Author Topic: Your Really STUPID Lab Mistakes....  (Read 13484 times)

0 Members and 1 Guest are viewing this topic.

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?