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Author: Subject: Bad days in the lab or with glassware?
Vosoryx
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[*] posted on 20-11-2017 at 09:59


Quote: Originally posted by TheNerdyFarmer  
I recently broke my liebig condenser. Was a very sad day. With this recent unfortunate event, my ongoing project has come to a halt and I am forced to wait patiently by the mailbox for its replacement to come.




Same here.
It was a really stupid way to break it, too. I had just finished a distillation, and turned the heat off. I took out the fraction i wanted, replaced the reciever to catch the tail, and decided i didn't want to come back out to the lab that evening, so i turned off the coolant water. Then it occured to me that now the fumes weren't condensing, the vapour was just being offgassed into my lab. So i filled up the water jacket, and plugged the ends and left.
I live in canada.
My lab is in an unheated shed.
It froze.
So did the water in the condenser jacket.
On the bright side, more boiling stones!


I ordered two, just so this doesnt happen again. It's hard, not being able to do what i want...
Oh well. With the extra time i deepcleaned by lab and assembled my aspirator pump.
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[*] posted on 2-12-2017 at 14:40
Lab without heating mantle


It wasn’t “just” a heating mantle for 250mL that broke when I added the calculated amount of NH4Cl that should form a sarurated solution at the bp. of water. The RB flask was already hot and after adding the NH4Cl to the 250mL RB flask everything went wrong. When water was added it didn’t take 1 minute to see sparks on the heating mantle and suddenly I saw a white solid on the mantle. This did cause even an short circuit..

This accident was caused by hot glassware in combination with the endothermic reaction. Just a few weeks earlier the hot plate on the magnetic stirrer wasn’t work anymore.

To make it all worser the new lab equipment is still ordered and payed... 2 weeks ago and this company even didn’t check the e-mails or when you call: voicemail.

I have no idea what to do without destillation, cleaning up the lab, I can do crystallizations in the cold, filter out solid particles (e.a impurities), measuring the dendity of various solutions and determine the concentration/M.

3 accidents in just 2 weeks: it’s enough!
An accident comes never alone... :(
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[*] posted on 15-12-2017 at 10:54


I was vacuum filtering off a dilute nitrating mixture (1:1 H2SO4:HNO3) from ETN, and forgot to check the level of my receiving flask (my Buchner frit has a vacuum neck built in, which I'm not used to), and sucked a good 10 mL of solution into my vacuum pump. Luckily, I was using a positive displacement pump (diaphragm type), and the diaphragm didn't react with the solution, miraculously. The solution that didn't stay in the pump was sprayed out of the exhaust side. I'm pretty sure a bit got on my ceiling. That was probably the worst lab accident I've had in a long while, followed by at least an hour of cleanup. I felt so stupid after that one.



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[*] posted on 23-12-2017 at 19:24


Trying to make magnesium nitride today, apparently red hot magnesium isn't compatible with fused quartz :)

I think that it made magnesium silicide with the glass, judging from the small explosions when I tried to clean my tube with HCl. Strong acid and vigorous scrubbing wont take the black color off. Now my tube doesn't look very nice anymore :(

https://www.youtube.com/watch?v=zpJrhak5NdE
I was really surprised when I heard the popping!




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[*] posted on 24-12-2017 at 16:35


I decided it would be a good idea to try to fit a brush between the coil and wall of my reflux condenser. Big mistake. Once I extract the coil and seal the tube I'll have another air condenser.... Next time I am going to try pipe cleaners.



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[*] posted on 24-12-2017 at 21:58


There was a monstrous hunstman spider in my bathroom which is where I do any experiments that require some level of ventilation. Luckily it didnt happen while i was in the middle of doing something... I was lucky enough to notice the beast from outside of my bathroom where it was as my door was open and i looked in and there it was... a spider with a legspan almost the size of a dinner plate that is usually noticed very high on a wall or corner, which is fine as long as you make this observation from the other side of the room... not when it's in the same corner as you and you dont even know its there until you turn around or look up from where ur sitting and its directly above your head or in a place that essentially traps you in a small space with this thing... millions of yrs of evolution has programmed me to feel a dread and fear so primal and debiliating when i see this thing... its really kinda cool in a way... not at the time lol]




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[*] posted on 26-12-2017 at 02:18


Quote: Originally posted by WangleSpong5000  
There was a monstrous hunstman spider in my bathroom which is where I do any experiments that require some level of ventilation. Luckily it didnt happen while i was in the middle of doing something... I was lucky enough to notice the beast from outside of my bathroom where it was as my door was open and i looked in and there it was... a spider with a legspan almost the size of a dinner plate that is usually noticed very high on a wall or corner, which is fine as long as you make this observation from the other side of the room... not when it's in the same corner as you and you dont even know its there until you turn around or look up from where ur sitting and its directly above your head or in a place that essentially traps you in a small space with this thing... millions of yrs of evolution has programmed me to feel a dread and fear so primal and debiliating when i see this thing... its really kinda cool in a way... not at the time lol]


And here you could get £65 for it!! Happy days if i saw a few of those in my room!

On a sad note, i left water in my condenser overnight :(, the room is cold and unheated and the water turned to a solid....
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[*] posted on 26-12-2017 at 03:37


Quote: Originally posted by NEMO-Chemistry  

And here you could get £65 for it!! Happy days if i saw a few of those in my room!


65 Quid?!?! Really? I'm assuming the market for them is as pets not for the other far more lucrative reason which is milking certain spiders for thier venom, primarily for the purpose of attaining anti-venom from them

I can't imagine being terrible profitable. It can be if you breed the spiders yourself and you are selling them within your own country or say within the EU if you live there. I dont believe you need to attain costly liscences but if you were exporting them thats a whole different kettle of fish. In the case of milking them from the venom is a little different. In Australia the Syndey funnel web spider is debatably the most dangerous spider in the world. If you are ever bitten it is encouraged where possible to attempt to capture the spider and bring it to the hospital. The reasons are two-fold: Firstly, it's done for identification purposes. Anti venom (and don't quote me on this) may have very adverse effects if the wrong one is given, I presume this is becauase whatever positive effects the incorrect anti-venom may have (if any... it may make it worse?) they are outweighed but whatever those risks are. The thing is there are many highly venomous spiders here that look just like funnel webs and to the untrained eye they look almost identical.
Secondly they need as many spiders to milk as they can... spider venom is an extrmely complex mixture of countless differenent toxins.

Taken from Wikipedia:
"Delta atracotoxin (δ-ACTX-Ar1, robustoxin, or robustotoxin) is a low-molecular-weight neurotoxic polypeptide found in the venom of the Sydney funnel-web spider (Atrax robustus).
Delta atracotoxin produces potentially fatal neurotoxic symptoms in primates by slowing the inactivation of sodium ion channels in autonomic and motor neurons. In the spiders' intended insect prey, the toxin exerts this same activity upon potassium and calcium ion channels.[1]
The structure of atracotoxin comprises a core beta region with a cystine knot motif, a feature seen in other neurotoxic polypeptides".[1][2]

This stuff is worth alot of money but I think you see a special permit for it.

Sorry for the format error... that was very strage.

[Edited on 26-12-2017 by WangleSpong5000]




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[*] posted on 26-12-2017 at 04:45


Exotic spiders are kept as pets here, The ones with dangerous venom you need a license (just like you do with snakes), i dont fancy milking spiders! for a start with my luck it would be a male spider ;). Plus your gonna get back ache on a milking stool that small :D.

I am allergic to Bee's big time, i carry a special pen in case i get stung. I love spiders and snakes but its recommended that people who are allergic to Bee's dont keep them. I cant remember the name of it, but there is an extremely common spider in the UK, its supposed to be the most venomous of all spiders. Its perfectly safe however as its only 7mm full size, it cant harm or bite people because of the tiny size, but the actual toxin in supposed to be amongst the most dangerous.

Nature is a funny thing, the fangs on this spider are so small it cant hurt much, and yet its poison is really bad...

I hear some spiders in Aus like hiding under toilet seats! Thats just plain out of order! a man should be allowed to have a shit in peace FFS.
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WangleSpong5000
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[*] posted on 27-12-2017 at 22:49


Deleted due to me incorrectly formatting it in a dead dogs arsehole

[Edited on 28-12-2017 by WangleSpong5000]




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[*] posted on 27-12-2017 at 23:39


I generally don't have a problem with spiders, all except the white tail, I can't stand white tails and kill them on site.

I killed 9 of em' in one week here last month, two of them were absolutely massive, they get huge here in S.A and this morning when I got up and put my jeans on guess what falls out of the leg and scurries under the bed? yep, a bloody white tail spider.

Good thing I'm leaving soon, I'm sick of these damn white tails
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WangleSpong5000
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[*] posted on 28-12-2017 at 06:18


Quote: Originally posted by NEMO-Chemistry  
Exotic spiders are kept as pets here, The ones with dangerous venom you need a license (just like you do with snakes), i dont fancy milking spiders! for a start with my luck it would be a male spider ;). Plus your gonna get back ache on a milking stool that small :D.

I am allergic to Bee's big time, i carry a special pen in case i get stung. I love spiders and snakes but its recommended that people who are allergic to Bee's dont keep them. I cant remember the name of it, but there is an extremely common spider in the UK, its supposed to be the most venomous of all spiders. Its perfectly safe however as its only 7mm full size, it cant harm or bite people because of the tiny size, but the actual toxin in supposed to be amongst the most dangerous.

Nature is a funny thing, the fangs on this spider are so small it cant hurt much, and yet its poison is really bad...

I hear some spiders in Aus like hiding under toilet seats! Thats just plain out of order! a man should be allowed to have a shit in peace FFS.


In the case of funnel webs it's the males the pay primarily milk, they are something like 9 times more venomous than the female, or at least they are 9 times more deadly which which could be mean they inject more venom per bite and/or the venom itself it far more toxic. Again... don't quote me on the specifics lol

The small fangs thing is true here for red back spiders. Probably number 2 or 3 of Australias most deadly spiders. They are quite small with maybe an abdomen the size of a pea. It they bite you on the hand or the sole of the foot you are fine (kind of) as their fangs don't penetrate the skin well. If the bight you on the arse you are in serious trouble. Happened to a friend of mine once. The bight wasn't particularly painful and he was completely fine for about 1 hour. After that? He was certainly NOT fine... I got to see first hand the symptoms of spider venom... and they were horrific. He was delirious and trying to pull out the hospital IV's. He was sweating profusely and wailing in agony. This went on for many hours. Scary stuff! I found one the other month in a small web under my porch deck chair.

The fact is these spiders are everywhere here but they really are nothing to fear. Just don't put your fingers anywhere you can't see and never leave your shoes outside.

The toilet seat thing is true but really only applicable to those that live in the outback or the country where people have outside toilets. This is a bit of a throwback to the Australia of yesteryear and not really an issue today.

For me the biggest concern a huntsman spiders because you WILL find them in your house and there WILL be more than one. Generally during the summer months which is now in Aust. They are harmless but I don't care. They are fucking huge and very fast but in reality they just sit in the corner of a room motionless for hours, even days on end and they aren't aggressive.




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[*] posted on 28-12-2017 at 08:30


Destroying your electric coffee grinder trying to grind steelwool into a powder for nitroarene reduction... only to find that iron powder and magnetic stirring don't work together anyway. :)
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[*] posted on 28-12-2017 at 08:43


I can't picture a coffee grinder being able to deal with steel wool particularly well either :D



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[*] posted on 28-12-2017 at 08:56


Wasn't sure which would be grinding which either, it put up a descent fight though.
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[*] posted on 9-3-2018 at 20:06


"Tink"

The noise no one wants to hear.

IMG20180310135423.jpg - 774kB




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[*] posted on 31-3-2018 at 11:12


Today one 2.5 l bottle containing acidified n-butanol (wood paint drying accelerator = BuOH + 5-7% HCl) burst and spilled its content all over the floor (or whatever you call tessellated broken pavement). The odd thing is that a few minutes before that happened, I just left my lab, and when I came back I began hearing drips of liquid hitting the floor and a strong smell of BuOH in the air. I quickly removed all the other bottles and boxes from the shelf and below, two were already soaked and ended up burning them in the yard. I quickly washed the shelves with water to remove all acid traces. Since my lab is just two walls, a half-wall and a crappy door and there's a permanent strong air draft if the door is open, the solvent was gone in a few hours, and so far I haven't seen any signs of corrosion from the acid vapors, though I might have to wait a few more days to be sure.
I'm not sure what caused the bottle to burst. The upper part of the bottle was "decapitated", so I believe there was pressure build-up from the HCl, which must have desorbed from the BuOH (though I never had any problems last summer when it was very hot). However, I also have another 2.5 l bottle with the same stuff, and when I opened it to check it, there was no pressure release. Originally the BuOH was kept in different bottles and a few weeks ago I added the BuOH to two different bottles. Both bottles were filled and closed at the same time, and both kept in the same conditions, at relative low temps (5-10 °C) and in dark. The only other explanation that I can think of is that I filled the first bottle almost to the screw level, while the second was only filled to the 2.5 l mark, though there must have been quite some pressure build-up in such a small place to break the bottle like that (the whole bottle broke in multiple pieces). One thing I remember is that the bottle itself might have had a defect, since I recall having an empty bottle with a small air bubble in its glass wall, and maybe that's where it broke and caused the whole bottle to shatter.
To avoid similar incidents in the future, I think I'll keep the other bottles in buckets, so that if they break, they won't spill content all over the lab. And avoid any bottles with even the slightest defect.
Oh and if anyone wonders why I kept the BuOH with HCl, it's because I never got around to neutralize it, let alone distill the BuOH.




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[*] posted on 31-3-2018 at 12:08


Quote: Originally posted by Mabus  
Today one 2.5 l bottle containing acidified n-butanol (wood paint drying accelerator = BuOH + 5-7% HCl) burst and spilled its content all over the floor (or whatever you call tessellated broken pavement).


Can you share the name of this product? I have looked for BuOH everywhere and haven't seen it on shelves.




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[*] posted on 31-3-2018 at 14:37


Sure. The product is an acid-curing parquet lacquer/varnish (for some reason I can't find a similar product in the West) and the one I use is this one (though the bottle I bought from the store is slightly different):
https://www.adrenco.ro/image/cache/data/Lacuri/intaritor-dur...
I can't find an SDS for the product in English on the manufacturer's site.
Other products also have xylene besides butanol. Some parquet glues have isobutanol instead of n-butanol. Interestingly, while I can find both acidic and neutral isobutanol lacquers in hardware stores, I haven't been able to find products with neutral n-butanol.




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[*] posted on 1-4-2018 at 18:23


I was working with a solution of indole in ethanol today and some bad technique resulted in a minor spill with splashing onto me, of course. The garage smells interesting. When I came into the house to clean up, my wife asked me if I had filled my pants. That smell cannot be washed off. It looks like a few nights on the couch are now facing me.

I am still going to finish that damn reaction.

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[*] posted on 9-4-2018 at 07:53


Spilling a solution of HgSO4 and H2SO4 into your glove can really ruin your day! I will never pick up sth off the floor again next to the bench while working with hazardous stuff, seriously. Learned it the hard way.
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[*] posted on 9-4-2018 at 10:00


What's the relationship between this thread and this one?
https://www.sciencemadness.org/whisper/viewthread.php?tid=24...
It almost looks like one was split from the other, though I don't see any thread-split markers.




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[*] posted on 9-4-2018 at 14:33


Quote: Originally posted by mayko  
What's the relationship between this thread and this one?
https://www.sciencemadness.org/whisper/viewthread.php?tid=24...
It almost looks like one was split from the other, though I don't see any thread-split markers.

My error. I submitted a post to the wrong thread. I had no idea there were two.
I will merge them together -- that seems to be a logical thing to do.




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[*] posted on 18-5-2018 at 21:17


Corn cob, you can go furfural yourself...

IMAG5914.jpg - 1.1MB IMAG5972.jpg - 927kB

Had a few min extra to prep Corn cob for drying before work, shove it in the dehydrator. The better half checks in to see what I'm up to just in time to catch me try to crown my ring finger... Working hands fought back despite applying more than enough force.

Some time down the road I want to have a go at furfural for learning experience and a few ml to inspect. Then compare pine sawdust route maybe. Should be getting more time home soon... Chemistry may actually get to happen instead of just being read.




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[*] posted on 26-5-2018 at 15:18


Quote: Originally posted by nitro-genes  
Destroying your electric coffee grinder trying to grind steelwool into a powder for nitroarene reduction... only to find that iron powder and magnetic stirring don't work together anyway. :)


Ah, your pain will be very helpful to me indeed. I still may try this as an experiment, but mostly without the expectation of success!

Thank you!
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