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Author: Subject: Bad days in the lab or with glassware?
Magpie
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[*] posted on 8-1-2010 at 09:38


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
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[*] posted on 8-1-2010 at 16:20
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 :mad: ). Heating it over instead of on the heat source should have helped too.
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psychokinetic
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[*] posted on 9-1-2010 at 12:20


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
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[*] posted on 10-1-2010 at 16:03


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
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[*] posted on 10-1-2010 at 16:12


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
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[*] posted on 11-1-2010 at 15:08


... 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
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[*] posted on 11-1-2010 at 16:12


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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[*] posted on 29-1-2010 at 19:12


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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[*] posted on 29-1-2010 at 20:04


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.

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What a fine day for chemistry this is.
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entropy51
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[*] posted on 30-1-2010 at 08:05


Quote: Originally posted by havarti_gouda  

Moral of the story: Don't let strong NaOH solutions sit for several days in closed up glassware. :-)


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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[*] posted on 7-2-2010 at 09:55


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. :mad::mad:

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
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[*] posted on 7-2-2010 at 10:52


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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[*] posted on 8-2-2010 at 10:29


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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[*] posted on 8-2-2010 at 10:50


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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[*] posted on 9-2-2010 at 11:03


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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[*] posted on 13-2-2010 at 07:09


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.

http://www.test4mercury.com
There's a video at this website that shows the mercury vapors.
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[*] posted on 13-2-2010 at 08:08


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

2L with actinic_01_small.jpg - 199kB New and Improved 2L_small.jpg - 137kB

[Edited on 14-2-2010 by Ozone]




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[*] posted on 13-2-2010 at 08:58


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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[*] posted on 13-2-2010 at 10:51


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.



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.




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'In organic synthesis, we call decomposition products "crap", however this is not a IUPAC approved nomenclature.' -Nicodem
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[*] posted on 14-2-2010 at 16:00


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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[*] posted on 15-2-2010 at 15:45


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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[*] posted on 16-2-2010 at 03:00


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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[*] posted on 25-3-2010 at 21:57


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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[*] posted on 26-3-2010 at 01:16


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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[*] posted on 28-3-2010 at 18:40


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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