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Author: Subject: Bad days in the lab or with glassware?
Texium (zts16)
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[*] posted on 30-7-2016 at 09:28


Quote: Originally posted by mayko  
This has been a bad *summer* in the lab, or rather out of it b/c it's so hot in the shed that the hot surface warning sensor on the hot plate trips :(
I feel for ya man. The other day I saw that my thermometer, sitting in a drawer in my lab bench, was reading 42ºC. This summer I've had to get up early in the morning any day I've wanted to do anything in my lab, and by 11AM I have to come back inside the house. On some days I've actually gotten up at 5AM and gotten into the lab before dawn, and that's great but I can't seem to keep that schedule up for more than a few days at a time.



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myristicinaldehyde
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[*] posted on 22-8-2016 at 12:24


I was mass extracting aspirin from tablets, but using my hot plate rather than microwave. I used a round bottom with water to allow a surprisingly effective reflux, but I put the stopper harder in than I thought. Instead of leaking steam, it popped out with incredible velocity, followed by the lovely tinkling of Chinese glass :/ Oops.
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Texium (zts16)
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[*] posted on 22-8-2016 at 12:28


Dude. Don't heat a closed system. Ever.*

*Unless of course it's an apparatus that's meant to operate at high pressure, but that's another story.




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myristicinaldehyde
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[*] posted on 22-8-2016 at 12:59


And check first if it is a closed system!
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Texium (zts16)
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[*] posted on 22-8-2016 at 13:54


I mean, if it has a stopper in it, I'd definitely consider that to be closed whether the stopper was loose or not. If you don't want it to be completely open, stick a thermometer adapter or something in there. Or better yet, a condenser.



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XeonTheMGPony
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[*] posted on 22-8-2016 at 19:10


Quote: Originally posted by zts16  
I mean, if it has a stopper in it, I'd definitely consider that to be closed whether the stopper was loose or not. If you don't want it to be completely open, stick a thermometer adapter or something in there. Or better yet, a condenser.


or a bubbler air lock!

My hand healed up well from a beaker that shattered in my hand while I was drying it, you got to be all ways care full and vigilant with glass from any place!

[Edited on 23-8-2016 by XeonTheMGPony]
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[*] posted on 24-8-2016 at 18:17


Another one *DJ Khaled voice*



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[*] posted on 27-8-2016 at 02:26


Today was a really bad day in my lab. I was synthesizing hydroiodic acid by hydrolyzing phosphorus triiodide. First, I got a nice, clear mixture of hydroiodic and phosphorous acids. Then the distillation flask fell from the apparatus and I had a minor spill of the mixture.

But wait. There is more! It turned out that my Liebig condenser had some minuscule amount of sulfuric acid from my previous experiment. When HI started distilling, it reacted with this sulfuric acid, and I got milky white distillate with a smell of hydrogen sulfide!

Of course, I immediately stopped the distillation.

Results: 80% of my solid iodine stockpile was depleted in vain. I got no hydroiodic acid. People, watch out for dirty Liebigs before you start any distillation!




Smells like ammonia....
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[*] posted on 17-9-2016 at 06:06


Well I can't compare to that I think I snapped the cheapest 24/40 adapter in existence. 90° Gas outlet/inlet



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Sulaiman
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[*] posted on 30-9-2016 at 08:54


today I was experimenting, developing a diy magnetic stirrer
I put the spinning magnets too close to my one and only large beaker ... :(
it was so useful

on the brighter side, I now have plenty borosilicate shards to test as column packing :P




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[*] posted on 30-9-2016 at 09:21


The Rule-of-10/4 :-

If it looks useful, buy 10.

By next week you'll have at least 4 left.




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[*] posted on 8-10-2016 at 17:52


Not a personal story but interesting nonetheless. 50 grams of Cs worth a whole lot of dollars.

https://youtu.be/ytxx95g-kiA?t=1m57s


He blames the fact that he was working with it in liquid form. I think his method for opening the ampoule is more to blame. He would have been better to have the whole thing submerged.


Fortunately he was able to redo everything with a fresh 50g of caesium. (gasp)
As an aside, is it just me or have other people noticed more and more amateur chemist YT contributors opting for commercial sponsorship lately?




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[*] posted on 8-10-2016 at 19:07


I've noticed more popular YT channels in general getting sponsored lately. I think businesses are catching on to the fact that these are a new and more marketable form of 'celebrity.'

Interesting to see that caesium is somewhat stable when coated with oil - I would have thought not even that would stop it.




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[*] posted on 11-10-2016 at 16:56


I broke two really nice pressure equalised addition funnels and a condenser on the same day. Saving 2 minutes to get another clamp cost $500

Never forget to clamp glass properly.
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[*] posted on 11-10-2016 at 18:15


I was distilling some benzyl chloride with plastic Keck clips. I shifted the glassware slightly, the clip holding the boiling flask melted and broke, the boiling flask fell, the boiling flask shattered, I got a face full of benzyl chloride. Last time I make that mistake again!
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[*] posted on 14-10-2016 at 02:33


Quote: Originally posted by elementcollector1  

Interesting to see that caesium is somewhat stable when coated with oil - I would have thought not even that would stop it.


Yes, it behaves pretty much like Willy Pete, slowly reacting with air, melting itself and finally igniting.




Smells like ammonia....
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[*] posted on 15-10-2016 at 20:55


I lost about 20% of my beakers two nights ago. I stupidly let my crystallization progress too long, and I was forced to drill the solid out with a knife, cracked a hole in the bottom of the glass. My other glassware fault was a thermal shock, due to the cooling temperature of nature. Damn thee vile mistress!


(Yes I only have 10 beakers)
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[*] posted on 16-10-2016 at 07:35


Lets see now.

Recently:

A red phos/I2 reduction about 4/5ths of the way through setup. Only accidental clogging of the bore of the flask neck, thought it was merely a coating spread along the surface where a little moisture had adhered some red P to the inner surface of the flask neck, only it wasn't, and by the time I'd realized it was actually a clogged neck, from using too narrow a flask, but, after addition of water, not realizing what had happened, had to sort the clog out by poking down the remaining P bit by bit (or rather, trying to)

It all went down at once, taking a splash of the water used to initiate the rxn and form HI(aq) along with it. Result? kicking off something fierce, rapid evolution of a HUGE plume of noxious acidic fumes, HI, PI3 and enough iodine vapor to leave my face, where unprotected by goggles and mask, looking like a panda in reverse. A laevo-panda, if you will:D

Had enough time to notice the 'plop' noise as a sizeable proportion of the phos and H2O slam dunked into the flask to think 'oh sHIIIi...!!; stepped back just in time to avoid the resulting krakatoa in microcosm.

That fucked up my calculations, owing to inability to calculate the quantity lost, seeing as the glassware itself had not been weighed beforehand, and lost a fair bit of the volatile elements of the reaction.

Did manage to salvage things by adding a bit more RP and a gram or two more of I2 to compensate for losses. Not my best work or finest hour.



And a less hazardous but perhaps nastier wee bit of squirrelyness.

Hotplate bust a gonad somewhere in the thermstat, and unbeknownst to Tsath', the damnable thing had gone and heated what was meant to be refluxing at 110-120 'C, had instead, been roasting at about 460-470 'C:o

Diethylene glycol in the heating bath absolutely stank something rotten. Its not strong, but it gives off this appalling, subtle sweetish-rancid-stagnant kind of stench when overheated to that temperature. Could smell it from several rooms in the house away through closed doors, don't quite know what it is thats so bad about it, as such, but it is, and fair made my guts heave.


Quite some time ago:

Distilling chromyl chloride, bottom of the still cracked and dropped out. Splattered the best part of a liter of 98% H2SO4, and stoich. quantities of NaCl and dichromate. Forgot which, potassium or sodium, either way, narrowly avoided getting doused from the waist down in the above, plus a few hundred ml, maybe a bit over a quarter liter, 300-350ml roughly.

Nasty, messy cleanup that was, cut away a section of contaminated bench top and replaced it with thick plywood. Not ideal but its the best I could rustle up at zero notice.

Had to rescue my £250-300 microscpe another time, after a company sent me a 4 gallon drum of conc. hydrochloric with a crappy tap that leaked vapors and over time, corroded the everloving shit out of a lot fo the metal stuff in the lab. Thankfully the optics and moving parts are unaffected and some lovingly applied acid to the stage of the 'scope got rid of the green color (nickel or chromium from the color I think) and a little tarnishing of the brass here and there on the lenses.

And last but not least, a permanent thickening of the palm of one hand, crappy skin condition there after spilling SOCl2 and having it eat right through the thickish leather gloves I was wearing at the time, then carry on going, right down to the muscle. Careless of me, but at the time I was just a little kid.

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[*] posted on 19-10-2016 at 06:11


This morning i had butter fingers and a 3/4 full gallon bottle of 50% H2O2 broke when i dropped it. And it was plastic! When it contacted the grass outside it started reacting and putting off steam. Now this stuff if left on a paper towl will combust in a matter of minutes. So it made a mess and i lost all my peroxide so i need to get more now. Not good start to the day. Luckily i can get the 50% stuff very easily and cheap.
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[*] posted on 22-12-2016 at 21:17


I took my brand new 600 mm reflux condenser out of the package yesterday only to discover that the internal coil was broken.

The seller is a reputable one and gave me an immediate refund. I guess with a little work I'll have a 600 mm Hempel column.

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[*] posted on 23-12-2016 at 05:22


Managed to get a large oval stirbar stuck in the neck of a 1L flask while pouring the product out of my reaction , almost 60 grams of a valuable intermediate, thankfully got most out before that, then when I turned the flask back upright slowly to try to get it to come loose, it popped back into the flask, right through the bottom of the flask. Still lost some material as hard to rinse the reaction contents from the flask then, but lost one of my favorite flasks. Just thankful not to have spilled much of the material in the process, also very acidic reaction, and I did not manage to spill much acid in the hood, which was nice.
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[*] posted on 28-12-2016 at 08:32


I was all ready for a good chemistry day today, when while I was making my morning tea I accidentally swept my hand over the spout of the kettle. Got a nasty steam burn to show for it, and now I'm not sure if I'll be able to do anything since it'll be hard to wear gloves, and I certainly don't want to expose the soft unweathered skin to potential chemical attack.

Edit: it is however making me wonder now if I could somehow convert a cheap, secondhand electric kettle into a steam bath...

[Edited on 12-28-2016 by zts16]




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[*] posted on 28-12-2016 at 08:51


Ouch !

Hope it heals up quickly to chemical-resistant status.

Washing-up tends to destroy more glass here than the actual usage. Today's loss was the drip spout on the new, only-used-once 250ml fritted vac funnel.

Saves having to clean the brown stuff out of the frit, so not all bad.




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Texium (zts16)
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[*] posted on 28-12-2016 at 14:53


Only the drip spout broke? Seems like you should still be able to use it.



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[*] posted on 28-12-2016 at 15:06


Vac will suck the liquid into the pump like mad without that bit of glass to prevent it.

Better to just get a new one.

To be honest, i do not really know what it's for (the entire fritted filter thing) so no great loss.

[Edited on 28-12-2016 by aga]




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