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Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
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Mood: Chemistry: the subtle science.
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In my recent refresher organic classes there weren't any ludicrous rules. Of course elemental phosphorus is long gone from any experiments, most
likely due to concerns about diversion rather than hazards. We used elemental sodium for fusions for qualitative analysis with no undue concern. An
oxymercuration experiment had been removed to eliminate the use of mercury compounds. A "thought experiment" was substituted for this. 
I did witness one dramatic fire. This was caused by the spillage of a flammable solvent onto the bench and a plastic distillation kit case with the
foam padding. This, along with a lit bunsen burner, resulted in an immediate and sizeable fire. The instructor kept his head and quickly put it out
- with just water.
The single most important condition for a successful synthesis is good mixing - Nicodem
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Formatik
National Hazard
Posts: 927
Registered: 25-3-2008
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Mood: equilibrium
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Bad days with glassware
I've had plenty of those. Thermometers, beakers, flasks, distillation flasks, you name it. The real heart-breakers are the more valuable and hard to
get items.
The most recent break occurred some time ago with a several year old 1-L Schott FB flask after being heated on a hotplate (which got over 500º
according to the multimeter), simply after removing the flask and setting it on a warm room temperature surface was enough to put several cracks in it
(I should have clamped the flask and let it air cool instead  ). Heating it
over instead of on the heat source should have helped too.
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psychokinetic
National Hazard
Posts: 558
Registered: 30-8-2009
Location: Nouveau Sheepelande.
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Mood: Constantly missing equilibrium
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My old chemistry teacher was a rugged sort - he's not allowed curtains anymore.
“If Edison had a needle to find in a haystack, he would proceed at once with the diligence of the bee to examine straw after straw until he found
the object of his search.
I was a sorry witness of such doings, knowing that a little theory and calculation would have saved him ninety per cent of his labor.”
-Tesla
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anotheronebitesthedust
Hazard to Others
Posts: 189
Registered: 24-6-2007
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Mood: No Mood
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I've broken so many lab glass items it's not even funny.
1L erlenmeyer flask
1 600mm gram condenser
2 600mm allihn condenser
1 5L1-neck RBF
1 5l 2-neck RBF
1 2L Sep funnel
1 4L Sep funnel
1 1L RBF
1 2L Beaker
1 50ml Pipette
The list goes on, I'm such a klutz, I need a new hobby.
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Magpie
lab constructor
Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline
Mood: Chemistry: the subtle science.
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Quote: Originally posted by anotheronebitesthedust  | I've broken so many lab glass items it's not even funny.
1L erlenmeyer flask
1 600mm gram condenser
2 600mm allihn condenser
1 5L1-neck RBF
1 5l 2-neck RBF
1 2L Sep funnel
1 4L Sep funnel
1 1L RBF
1 2L Beaker
1 50ml Pipette
The list goes on, I'm such a klutz, I need a new hobby. |
Wow, you work on a large scale. Maybe that is a factor breaking more items than usual?
The single most important condition for a successful synthesis is good mixing - Nicodem
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aonomus
Hazard to Others
Posts: 361
Registered: 18-10-2009
Location: Toronto, Canada
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Mood: Refluxing
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... add one 400mL beaker to the list
Stupid saturated sodium carbonate solution was slippery as hell when I was washing it in a tub, let it slip, it landed ontop of a half-submerged
filter flask, and shattered. Not a scratch on the filter flask though (thank goodness).
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JohnWW
International Hazard
Posts: 2849
Registered: 27-7-2004
Location: New Zealand
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Mood: No Mood
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Do not throw the broken glassware out, even if unrepairable! You should save up all the broken Pyrex (or other borosilicate brands) glass, until you
have enough to do your own glassblowing, to make your own custom glassware.
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havarti_gouda
Harmless
Posts: 33
Registered: 23-1-2010
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Mood: No Mood
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Here's something I learned which resulted in a SLICED UP hand and ruined glassware.
NaOH + glass = SEALED.
I was trying to pull the glass stopper out of an RBF, that had NaOH solution sitting in it and sealed, with a pair of plyers among other things. Put a
HUGE gash in my hand when glass broke.
Moral of the story: Don't let strong NaOH solutions sit for several days in closed up glassware. :-)
Otherwise, butter fingers and not realizing something is blazing hot have been the causes of me breaking a plethora of glassware.
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User
Hazard to Others
Posts: 339
Registered: 7-11-2008
Location: Earth
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Mood: Passionate
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Little of topic maybe but..
How bad is NaOH in solution for glassware.
Oke, I know that NaOH eats glass.
But to what extend can this do damage to glassware??
I understand that having molten hydroxides in a glass container is just plain stupid but how about strong heated alcoholic solutions?
I normally use old glass for reactions with OH's.
Is it really something to be considering or are the rates so low that it might be just panicing over nothing.
User
What a fine day for chemistry this is.
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entropy51
Gone, but not forgotten
Posts: 1612
Registered: 30-5-2009
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Mood: Fissile
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Best to avoid glass stoppers with strong bases. If you use them, and I sometimes do, use good stopcock grease on the stopper. When I want to avoid
grease, I put a strip of filter paper about 5 mm wide into the joint with the stopper. The paper strip prevents the stopper from sealing tightly and
sticking.
I once broke a small bottle of Br2 in the same way. But I had on thick work gloves and got neither cut nor burn. The red clould does tend to focus
one's attention however.
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User
Hazard to Others
Posts: 339
Registered: 7-11-2008
Location: Earth
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Mood: Passionate
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Ohm man today sucked.
I broke a mercury thermometer.
I was cleaning the wall of my lab with some ammonia really nice black smudge coming of.
There was a thermometer hanging on the wall, it was an old one and the mercury had split because apparently it was lying down for a long time.
Anyway somehow I and my stupid head tipped the thing of the hook and it fell down on my desk.
It god damn shattered.
So yeah i had tiny drops of Hg all over the fucking table top.
I spent 2 hours of cleaning it with an eye dropper and still not convinced that it is all gone.
I used the last of my sulphur on the floor.
Now ill be putting the radiator at max with the window open hoping to evap all of it.
Maybe ill put my gassmask on and use a blow-dryer.
What a way to start your freaking day.
Any one got some tips?
What a fine day for chemistry this is.
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Jor
National Hazard
Posts: 950
Registered: 21-11-2007
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Mood: No Mood
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Zinc powder is more effective than sulfur. You COULD use the vaccuum cleaner, although this is generally not recommended and is dangerous, as lots of
vapours form, but i think you will be fine as long as the exit (where the hot air comes out of the cleaner) is going into a hood or outside.
Well in a thermometer there is only a few grams. Say you cleaned most of it, the amount of mercury present is only a threat if you live in the room
daily but if your lab is your garage and it has ventilation, I think you'll be fine.
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User
Hazard to Others
Posts: 339
Registered: 7-11-2008
Location: Earth
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Mood: Passionate
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Well i cleaned up the mess.
Had an electric heater running all night with the window open.
This morning i vacuum cleaned my whole lab.
Had a ventilator running and I was wearing a gas mask.
Maybe iam over reacting but i hate the idea of chronic poisoning.
I feel quite convinced that its fine now, my lab has never been this clean.
Also I have a nice sealed of glass tube with some Hg.
What a fine day for chemistry this is.
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bbartlog
International Hazard
Posts: 1139
Registered: 27-8-2009
Location: Unmoored in time
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Shattered a porcelain dish in the microwave yesterday. Had some mixed CuCO3/NiCO3 that I had partly decomposed into oxides by heating on the hot
plate, but being unsatisfied with the progress I put them in the microwave. CuO however is quite a good microwave susceptor, and after just a few
minutes the thermal stress cracked the dish. Luckily the microwave was unharmed.
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rrkss
Hazard to Others
Posts: 193
Registered: 18-12-2009
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Got a new delivery of glassware. Everything was intact except for one multinecked 250 mL Roundbottom was planning on starting a multistep temperature controlled synthesis tommorow using that flask but now I have to wait
until it gets replaced.
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anotheronebitesthedust
Hazard to Others
Posts: 189
Registered: 24-6-2007
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| Quote: |
Well i cleaned up the mess. Had an electric heater running all night with the window open. This morning i vacuum cleaned my whole lab. Had a
ventilator running and I was wearing a gas mask. Maybe iam over reacting but i hate the idea of chronic poisoning.
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http://www.test4mercury.com
There's a video at this website that shows the mercury vapors.
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Ozone
International Hazard
Posts: 1269
Registered: 28-7-2005
Location: Good Olde USA
Member Is Offline
Mood: Integrated
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Here's one of the more recent "tragedies". Bottom fell out of this flask while it was in the sonicator.
Solves that ship in the bottle problem, though .
Cheers,
O3
 
[Edited on 14-2-2010 by Ozone]
-Anyone who never made a mistake never tried anything new.
--Albert Einstein
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The_Davster
A pnictogen
Posts: 2861
Registered: 18-11-2003
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Mood: .
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Popped the stopper in my column for flash chromo the other day while adjusting the nitrogen flow. Glass stopper went up, and came down landing on a
funnel, shattering it. Oh well, it was filled with used drying agent, and was at work. No personal investment, no loss. 
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UnintentionalChaos
International Hazard
Posts: 1454
Registered: 9-12-2006
Location: Mars
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Mood: Nucleophilic
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| Quote: Originally posted by bbartlog | Shattered a porcelain dish in the microwave yesterday. Had some mixed CuCO3/NiCO3 that I had partly decomposed into oxides by heating on the hot
plate, but being unsatisfied with the progress I put them in the microwave. CuO however is quite a good microwave susceptor, and after just a few
minutes the thermal stress cracked the dish. Luckily the microwave was unharmed.
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I'll do you one better. Was dehydrating MgSO4*7H2O in the microwave in a glass dish with fairly thick walls, which goes fairly readily and gets pretty
hot. I've previously done CaCl2 with no hitches and once dry, let it run a few minutes more just to make sure. Well, anhydrous MgSO4 seems to be a
better microwave acceptor than anhydrous CaCl2, because during those few extra minutes, the bottom of the glass dish melted and fused
to the glass plate in the microwave under it.
Department of Redundancy Department - Now with paperwork!
'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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crazyboy
Hazard to Others
Posts: 436
Registered: 31-1-2008
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Mood: Marginally insane
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| Quote: Originally posted by UnintentionalChaos |
I'll do you one better. Was dehydrating MgSO4*7H2O in the microwave in a glass dish with fairly thick walls, which goes fairly readily and gets pretty
hot. I've previously done CaCl2 with no hitches and once dry, let it run a few minutes more just to make sure. Well, anhydrous MgSO4 seems to be a
better microwave acceptor than anhydrous CaCl2, because during those few extra minutes, the bottom of the glass dish melted and fused
to the glass plate in the microwave under it. |
I had that happen to me once, had to replace the microwave, but I guess that's what happens when you try to cut time.
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Safetylast
Harmless
Posts: 1
Registered: 28-1-2010
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Mood: No Mood
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When I was a kid I would use a large 4 cup Pyrex measuring cup placed directly onto a hot plate for boiling. It worked fine for a while, but one day I
was boiling a KCl solution for KClO3 production and couldn't dissolve all of the KCl. I stupidly added some room temp water to the measuring glass
full of boiling solution and BOOM, hot water and broken glass everywhere. It scared the piss out of me. Luckily I was uninjured, I made a lot of dumb
mistakes as a kid.
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Panache
International Hazard
Posts: 1290
Registered: 18-10-2007
Member Is Offline
Mood: Instead of being my deliverance, she had a resemblance to a Kat named Frankenstein
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| Quote: Originally posted by JohnWW | | Do not throw the broken glassware out, even if unrepairable! You should save up all the broken Pyrex (or other borosilicate brands) glass, until you
have enough to do your own glassblowing, to make your own custom glassware. |
Yeah right, your own custom glassware, have your tried this shit, i have most of the requisite tools (well a glassblowing torch, a lathe (actually
that's an old rotovap converted, and a kiln, i do however have shitloads of new glassblowing blanks, fittings etc, oh i also have several books and
brass tools) and my best work is so crap that it cracks if you walk with it past the refrigerator, or the oven, even if neither are on, it just gets
scared. I would not trust it to do anything in.
However i have some other advice, if you give a toss about recycling, don't throw your borosilicate into the glass recycling even small inclusions
decrease the efficiency of the processes dramatically. I shared a lab with a laser dude once who was trying to develop a fast detection method to
enable a process line to punch out of the line any possible borosilicate.
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rrkss
Hazard to Others
Posts: 193
Registered: 18-12-2009
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Mood: No Mood
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Was doing a reaction that involved a solution of NaOH. Ended up freezing the joints to one my adapters. Being stupid, I took a pair of pliers and
got the joints free but at the expense of shattering the adapter.
In short, don't use pliers to free frozen joints and use grease if you are working with strong bases.
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JohnWW
International Hazard
Posts: 2849
Registered: 27-7-2004
Location: New Zealand
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Mood: No Mood
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| Quote: Originally posted by JohnWW | | Do not throw the broken glassware out, even if unrepairable! You should save up all the broken Pyrex (or other borosilicate brands) glass, until you
have enough to do your own glassblowing, to make your own custom glassware. |
I can suggest another two uses for broken pieces of heat-resistant borosilicate pyrex-type glass:
(b) After breaking them into reasonably uniform sized pieces, they could be used as packing for a packed column, which could be used for two-phase
gas-liquid reactions, in which usually the liquid enters from the top and the gas is forced in from the bottom.
(c) Broken into fairly small pieces, they could be used as "bumping chips" in beakers or flasks in which a liquid is boiled.
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Skyjumper
Hazard to Self
Posts: 93
Registered: 1-3-2010
Location: Assachusetts
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Mood: Refluxing
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Lets see
Glass stir rods x5
Glass tubing I dont even know
3 earlimyers, 250-500ml
Plenty of beakers
a pipette pump
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