust for maintenaince...". Of course the bromo eruption happened right when there was no exaust! Had to leave the house and come back when the thick black smoke settled in a few hours. I nice thick film of black tar still to this day resides on some book covers, cieling, keyboar/comp/monitor and other hard to reach places or places not deemed worthy of the excessive amount of energy/solvents it take to clean this crap.
-always take steps to minimize "black tar" when making bromo:
*Make sure there is absolutely no Br2 in your Hbr. i.e. Do not use sodium bromide to produce HBr and do not use tainted HBr in GAA (should be clear yellowish not dark black!) in your reaction!
*If using GAA as solvent make sure the temp is kept nice and low untill it's been washed/neutralized.
*monitor your vaacuum with a gauge during distillation to get indication of loss of vac early.
*perhaps a nice teflon vac pump?

Also, here's some other no no's learned the hard way:
-Never just simply "drop" in a big magnettic stir bar in to a flask.
-Be carefull of extreme pressure build up especially when an a/b from a NaBH4 synth.
-Never use FB flask under vaacum or any other flask not meant to hold a vacuum for that matter.
-When using pressure vessels make sure you know exactly how much pressure you're working with and that ALL parts (including the end caps of a "pipe bomb") are able to hold this pressure safely.
-When using silicagel in a NaBH4 synth make sure it is the non indicating type! Washing this silica gel thouroughly with water does not get all the Cobalt Chloride out! Yield will be 100% the alcohol!

methymouse

  • Guest
List
« Reply #91 on: January 10, 2004, 11:17:00 PM »
Where to start?

(1) Adding a 5M NaOH solution to a bunch of aluminum foil (to make alumina).  The jar I was doing it in quickly overflowed with very hot caustic juice, destroying a stirplate.
(2) Assuming that the concentration of KHSO5 was the same as another pool product when I couldn't find the MSDS for the one I was using.
(3) Heating an important solution (~10ml) in a small test tube with a few drops of chloroform at the bottom.  When a few drops of chloroform boil, they can force about 8ml of liquid out onto a sandbath.
(4) Not washing a glass stopcock sep funnel which had been used to hold an aqueous NaOH solution.  That fuses frosted glass, in case you didn't know.
(6) Using too much HCl in salting a certain amine, which was later snorted.  Wow!  I don't think I've ever found sodium bicarbonate that quickly before...
(7) Trying to distill H2SO4 out of drain cleaner.  My god is this a mistake if you ever want to see your flasks and distillation adapters again.  H2SO4 gas fuses silicon plumber's grease, BTW.


politoxicomania

  • Guest
Great fun ........
« Reply #92 on: February 24, 2004, 11:40:00 AM »
New species....
Reaction for about 500€ ......
Cooking and workup 3 weeks ......
Happy about some mm-Crystals .....
Analyse with IPDS ....
Wondering why it is NEt3HCl ....... priceless


auntyjack

  • Guest
shake, pop, splash.......F#^^&^@@$%*($%*)(
« Reply #93 on: February 28, 2004, 03:03:00 PM »
think i read about this phenomena but had to learn the hard way...
        days of ephedra extraction and work up...28 hour reflux...work up...all going well, down to the very last np wash of the hcl water/meth which was done with tce(tetra) and dcm...just for the heck of it the flask was heated till the dcm boiled a little and was left to cool....not for long enough...one shake, the dcm boils explosively and 4/5ths of the rxn now grace the ceiling and floor...this was upsetting...
               i'm not 100% sure but it seems as though the water was still holding enough heat to boil the dcm but it had to be shaken for the heat to enter the dcm...

ps yes, i just read of a very similar accident...what is this dcm not boiling until shaken business?


Teon

  • Guest
As simple as they get
« Reply #94 on: May 15, 2004, 02:35:00 PM »
I'm in lab, go to give the sep funnel one last good shake, throw myself off balance, fall, and shatter the funnel. The extra lab period really made that a wonderful week.  >:(

I swear, I'm not retarded or anything. I was just hung over and my sense of balance hadn't completely returned from the night before.

xaja

  • Guest
Acid burns
« Reply #95 on: May 19, 2004, 08:43:00 PM »
SWIM used to sometimes boil down battery acid when wasn't possible to get H2SO4, just for the gas-maker. Two bad experiences here. First was pouring boiled-down stuff into jar (instead of beaker) which shattered because acid was hot as fuck. Ruined benchtop, carpet, paint on wall. Second incident involving this shit was as follows: even stove-concentrated shit was weak, could just pour 50-100mls into gas-maker and put lid on. Friend brings in lab-grade H2SO4, much better. But SWIM forgot it was stronger and poured ~100mls into gas-maker. Next thing volcano erupts and SWIM covered head-to-toe in conc H2SO4. Not nice. Luckily the tub full of water for waterpump for reflux, so grabbed bucket and furiously tipped water all over SWIM. Needless to say clothes SWIM wearing were completely fucked after this.   :(


Bandil

  • Guest
Read the fucking label!!
« Reply #96 on: May 27, 2004, 02:24:00 PM »
Just when i thought i had become a little smarter and didn't make stupid mistakes any more (cocky is the proper expression), i made the biggest mistake so far.

While forming the Vilsmeyer complex in a solution of 45 mL NMF with 40 mL POCl3, a slight course change happened. Apperently, the bottle of presumed N-methylformanilide, really contained N-metylformamide. It also said so clearly on the bottle. My brain had read it differently however.

Imagine my suprise, when approximately 10 g's of the phosphorylchloride was poured into the NMF (nope, no fumehood here), giving a gigantic volume of gasseuos HCl in less than a a second. At the same time the solution started boiling etc.

Luckily nothing happened to anyone (me) physically, except my personal chemist karma points has fallen alot  :) .

Oh well, you live and you learn  ;)

Regards
Bandil


Vaaguh

  • Guest
Clamps and water flow
« Reply #97 on: May 28, 2004, 10:12:00 AM »
In a 2 neck RBF solvents where refluxed at 170 °C this RBF was equiped with a mercury thermomterer, a reflux condenser and a gas outlet on top of the condenser for leading the minor escaping gasses into a bowl of dilute NaOH.

At some point due to electrical problems the waterflow in the condenser halted and when it was noticed the condenser was completeley filled up with smoke.

A couple of minutes later the waterpump was turned on again this ofcourse caused the vapors to cool down so fast that the condenser with the gas outlet attached to it sucked up a royal ammount of the dilute NaOH into the reaction mixture.

From here there are reasons to beleive that the not so planned addition of NaOH synthesized a very angry dragon. After hearing a deep roar from inside the RBF extreme gas evolution caused the RBF to bee pressurized so bad that the unclamped mercury thermometer skyrocketed away with enormous speed only to be stopped and shattered by the roof.

For another minute the roaring continued accompanied by a fountain of very hot brown gunk  :( .


MadMunkey

  • Guest
Pyradine SUCKS!
« Reply #98 on: June 23, 2004, 10:39:00 AM »
today i had my first expirience with pyradine. i work as a lab assisstant and my boss had me distill about 1.5L for a rXn he was doing then left. he forgot to tell me the fumes SUCK! so i set up the RotoVap, pour the shit in the rotoflask and go to breath and promptly drop the flask. luckily it landed in the water bath, but shit. i hate the burning in your throught that you get from that shit, my fucking god.


MadMunkey

  • Guest
dammit
« Reply #99 on: June 28, 2004, 11:17:00 AM »
i keep fuckin forgeting to turn on the water running thru the condensor coil. "the rotovap isn't running as efficiently as i should, damn it's hot... o, thats's why, shit!" :(