Author Topic: Your Really STUPID Lab Mistakes....  (Read 13304 times)

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ClearLight

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Your Really STUPID Lab Mistakes....
« on: November 05, 2002, 10:01:00 AM »

  Here, for the erudition of all, is where we get to post our favorite "DUH" lab mistakes...  thus we can learn and be entertained at the same time...


  1.)  My most repeatable one is pouring my solution into the sep funnel with the stop cock open... even better when I haven't put the beaker under it!

  2.) Shaking a mix of RP and KCl03 dry on a filter paper under the hood, which promptly ignited!

  3.)  Using the tlc reagent sprayer without setting the pressure gauge on the tank, and fogging the lab with a nice mist of HCL+Erlich's reagent, while not wearing a respirator!   :o



Infinite Radiant Light - THKRA

GC_MS

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used
« Reply #1 on: November 05, 2002, 10:09:00 AM »
1 - I used NaOH to acidify a solution of p-methoxyphenol (was after a long night of hot steamy sex, perfumed with a divine 2C-B trip).
2 - Accidentally used concentrated H2SO4 in the pinnacol rearrangement of methylenedioxypropanediol to MDP2P. All hail the formation of useless black tar  ::)  (after a long night of sexual failure, due to severe alcohol intoxication).

Ave Hive, synthetisandi te salutant!

b159510

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I'm sure this will be moved
« Reply #2 on: November 05, 2002, 10:35:00 AM »
but- Rinsed a beaker with acetone. The beaker had bromine residue in it.  8)

Grabbed a solution of sodium thiosulfate, thinking it was sodium bicarbonate, and briefly tried to neutralize an acidic solution. Very  8)

BTW, aqueous sodium thiosulfate is used for bromine burns.

Thankfully nobody was around to witness these incidents, and they happened in a fume hood. Still nasty though.
You don't fool me, Oilman

lab_bitch

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I have a venting system that bubbles any ...
« Reply #3 on: November 05, 2002, 11:10:00 AM »
I have a venting system that bubbles any methylamine smelling gas generated by the nitro amination through HCl.  There is an inline valve that can be used to open or close this vent.  A while back, one of my workers was running the reaction and forgot to open the valve.  After adding about half the nitro, the rxn setup began to leak at all the joints and it was obvious that pressure was building up.  Wanting to get a better look at what was going wrong, 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.  Frantically trying to get the mercury off, they both ran to the nearest bathroom, stripped down butt naked and both climbed into a shower that would have been a tight squeeze for just one of them (they are pretty big guys).  At this point, I come in to see what all of the commotion is about only to find one of them bending completely over and sticking his head under the faucet, while the other one stood directly behind him trying to get to the faucet as well.  You can probably figure out what was going through my mind at this point.  Horrified, I asked them what in fucking hell they were doing.  They quickly clarified the situation only to have me point out that there were actually two bathrooms in the house.  I bet that made them feel really good!  To this day, I still continue to make fun of them about that incident and they have never forgotten to open the valve again.  I guess the moral of this story is to think before you act (i.e. opening a valve; jumping butt naked into a shower with another guy when you could just go across the hall; walking into a bathroom where you here the shower running and two guys yelling at eachother)

Sunlight

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shaking a warm solution
« Reply #4 on: November 05, 2002, 11:38:00 AM »
Shaking a still warm solution to extract the amine in a sep funnel with DCM, more than a half was directly spitted.
Shaking "slightly" a flask with the magnet inside, the flask was broken and it had THF...
And many more...

yellium

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Dumping a small amount of NaH (used for drying) ...
« Reply #5 on: November 05, 2002, 12:52:00 PM »
Dumping a small amount of NaH (used for drying) in the same sink where I'd thrown away some ether washes. NaH starts fizzing, as it usually does when you destroy it with water. Then starts burning. No problem, was only a small bit, so it should be out in half a second. Instant *woosh* as the ether fumes ignite.  Got only a few small burns on my hands (and removed all the hair on my knuckles). Organic chem fires are *intense*.

(lessons learned:
-don't throw flammable solvents down the sink.
-destroy NaH in the proper way, by titrating with EtOH and then dissolving the ethoxide in water.)

When all you've got is a nailgun, every problem looks like a messiah...

PoohBearium

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Mistakes
« Reply #6 on: November 05, 2002, 02:55:00 PM »
1)Using a pyrex bowl that was not stovetop certified to boil off the water in the very final step of a perfect 20g pseudo/I/rP, that took weeks to prepare for, SWIP's very first dream (still recovered enough in a towel that was under the bowl to OD on...  ::) )

2)Assuming that a glass salt shaker would withstand the pressure of a 1g nano, when doing a sealed reaction.

3)Trying to cut corners (too many to list!!!)

PB

WARNING:The punishment for self-rating your posts is a slow and agonizing death!!!

Rhodium

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Lab-size Mushroom Cloud
« Reply #7 on: November 05, 2002, 04:42:00 PM »
Adding 10g LiAlH4 through a powder funnel in one portion to 250ml of wet washing THF (used by mistake instead of the anhydrous THF prepared for this particular occasion). To make it even funnier I used a single-neck RB flask, so that the massive amounts of instantaneously evolved hydrogen pushed the remaining fine dust (which was still in mid-air inside the funnel and flask) upwards, forming a mushroom cloud, covering all the lab benches and the floor with a thin grey carpet of quietly hissing LiAlH4 slowly reacting with the moisture in the air.

wacko_reaco

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6kg performic run going horrible
« Reply #8 on: November 05, 2002, 05:01:00 PM »
all the reactants were in the pilot vessel, the temperature being contain by turning the cooling water on and off, when the temperature stopped going past 32C i was curious as to why, realised the chuck on the overhead stirrer had come loose and stirring had stopped for god knows how long, so instead of cooling the system right down and beginning stirring very slowly i just re-tightened the chuck in a panic and turnt he stirrer back on full, two seconds later 20Ldcm, 20L performic acid and 6kg iso were all over me and i was doing the mad dash to the shower, cleaning up that ffucker took two days and three pairs of rubber soled shoes (dcm likes rubber)

wacka wacka wacka

Tyler_Durden

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h2o2
« Reply #9 on: November 05, 2002, 10:04:00 PM »
Misunderstood the labeling of H2O2 40 volume for 3 YEARS, until about a month ago - ARGH!!!!

Oakenfold, LSD, Sasha, Shrooms, Digweed, MDA/MDMA

Moriarty

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I have some rhymes for the house!
« Reply #10 on: November 06, 2002, 01:37:00 AM »
I.  When SWIM was fourteen (14) years old, an age at which all sorts of mischeif seems to occur in the human male, SWIM was making murcury fulminate Hg(ONC)2 which is a common primary explosive many at that age try to make (generally successfully, as it is an easy synthesis for a young chemist).  What can SWIM say, he was interested in chemistry, and explosives are a given for a boy that age.

Anyway, if SWIM's memory serves him well, and it might not since that was 12 to 14 years ago, the reaction looks something like this:

Hg + 2HNO3 -----> Hg(NO3)2 + H2 + NO2 + HNO3 (excess)

Hg(NO3)2 + C2H5OH + HNO3 -----> Hg(ONC)2 + 2CO2 + H2O

NOTICE: SWIM DIDN'T TAKE THE TIME TO BALENCE THIS EQUATION AND IS NOT EVEN SURE IF THOSE ARE THE CORRECT REACTION BYPRODUCTS.  THAT PORTION OF THE POST IS NOT IMPORTANT TO THE STORY!!!  BY THE WAY, SWIM's NOT PROVIDING INFORMATION ABOUT EXPLOSIVES THAT ARE NOT ALREADY KNOWN BY EVERY 12 YEAR OLD CHEM ENTHUSIAST.

Anyway, that experiment and the production of Cyclonite (CycloTrimethylenetrinitramine [sp?]), the secondary explosive in C-4 plastique explosives won him several felonies and caused him to lose interest in chemistry until just about a year ago.

Anyway, here's his big snafu.  When the reaction was really moving along in a glass jar of about 2 gallons it overflowed.  Oh course SWIM was smart.  He scaled up for an exothermic reaction!!!  He was doing whatever it is he did back then but diddn't notice.  To make a long story short, when he tried to lift the jar with the mercury fulminate in it he hadn't noticed that a great deal of this very volitile, shock-sensitive explosive had dried beneath the heavy glass tea jar with indented grooves on the bottom.  He tried to lift it and FLASH!!!  Yep, an explosion occurred.  He had glass everywhere.  He's lucky only a small amount actually made it's way out of the jar and dried or he'd be dead.  Anyway, thankfully the shock wasn't enough to set off the fulminate in the alcohol solution or half his garage would have had SWI-Moriarty splatterings all over it.

I don't know if this really fits in this forum but it was a definate lab mistake that cost him :-[ !

II.  SWIM aminated some ketone last year.  He came out with nothing.  He recalculated the amount of 5% NaOH solution he added to basify for his A/B extraction and realized that he didn't add enough to get the pH above 7, meaning he threw all his honey away.  Save everything until your finished bees, that mistake hurt SWIM in amazing ways (he needed the money)!

Who wants to play cops and dope fiends?

Cyrax

  • Guest
When you neutralize a NaHCO 3 or a K 2 CO 3 ...
« Reply #11 on: November 06, 2002, 03:39:00 AM »
When you neutralize a NaHCO3 or a K2CO3 solution with HCl, place the damned beaker in an ice bath and add the acid DROPWISE.  If you don't - like me once - the freaking solution will jump right out of the beaker in a kind of mini explosion (due to the evolution of CO2) ... 
It was quite spectacular ... a piece of the erlenmeyer was blown away and the carefully synthesised product was splattered all over me.

Chromic

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THF volcano
« Reply #12 on: November 06, 2002, 06:44:00 AM »
1) THF volcano when mixing H2O2, THF and radical initiator in hopes of making GBL.
2) accidentally making some volatile bromo-organic compound when brominating THF.
3) shattering pyrex pie plate on element (flying hot sharp glass fragments, ouch! that one hurt)

Then there were SWIC's days with gun powder & other flammables...

BlizzardofOzs

  • Guest
Assumption!!
« Reply #13 on: November 06, 2002, 04:15:00 PM »
Happened twice should have learned the first time. But you know us. (Shit, yeah right) Never, ever assume that someone helping or for that means getting in the way of the "expert" knows what ther doing. My(worst)example; SWIB's usual work about 330 g's already ph'd ready to drop (helper) say's they know what to do. SWIB's not looking and when he doe's notices massive fumes coming from the 4 litre vission. Helper dropped water and half of the fuel. SWIB pulled it off heat and helper lights torch and Coleman fumes don't fuck around. Boom!!! all gone. That Gary Coleman's a mean mother fucker that's why I don't play with him no more. 

Ohhh yeahhh,the "SPIN DR." is in!!!!

Sifty

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Salt Peter
« Reply #14 on: November 07, 2002, 12:55:00 AM »
When I was 12 I was trying to melt a mixture of 50% sucrose 50% sodium nitrate in order to make a slow burning smoke bomb.

I was melting it on a gas stove.

It promptly erupted with a 2 foot purple flame and sounded like a jet engine, spraying molten sugar all over the kitchen. The sugar melted the carpet (replaced), the counter tops (replaced), the ceiling (repainted), and the fucking metal fume hood thing over a stove! Talk about hot!

Not to mention, a neighbor saw the smoke from the prematurely ignited smoke bomb pouring out a window and called 911!

After speaking with a police officer and 4 firemen, my mother finally came home and kicked the SHIT out of me. I was grounded for years.

-Sifty

"...Come with us and leave your earth behind..." - Chem.Bros.

pHarmacist

  • Guest
Duh!
« Reply #15 on: November 07, 2002, 04:44:00 AM »
Doing a reaction, workup and what not, finished, friend calls, wants to hang out, ok fine, "-should i clean it now or later, nah.. I'll stopper the RB with a glas stopper so it dosen't stink, then I'll do clenup when I get back.. yes", being impulsive I got back home  after several days, I still havent managed to get the stopper out, this was a year ago... way to go..

Never underestimate the power of retrosynthesis.

thethethe

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Lab Mistake
« Reply #16 on: November 07, 2002, 04:26:00 PM »
Always label your containers of clear liquid!!!

See:

Post 235232

(Rhodium: "Re: Tasting E freebase oil..", Chemistry Discourse)


TTT

Drug shortage is a worldwide problem with neighborhood solutions.

Ace99

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Mixing GBL and NaOH inside the glass bottle the ...
« Reply #17 on: November 08, 2002, 07:14:00 PM »
Mixing GBL and NaOH inside the glass bottle the GBL came in, inside a hotel room. Since it was large scale and going slow, someone put the lid on, and swirled it. It started boiling inside, pressure was building up. Someone tried to take the lid off to relieve pressure and it sprayed everywhere like shaking up a bottle of pop and opening it, except much stronger. There was a loud pop, and it was all over the ceiling and walls. It was only half reacted so there was this really greasy oily GBL coating, no matter how much tried to wash it it was still greasy. Just said "fuck it" and packed everything up and left the room disgusting. I wonder what the maid thought about the greasy stuff on the walls and mirrors and ceiling that just wouldn't come off.

Xicori

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when SWIM was a young stupid boy he tried his ...
« Reply #18 on: November 11, 2002, 06:23:00 AM »
when SWIM was a young stupid boy he tried his first amphetamine synthesis:
after the Benzaldehyde/EtNO2-Reaktion he wanted to remove the residual EtNO2 on the hotplate - his nitropropene burnt and the room was full of tear-gas-like vapours ... ::)

so swim learnt that it is important to use an oil bath and destillation setup :)

ChambeRed

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Unlabeled containers+pigsty lab+poor ...
« Reply #19 on: November 11, 2002, 10:06:00 AM »
Unlabeled containers+pigsty lab+poor memory=recipe for disaster!label those containers! ::) .

Bee's don't die,we just multiply.

Scooby_Doo

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Doing a 22Lt size Grignard, and trying to start ...
« Reply #20 on: November 11, 2002, 09:33:00 PM »
Doing a 22Lt size Grignard, and trying to start it by adding way over 10% more like 40% of the THF sol to the Mg. It still wouldn't start so Scooby being so smart thought a little controlled heating would be the way to go. The next thing Scooby sees is the drierite being shot out of the drying tube and 10 Lts of THF vapour/liquid filling the room, with lots of electrical stuff running. Talk about funny!?!

Xicori

  • Guest
and scooby, what was the consequence? :-( ...
« Reply #21 on: November 12, 2002, 05:12:00 AM »
and scooby, what was the consequence?  :(

...sounds horrible...

pHarmacist

  • Guest
How about
« Reply #22 on: November 12, 2002, 06:55:00 PM »
Making PCE... oh, about to use cyclohexanon, not reading the flask-label swim added cyclohexanol, what a suprise: it didn't work..

Scooby_Doo: That's what makes chemistry fun!  ;D


1-2-3 ACiD

sponsan

  • Guest
methylamine
« Reply #23 on: November 13, 2002, 07:20:00 PM »
During the last recrystalisation step of the first attempt to make methylamine, the glass beaker containing methylamine in methanol was promptly dropped inside the fridge, shattering and spilling everywhere.  After a 3 hour cleanup operation, which included having to place the fridge upside down and washing nearby walls and floors, the "chemist" was sitting on the couch exausted, smelling of rotten fish and poor hygene.

The cleanup operation had to be repeated a number of times on the subsequent days, due to extremely bad smell in the house.  Three packs of nag shampa insence were spent as well as multiple cans of deodoriser and many cleaning agents.

The fridge had to be cleaned inside and out three times, and two weeks later a faint smell of something resembling baked urine can still be smelled next to the area immediatly surrounding ground zero.

The "chemist's" partner was not impressed.  Never again.

pHarmacist

  • Guest
My Mom would've killed me if I did that!!
« Reply #24 on: November 13, 2002, 07:23:00 PM »
...

1-2-3 ACiD

Scooby_Doo

  • Guest
Xicori: Mr THF and me had a little race to see ...
« Reply #25 on: November 13, 2002, 09:33:00 PM »
Xicori: Mr THF and me had a little race to see who could get to the power points first, luckily for me THF is pretty slow off the mark. :)

pHarmacist: That's what makes chemistry fun!

I would probably agree with you there, after you have survived doing insanely crazy and flat-out reactions, everything else seems a little dull. ::)


Dazza

  • Guest
back wen some friends and i were kinda 'new' to ...
« Reply #26 on: November 16, 2002, 02:46:00 AM »
back wen some friends and i were kinda 'new' to chemistry and we tried to make some chloroform, we were doing the reaction and distillation in one setup, and we had stoppered all the ends so there wasn't any room for the pressure to escape during the reaction.
one moment we were standing there watching wat we thought was going all fine wen suddenly the condensor blew up and the sudden release of pressure pushed the reactants up out of the RBF really fast and all over the whole room. took a while to clean up  ::)  ...
and in our next try to make it one of my friends decided to hold the 2L RBF instead of attaching it to the retort stand and it got too hot for him to hold so he dropped it :(

and all the other glassware we've broken b4 that and since then :(  ....

Buckshot

  • Guest
major mbrp accident
« Reply #27 on: November 16, 2002, 01:51:00 PM »
A few weeks back Swib cut the strikers from 15 boxes of matches. All the strikers were set aside, and the actual matches were thrown into a plastic bag. 15 boxes of matches is now 750 books of matches without any cover on them to protect them from friction.
So Swib tosses the whole bag of matches into his 15th floor garbage shoot. And guess what, matches are friction sensitive. So during the 15 floor drop they must have ignited, becasue within minutes the fire alarm went off, and the building was burning. The fire was in the garbage bin, but the fire dept smashed in the walls to see for fire inside the walls. They casued thousands of dollars in  water damage.

Well nobody asked Swib about it, so swib never mentioned it.
750 books of matches is an excellent arson device. Actually it's a crude match head bomb.

BEE_N_COGNITO

  • Guest
EtOH fumes -> Drunk Off Ass
« Reply #28 on: November 18, 2002, 09:22:00 AM »
Pinch situation,
    Recreational camper evapping 10gal. of EtOH using electric skillets and hot air guns with very inadequate ventilation. (nuf sed)
   

A false sense of security, is worse than being unsecure.



pupilage

  • Guest
Really bad day
« Reply #29 on: November 19, 2002, 12:18:00 AM »
Missing label. Thinking container held NaBr (but really held sodium Hypochlorite) poured into DMSO. Flask flashed and contents rushed to the ceiling.


"Sometimes I sits and thinks, and sometimes I just sits." Satchel Paige

abacus

  • Guest
volcano
« Reply #30 on: November 19, 2002, 02:09:00 AM »
Superheating a solution of filtered acetone and ethanol and then adding the stirbar in the flask.

Instant volcano covering the ceiling and filling the room with explosive solvent vapours, luckily no smokers where in the lab!.

zibarium

  • Guest
venting HCl vapor thru a fan motor
« Reply #31 on: November 20, 2002, 06:37:00 AM »
squirrel cage vent fan; seized up real quick; instant rust; left 'stupid' without a vent.

yellium

  • Guest
Never rotavap leftover extractions from a ...
« Reply #32 on: November 28, 2002, 01:36:00 PM »
Never rotavap leftover extractions from a standard, shulgin-style performic to dryness. I tried that once, on a rotavap where I'd set the heating bath to hand-warm. Ended up with about two or three grams of `dark-red/brown colored  oil'. Big surprise when I brought the rotavap to normal pressure and the gunk in the flask decided to explode. Rotavap instantly covered with smoke, fortunately no damage.  But I did realize that I was lucky...


Hardcore libertarians consider the idea of a Libertarian Party dangerously socialist.

X_Stacy

  • Guest
I once decided to try a hydration of safrole ...
« Reply #33 on: December 04, 2002, 01:14:00 PM »
I once decided to try a hydration of safrole using concentrated sulfuric acid. Without stirring or cooling. It took two weeks to clean and repaint the fucking room after the volcano of polymerized shit blew up the flask.
There was also the time I decided to try gassing methanolic solution of mdma base in a closed system. Those rubber hoses don't hold up like they should. I had to make an excuse at work why my face was red and my nostrils and mouth were torn to shit. Luckily, cleared up in a week. Also, on my first attempt at mdma, I tried to speed up the evaporation process with a stove top in a kitchen with no ventilation in the middle of downtown in a VERY small apartment. The neighbors were nice and called the fire department while we were trying to put the fire out. When the glass shatters and methanol seeps under the burner, it's a bitch to put out without a fire extinguisher. Anyway we played it off with a story that I was cleaning the stove with ammonia and didn't realize the stove was on. The list goes on and on... ::)

"I laugh in the face of danger, and then I hide until it goes away."

lab_bitch

  • Guest
I don't know about EtOH, but acetone vapors are ...
« Reply #34 on: December 05, 2002, 12:00:00 AM »

Cheapskate

  • Guest
Almost Fatal
« Reply #35 on: December 06, 2002, 12:43:00 PM »
Walking up to a motorhome parked with the lights off in the middle of the desert in the middle of the night without announcing my presence first.

Seems they were reacting some P2P with some other stuff and didn't like being surprised.

I've been shot at before but for some reason this time scared me more.

myles

  • Guest
tennis ball
« Reply #36 on: December 06, 2002, 08:52:00 PM »

metwurst

  • Guest
another volcano
« Reply #37 on: December 07, 2002, 08:16:00 AM »
not stirring conc. sulfuric acid while dripping in hydrochloric acid. wondering about the slow rate of HCL gas evolution after a few minutes, I jiggled the flask and painted me, the roof, and walls with about 300mL H2SO4/HCl. goggles and a respirator saved me from any serious damage, and without the goggles I suspect I woulnd't be able to see anymore.

seelite

  • Guest
Cumulus Methylaminus
« Reply #38 on: December 10, 2002, 09:04:00 PM »
To produce a "big" batch of methylamine HCl, ammonium chloride was added to formalin (about 2.5L)in a 5L RB and the reaction was allowed to progress at 104 degree.  Subsequent distillation and ammonium chloride recovery steps were then performed.  But for the final concentration and sublimation step, swim fell asleep (been going for 2 + days straight)and woke up suddenly to an entire house fuming with cooked methylamine HCL.  Swim ran to the lab and found huge streams of methylamine smoke flying out the vac adapter and the base of 5L RB was black with burnt methylamine.  It took swim 2days to wash every surface in that house and multiple weeks to air it out.

Everything went fine as it it appeared that the smoke billowing out of the house was coming from an overcooked turkey.  (swim feigned taking out a cooking pot on the balcony and everything 8) )

never, never again....

Don't drug the mind-let the mind use the drug-it won't mind.

madprosr

  • Guest
ran a 21g MeNO2 reduction using extra heavy duty ...
« Reply #39 on: December 12, 2002, 02:31:00 AM »
ran a 21g MeNO2 reduction using extra heavy duty foil. had to keep pouring water of the flask and overflowing the water bath to keep it under control. ran water all down the sides of the hotplate/stirrer, some of which must have penetrated it because the heating function is shorted out now.

don't do this!

uhm, and once tried to extract some mda from basic acqueous solution using IPA.

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.


baalchemist

  • Guest
Back a few years when Baals' first gotten...
« Reply #60 on: February 16, 2003, 01:41:00 AM »
Back a few years when Baals' first gotten interest in chem-hackin' came about, it started with hash oil after a friend gave me the 'cannabis alchemy' book. Seeing how Baal had ~20lbs of scrap leaf accumulated, extracting away he goes with EtOH and has this huge wad of oil when its all over. Decides that next, isomerization is wihin means seeing how the extraction was first chem experience and that went easily done. Went through the whole process unscathed & lovin' the new hobby already. Roomate gets home @ 1am and hits the sack, so Baal goes ahead and starts to evap off the ether from the iso-oil in a hot-water bath on the electric stove. All is well so far, then Baals roomy wakes him up at 7:30am as he's off to work. Baal realizes he is standing in the exact same spot as 6 hrs earlier, but cant account for his actions during that time. Seems that Baals stove's fume-hood isnt the same as a real labs', and he passed out from fumes and the knees were locked just rite and his head fell forward onto the fume-hood(while still holding the flask in the H2O-bath) and this formed a tripod of sorts that enabled Baal to sleep standing up just like Mr. Ed. The oil was awesome!!!!
A couple years later after Baal had gotten the Al/Hg figured out, theres a freshly toluene-extracted 100g reaction in a beaker in hand and Baal then has a friend pouring this into a 6L sep-funnel that Baal is holding. Friend being a non-chemhack is doing exactly as told by Baal, but Baal forgets to remove the huge stirbar from the beaker. Plop goes the stirbar, tink-boom goes the sep-funnel into pieces and ~3L of toluene/freebase mixture ends up soaked onto Baals clothing. Within 5 seconds or so Baal runs over to this 3 ft diameter plastic dish like thing and stands in it and orders the now freaking out friend to quickly take a gallon can of Toluene and  extract Baal. After the full body toluene extraction, clothes were given a final rinse & wrung into dish as well. After a well deserved H2O-shower, Baal finishes the final workup on his giant dish o'stuff. After gassing, the final yield was 87g's. The irony of it all was that was Baals highest yield ever up until that point. ::)


scram

  • Guest
LOL Baal!
« Reply #61 on: February 16, 2003, 08:17:00 PM »
Thats what I call "gettin' high ghetto style!"
Man are you nuts? Dont ever get toluene on your the sensitive parts of your skin like your thighs and espcially your balls!

abolt

  • Guest
Baal
« Reply #62 on: February 16, 2003, 10:45:00 PM »
Fucking hilarious. That post should go into the Hive hall of Fame :)  :)  :)

yellium

  • Guest
Better be glad he didn't use acetone.
« Reply #63 on: February 17, 2003, 07:14:00 AM »
Better be glad he didn't use acetone. Instant mdma overdose by dermal absorbtion.

food

  • Guest
looked like peanut oil
« Reply #64 on: March 14, 2003, 03:23:00 PM »
Not a life and death mistake or nothing ...
swif's assistant pippin was busy in the cellar. Cooking away. Noticing that the oil bath looked low he picked up an unlabeled bottle of light gold liquid; looked like peanut oil. And, you guessed it, poured in into the hot oil bath. Cept the unlabeled bottle wasn't peanut oil, but safrole tainted by a boil-over. I don't think he noticed it as deep in concentration as he was, but when arrived at swif's front door he was no longer pippin, the erstwhile assistant, but pippin the world's largest walking talking sassafras potpourri.
Lesson:
-label bottles. With something.
-try freezing to isolate safrole maybe
-just plain 'pay attention'!

--
food

scram

  • Guest
Unlabled chems
« Reply #65 on: March 15, 2003, 01:10:00 PM »
"Lesson:
-label bottles. With something.
-just plain 'pay attention'!"

Yes indeed label bottles. I learned this doing the nitro al/hg once. Unknowningly placed the 150ml pre-measured diluted nitro in MeOH bottle next to an identical bottle with the 100% nitro. Proceeded to dump the about 75ml of this pure nitro in over 20 seconds. I don't think I need to explain what happened next.

Bandil

  • Guest
Wasting LAH
« Reply #66 on: March 31, 2003, 03:39:00 PM »
Just made a new bummer, that deserves mentioning in here.

After brewing up a nice batch of 2,5-dimethoxynitrostyrene for a little to-see-bee from 25 g of benzaldehyde whe nitrostyrene was weighted. It was 30 grammes :) AWESOME i thought and made the LAH for 30 grammes of nitrostyrene. After the LAH was put in the THF i discovered that the magnet was left in the nitrostyrene, which was a whopping 8 grammes :( Used the LAH anyway but i wasted about 6 grammes of LAH!

Wont make that mistake again!

Regards
Bandil


yellium

  • Guest
Consider yourself lucky because in this case...
« Reply #67 on: April 01, 2003, 01:13:00 PM »
Consider yourself lucky because in this case excess LAH won't hurt you :-)

GC_MS

  • Guest
LOL!
« Reply #68 on: April 01, 2003, 01:23:00 PM »

AWESOME i thought and made the LAH for 30 grammes of nitrostyrene. After the LAH was put in the THF i discovered that the magnet was left in the nitrostyrene, which was a whopping 8 grammes :(




LOL! Join the club, my friend! Leaving the stirbar somewhere in my crystalline mass is one of my very-often made mistakes. The reason why I make this mistake so often is because I usually do small-scale synthesis, using tiny stirbars that easily disappear in the crowd of glistering crystals. Especially when I'm doing nitrostyrenes... And no, my latest reported yield of 80% 2,5-DMNS was WITHOUT the stirbar  :P




Richy

  • Guest
Stupid lab mistakes
« Reply #69 on: April 19, 2003, 03:52:00 AM »
My biggie would have to be while cooking a 9g HI/P reaction. There were leaks in the pipework and HI gas was filling the lab, so I employed a fan to rid myself of the nasty fumes. Bad idea. Although the fumes were taken care of, the cool air from the fan blew onto my thermometer which was monitoring the temperature of my reaction. I'd assumed that my hotplate was being an annoying bitch, so i cranked it up a few notches. While my thermometer read 120 degrees, the contents of my flask were actually heated closer to 280 degrees, and the pseudo was burnt to a crisp. That was my first dream.  :P

My second mistake was during my first extraction dream. During a waterless A/B i added toluene to the basified PM, and after shaking and swirling for 15 minutes or so, I promptly threw out the toluene and left the PM sitting in the beaker! :P  At the time I was under the impression that the toluene removed everything except the pseudo! I threw out about 4g worth.


DiMethyl

  • Guest
Almost fatal stupid mistake
« Reply #70 on: April 20, 2003, 02:42:00 PM »
While recrystallizing some phenylnitropropylene from methanol I experienced the following nightmare.
FIRE!
Yes---fire---which is what you would expect when using a mason canning jar over a bunsen burner flame. (dumb!!)
Almost twenty years later I can still hear that jar crack and break.
This was instantly followed by a blue flamed explosion and the small room I was in was engulfed in thick yelllow smoke from the burning phenylnitropropylene.
While the two smoke alarms blared pierceingly into the thick yellow smoke I realized that I was on fire and I could see the blue flames flickering through the smoke.
When you are on fire you can move pretty damm fast---real fast.
I grabbed a blanket off the bed and wrapped myself in it while choking on the smoke with fluids pouring out of my nose and eyes.
I headed for the window to open it to vent all that damm smoke while someone knocked on the door wanting to know if everything was alright.
I yelled as calmly as I could that everything was fine and that something had boiled over on the stove as I opened the window and the smoke bellowed out.
Once the fire was out and the room vented I realized that I was in considerable pain from the burns on my legs and stomach.
A call to my dentist got me a ride to the hospital where I was asked alot of questions but eventually arrived back home with some great pain pills.
No cops-----not one.
They would come about 6 weeks later in the form of a raiding party that took down that town's very first meth lab ever.
It took 20 years for me to get over that and to get back into lab work.
I hope that someone reading this can benefit from my mistake and avoid all the pain and grief that I went through.
DiMethyl


Nick_J

  • Guest
I've had a few...
« Reply #71 on: April 29, 2003, 07:32:00 AM »
I've made a few mistakes before, I try not to though since mistakes can (more easily) cost life and limb in my lab!
One mistakes was to evapourate a load of diethyl ether, and forgetting to turn off the bunsen at the other end of the bench. WHHOOOMPHH!! A big ball of fire erupted all around me, but after that it was just a little fire localised to an evapourating basin, so it was easily dealt with. No damage. That was a couple of years ago, and taught me a good lesson!
Most recently I was trying to recover spent acid from an RDX batch. I figured that refluxing the diluted acid would drive off and decompose remaining organics, so that the nitric acid could be fractionally distilled to azeotropic, then distilled from conc sulphuric acid to make it useful again. All went well for about 15 minutes, it was happily refluxing, then in a few seconds it suddenly erupted into a cloud of nitric acid, formaldehyde and nitrogen oxides, filling my lab with brown lachrymating fumes and smashing £50 of glassware on the ceiling... but again, a good lesson was learnt!
Luckily I have never had an accident with any serious high explosives, since I don't allow accidents to happen with these because I am aware of the risks. In the examples above, I simply wasn't familiar with what I was doing and this led to problems. Whoever said that ignorance is bliss was clearly lying...


ClearLight

  • Guest
PdCl and Nickle
« Reply #72 on: May 08, 2003, 04:22:00 PM »
Was dissolving some PdCl in a test tube w/ HCL and inadvertently grabbed the wrong spatula, which was a Nickle Plate SS one.. AKKK!  Pd precipitates and I now have a NiCl solution, elemental Pd and HCl!

  Don't use metal objects w/ Pd solutions!


Nephrine

  • Guest
graver outcome then Siftys
« Reply #73 on: May 14, 2003, 12:27:00 PM »
A similar thing happened to me when I was 15 except it involved potassium nitrate and sugar (4 cups of each), I was stirring the mixture on a ceramic stove when it ignited in my face (the guy with the fire extinguisher was taking a leak at the time) resulting in a month long stay at the hospital burn unit and markings on my face and hands. You know what they say: "what doesn't kill us makes us stronger and what kills us makes mom stronger"

Jubrail

  • Guest
Early failure
« Reply #74 on: June 02, 2003, 05:28:00 AM »
After extraction of DMT from MHRB, the first time I was ever in a real chem lab, I used a sep funnel to wash.  Being a complete idiot I had done everything wrong at every point, yet still yielded a small amount.  Of course, I dind't clean it up well and it was coated in NaOH.  I left my substance on a lit hotplate.  Smelling something burning I leaned over to check if it was my product.  Instead of wafting I inhaled a large amount of the vapor, which burnt the fuck out of my whole respiratory system and sent me onto the floor.  Definite pain.  I was lucky that I didn't get high off the D, that would have been a shitty trip.  Talked funny the rest of the day.


ClearLight

  • Guest
anhydrous ghb fuckup
« Reply #75 on: July 02, 2003, 10:53:00 AM »
Was preparing a 750 ml batch of ghb in a 2 liter flask when i noticed that the ph was 7.5 w/ only 30% of the molar gbl added...

  The process calls for addition of molar qty of NaOH to EtOH.  What I didn't do was check to make sure the 400 gms of NaOH was completely dissolved, due to cloudiness of rx mix and inability to see it completely... Skipping this step resulted in fusion of NaOH to the bottom of the flask, and then upon addition of water to try and cleanup/cool the partial reaction, a HUGE volcano of naoh/etoh/lactone/ghb/crap blows up out of the flask and covers the bench/floor/wall etc... 4 Hour CleanUP!

  Moral:  Make sure the solid is dissolved in the solvent!
         
          Never add H20 to anyhdrous reaction unless your SURE it won't react violently.


Antibody2

  • Guest
eyeballing doses
« Reply #76 on: July 03, 2003, 10:24:00 AM »
administering 2C-B without proper scales, dear god!


Bandil

  • Guest
Getting quite high off 2,5 mg's of DOB and...
« Reply #77 on: July 03, 2003, 10:28:00 AM »
Getting quite high off 2,5 mg's of DOB and ranting about how much fun it was, only to find out later, that it really was something else(non psychoactive) :)

Boy have i gotten sceptical about compounds after that one! Never underestimate the power of placebo!


pericles

  • Guest
Gah!
« Reply #78 on: July 06, 2003, 01:12:00 AM »
So I'm in my basement and, while playing with fire, notice that the matches I have seem to be leeching something blue. I conveniently have the bottle of 99% IPA I produced a few nights earlier by my side, so I soak a few matches in it, and get a blue liquid. Huh. Interesting.

Now I'm curious to get a sample of the substance itself, so I put the liquid on a watchglass, which is the only piece of glassware I'm daring enough to store at home. Hrm. No heat to evaporate it. OK, no problem. I take an empty vodka bottle and stuff its neck with napkins, which I then soak with IPA and ignite. OK, the flame's a bit bigger than I would have boped, but no problem.

Now, at this point I've realized that there's a reasonable chance the IPA in the watchglass will ignite when I try to evaporate it. I make a mental note not to try to blow it out.

OK, watch glass over flame.... A few minutes later the watchglass is damn hot, but most of the IPA is gone. So far so good. Ouch! Fuck that's hot! I shift the watchglass in my hand, causing a lone drop of IPA to dribble down the side/bottom of it. Instead the whole thing is on fire. SHIT!

Instinctively, despite my prior consideration, I try to blow it out. Naturally, burning IPA flies onto my desk, and from there onto my keyboard. Because I didn't have any glassware with which to dispense the IPA from the jar, I'd ended up making a fair mess of it when I poured it into the napkins, so there's a layer of it on the desk. Whoosh! It goes up in flames too.

OK. Priority 1: Keyboard. I have a small class of tea on my desk, which is instantly sacrificed to say my keyboard. Problem solved. Next I start frantically "mashing" the burning IPA with a plate on my desk, although at this point the desk itself is on fire.

Eventually the desk gets put out, and my keyboard lives (although there are some scorch marks).

What have I learned from this? If something seems like a really, really terribly stupid idea, it probably is.

pericles

  • Guest
Whoa!
« Reply #79 on: July 06, 2003, 01:35:00 PM »
Shit, really!? Thanks, there's no doubt in my mind you've saved me some major pain. It would have only been a matter of time.

But the glass _says_ Pyrex. Is all Pyrex not created equal?

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!" :(


Bozakium

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
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

  • Guest
"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

  • Guest
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...