Sciencemadness Discussion Board

Bad days in the lab or with glassware?

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ave369 - 12-11-2015 at 01:51

Quote: Originally posted by TheAlchemistPirate  
I now have a problem of finding an outdoor lab in the land of the eternal night, however...


This is a minor problem compared to what I have. I live in a country known for high latitudes, and this means both short day and cold climate. Right now, any outdoor lab for me means bitter cold, not just darkness.

The Volatile Chemist - 19-11-2015 at 10:10

Ouch. Our humidity is bad here in the summer, though not half as bad as south of here. Very wet, nothing evaporates on its own accord...except the things you don't want to evaporate.

mayko - 17-12-2015 at 15:49

I made a batch of trisodium phosphate a few days ago from phosphoric acid and sodium hydroxide. I let the reaction mixture cool overnight, and found some very lovely crystals in the bottom of the beaker.

Here began the comedy of errors. I poured off the supernatant into a funnel with filter paper, then broke up the crystals in the beaker. When I turned back to the funnel, I learned that the mother liquor had been supersaturated, and had solidifed halfway through the filtration!

To wash the solids of excess sodium hydroxide, I added some dry ethanol and stirred the slurry. Sadly, I did not use a proper stirring rod, and instead picked up a piece of glass tubing. It promptly snapped and I got a puncture/slice in my finger! (However, the blood dripping in the water of the wash basin made some very pretty patterns!)

I also managed to splatter silver nitrate solution all over myself in an unrelated incident and now have purple splash marks all over me. I didn't realize I had one on my forehead, though, until I'd been walking around with it for a day!


The Volatile Chemist - 30-12-2015 at 14:35

Haha, not fun...glad we have a place to joke about it, as I've found not many other people find the mistakes funny or are sympathetic.

aga - 31-12-2015 at 09:32

Was running out of sulphuric acid so went looking for some today.

25 litres of 36% for 16 euros, and i get to keep the container !
Very clear as well, unlike the drain cleaner stuff.

So, boiling some down is the obvious thing to do.

Add a Fan to speed things up ! Why not ?

BECAUSE THE BEAKER WAS TOO FULL YOU IMPATIENT CRETIN !

Quite a bit of acid got dumped straight onto the hotplate.

Never reached 98% conc so fast !

Sadly it rapidly decomposed, overwhelming the fume hood fan with choking thick white vapour.

First time i've had to clean up the hotplate whilst still very hot, and wearing a gas mask.

If it were not for the fume hood and gas mask, the best i could have done would be to pull the mains fuse out of the electricity meter 100m from the shed and wait for the choking SO2 to dissipate.

[Edited on 31-12-2015 by aga]

The Volatile Chemist - 31-12-2015 at 11:17

Ouch...
I've been hating the rate at which things evaporate here. 50 mLs of Zinc Acetate evaporating for 3 weeks, down to a little under 40 mLs...
I don't want to waste my NaOH or CaCl2, so I dessicated it in some anhydrous Copper(II) Sulfate. Turns out anhydrous copper(II) Sulfate is a terrible desiccant... going to do desiccant research as soon as the dumb stuff crystallizes...

aga - 31-12-2015 at 11:22

CaCl2 is wonderful stuff.

Make a LOT of it and keep it dry.

The Volatile Chemist - 31-12-2015 at 15:45

Tis a good plan, I should buy a bunch of CaO.

ave369 - 3-1-2016 at 06:51

Quote: Originally posted by aga  


[Edited on 31-12-2015 by aga]


Boiling the Bat requires sobriety.

kt5000 - 15-1-2016 at 16:48

Towards the end of selling my house, with an offer on the table, I got the itch to test an extraction in my office. A Soxhlet would have been awesome for the task, but I didn't have one and settled for a 250 mL flask on a hot plate with the window open. After heating slowly for maybe 15 minutes, I noticed there was no boiling chip in the flask. I grabbed a couple boiling chips, tossed them in, and WHOOSH--a jet of hot acetone that must have been 5 feet tall (hit the ceiling). If I'd had an open flame, it would have caught fire.

Lesson learned. I've never forgot the boiling chips since.


Atrum - 15-1-2016 at 17:06

Quote: Originally posted by kt5000  
Towards the end of selling my house, with an offer on the table, I got the itch to test an extraction in my office. A Soxhlet would have been awesome for the task, but I didn't have one and settled for a 250 mL flask on a hot plate with the window open. After heating slowly for maybe 15 minutes, I noticed there was no boiling chip in the flask. I grabbed a couple boiling chips, tossed them in, and WHOOSH--a jet of hot acetone that must have been 5 feet tall (hit the ceiling). If I'd had an open flame, it would have caught fire.

Lesson learned. I've never forgot the boiling chips since.



That is certainly one way to learn to always use boiling chips. Glad nothing serious came from that incident.

Atrum - 15-1-2016 at 17:08

Quote: Originally posted by aga  
CaCl2 is wonderful stuff.

Make a LOT of it and keep it dry.


Keeping it dry is the easy part. It is drying it in the first place that always makes me bang my head on a desk.

First time I prepared that stuff it turned into a solid brick. Then by the time I got it crushed up again, it had already become soggy.

The Volatile Chemist - 20-1-2016 at 17:31

Quote: Originally posted by Atrum  
Quote: Originally posted by aga  
CaCl2 is wonderful stuff.

Make a LOT of it and keep it dry.


Keeping it dry is the easy part. It is drying it in the first place that always makes me bang my head on a desk.

First time I prepared that stuff it turned into a solid brick. Then by the time I got it crushed up again, it had already become soggy.

Hammer time? :)

In regards to boiling chips, I've found that adding some of the solid reagent being used to the solution works to start up boiling as long as it is added before starting.

j_sum1 - 12-4-2016 at 21:09

I think this qualifies for this thread.

Today I learned yet again that glass at 300C looks exactly the same as cold glassware.
I picked up a flask and have some decent blisters on finger and thumb. (Typing is interesting.) happened at work so all costs are covered. It could be a bit painful and annoying for a few days.



2016-04-13 15.05.10.jpg - 1.1MB

JJay - 12-4-2016 at 21:25

It doesn't look that much different at 800C either... I've picked up red-hot glass with only minimal hardening of the skin on my fingertips. How did you get such serious burns?

j_sum1 - 12-4-2016 at 22:48

A bit of pressure nakes a difference as well as a decent contact area. 300C is just a guess. It had been in a Bunsen flame.

First aid office was rather thorough and enthusiastic. There are blisters but I think it will amount to nothing after a couple of days. The dressing means I can't bend my fingers though.

Loptr - 13-4-2016 at 00:16

Quote: Originally posted by j_sum1  

Today I learned yet again that glass at 300C looks exactly the same as cold glassware.


I don't know about 300C, but as glass gets towards the top end of my hot plate it has a different sheen to it, almost like a flame polish effect.

j_sum1 - 13-4-2016 at 00:31

Yeah. but my problem was that I was distracted talking with someone and not thinking about what I was doing. It could have been purole and I wouldn"t have boticed.
:)

Magpie - 11-7-2016 at 08:51

It's not good to leave your radio on top of your muffle furnace when using the furnace. The radio became a puddle of melted plastic. :( This was removed using acetone and a chisel.

pepe - 14-7-2016 at 16:15

About a week ago I broke my only Erlenmeyer. Granted I set it in a dumb spot and it will be easy to replace but it still sucks to break one of your only pieces of something and have to wait for backups.

Geocachmaster - 14-7-2016 at 17:05

Yes, I had just finished cleaning my largest and only 2L beaker when I dropped it in the sink. It only fell about 10 cm but it didn't survive and broke into many pieces. Very fun! The bigger they are the harder they fall...

RocksInHead - 20-7-2016 at 09:10

Just yesterday broke 2 test tubes by knocking over the rack, then 5 minutes later broke the stem off of a 1000ml seperatory funnel.

mayko - 20-7-2016 at 09:38

The nice thing about gravity funnels is that if you drop one, you get a stemless funnel for crystallization and a few inches of glass tubing!

ps guess what i did yesterday

[Edited on 20-7-2016 by mayko]

MrHomeScientist - 20-7-2016 at 09:53

A few days ago I was the victim of a comical series of events that led to some broken glass. I was carrying a crystallization dish and a beaker back inside after washing them down outside, when I fumbled the wet glass and clanged the two together. Everything seemed fine, so I breathed a sigh of relief and put the beaker down so as to only carry one thing at a time. I took a few steps and fumbled the wet crystallization dish a second time, but caught it right away. Breathing another sigh of relief, I took a few more steps then fumbled it a THIRD time, this time dropping it on the concrete and shattering it into a million pieces.

After cleaning this up and carrying the beaker inside, I discovered that I had also put a huge crack in it from the first fumbling. I need to reevaluate my "one-trip" mentality.

mayko - 30-7-2016 at 09:04

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 :(

Texium - 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.

myristicinaldehyde - 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.

Texium - 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.

myristicinaldehyde - 22-8-2016 at 12:59

And check first if it is a closed system!

Texium - 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.

XeonTheMGPony - 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]

JnPS - 24-8-2016 at 18:17

Another one *DJ Khaled voice*



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ave369 - 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!

Arg0nAddict - 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

Sulaiman - 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

aga - 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.

j_sum1 - 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?

elementcollector1 - 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.

adk - 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.

Cryolite. - 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!

ave369 - 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.

Fidelmios - 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)

Toady - 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.


Brom - 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.

JJay - 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.

RtnDownloadFile.jpg - 252kB

Dr.Bob - 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.

Texium - 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]

aga - 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.

Texium - 28-12-2016 at 14:53

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

aga - 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]

JJay - 28-12-2016 at 17:31

After distilling some water, I noticed that my favorite 3L flask is developing some nasty scratches, some of which are in an ugly pattern that looks like star cracking. I'm not ready to throw the flask away yet, but I'd be a little concerned to put it under vacuum or use it at high temperatures.

Looks like I will need to pick up a new flask pretty soon... I wonder if I should get one with four necks. I could use an overhead stirrer, reflux condenser, addition funnel and thermometer simultaneously that way, but I find that I rarely require such a complex apparatus, and I could probably get away with using a Claisen adapter on one neck....

Db33 - 29-12-2016 at 13:46

First time ive had glassware delivered broken. I think from now on im going to try much harder to find galssware already in the USA instead of having it ordered from China. Because not only does it take about a month, but you could get something like this, which totally bummed me out today when it came. I was really lookin forward to my first pressurized funnel. And now its here and its shit.


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Chemetix - 29-12-2016 at 14:58

I hate to say it, but that's why chinese glass is cheap. I see teaching labs complain about the scratching and star cracks in glassware that otherwise gets nearly 20 years of use.
I find it hard to do repairs because there is a difference in the borosilicate batches that china uses compared to the material from European and American suppliers.
That said there are also differences between modern batches and old stocks of glass that I've had difficulty using; and old, I mean older than 40 years.

Support your local glass blower, the difference in price is buying you a reliable service.

JJay - 29-12-2016 at 16:43

Some Chinese glass is good; some isn't. I have literally knocked pricechopper2011's flasks from a tabletop onto concrete without damage. I have seen American glass implode under vacuum and crack spontaneously for no apparent reason... there are many factors that affect quality....

When I ordered my addition funnel, it arrived broken twice due to shoddy packaging. When I finally received the funnel, though, it was like unwrapping a Ming vase. I am sure it will last a very long time if treated properly.

I imagine I'll go through the same ordeal with my reflux condenser, but I'm also sure I'll end up with one that will last 20 years.

For every item in those American-made sets that have lasted 20 years, how many got smashed when a spatula was dropped placed on top of them in the chemistry drawer or when they were placed on a cold tabletop after heating? Not every microchip ends up in a server, and not every adapter should handle boiling sulfuric acid... I'd bet you could drop kick a lot of ancient Chinese earthenware (or for that matter, 100 year-old china teacups) across the garage without any damage, but for every piece like that, there were hundreds more that have shattered.

China has subsidized shipping policies that I believe provide insurance, so shippers don't necessarily have a financial interest in supplying the best packaging.

[Edited on 30-12-2016 by JJay]

Texium - 29-12-2016 at 21:51

I have wondered if some of the older pieces of glassware that I own have survived for decades of use by natural selection of a sort. Maybe that the flasks that made it to me are more well-annealed and even than their compatriots that broke over the years.

It's an interesting thought, not sure if there's any truth to it though.

JJay - 29-12-2016 at 22:47

Quote: Originally posted by zts16  
I have wondered if some of the older pieces of glassware that I own have survived for decades of use by natural selection of a sort. Maybe that the flasks that made it to me are more well-annealed and even than their compatriots that broke over the years.

It's an interesting thought, not sure if there's any truth to it though.


Well, you could always do a controlled experiment to find out!

bad day

Sulaiman - 28-1-2017 at 09:15

A nice sunny morning, and I finally felt fit enough to distill some EtOH today :)

took almost 2 hours to set up (I'm not that fit yet)

the still ran long enough to get c20ml of distillate from 1.4l in the pot, then it stopped ...

my cheap hoplate melted it's internal thin pvc insulated ac input wires :(

... then it started to rain on my outdoor workspace :mad:



on the brighter side, the heating element for my diy 500ml 250W mantle arrived today :)
... now looking for tin cans .....

Geocachmaster - 28-1-2017 at 09:44

@Sulaiman I bought one of the 250ml liners, but I didn't think about the fact they're meant for 240 Vac... Then my poorly constructed heating mantle (not much insulation) meant only 20 out of the 65 watts made it into the flask. Not to mention the major electricution hazard from my poor wiring.:D

Sulaiman - 28-1-2017 at 10:18

IF you can find a mains transformer of required VA (i.e. 250 VA in this case)
that has dual 110 Vac primaries, you can use it as step=up transformer,
a 110:110 Vac isolation transformer of half of required VA also works.

Geocachmaster - 28-1-2017 at 10:34

That's what I was thinking but unfortunately I don't have the right transformer, it's back to the oil bath for now:)

tsathoggua1 - 28-1-2017 at 12:11

Last time I ordered glass from china, give or take a couple, 100 pieces or thereabout, every last bit arrived wrapped and packaged perfectly, even surrounding the condensers in blocks of something tougher than styrofoam but of a similar foamed plastic nature over the coolant inlet/outlets. Entire lot all packed up individually, and the dead-space in the crate filled with soft packing. Not a scratch on any of it. Only thing not to survive was a 100ml 2-necked flask, and that was my own fault, after having used it and dropping the damned thing. Empty at the time, thankfully.

beginner experience

Db33 - 1-2-2017 at 10:05

So i recently sent a bit of Propionyl Chloride to another member here. I have a bottle of this stuff and am saving it for something particular so i hadnt really dealt with it yet. I have never dealt with this chemical but i did have a tiny bottle of Acetic Anhydride once that i was told was kind of similar. So all i did was, i took the bottle of prop chloride and poured it into a graduated cylinder to measure it. Within seconds i couldnt even breathe and my eyes were hurting cuz of how strong this stuff is. It fumes a little and is extremely pungent. I thought it would be bad like dealing with hydrogen chloride but i think this was worse. IT was just really strong. Thats the last time i do that without a respirator and goggles.

MrHomeScientist - 1-2-2017 at 10:25

I had a similar experience when I bought tetralin without thoroughly researching it beforehand. Wasn't aware it had such a strong, nauseating (to me) smell. Transferring it from the jug it shipped in to several glass bottles was not a fun experience.

JJay - 1-2-2017 at 17:51

Ever open a bottle of bromine? :D

NedsHead - 28-2-2017 at 03:39

I had a close call with some nitrocellulose I was storing in my gun safe, I placed it in the ammunition compartment a long time ago and forgot about it.

it's summer here and the part of the house where I keep my safe gets quite warm and fluctuates a bit which sped up the breakdown of the guncotton (it was neutralised and washed thoroughly before storage)

When I opened the ammo compartment to grab some primers I immediately smelled NO2 and saw a layer of rust on the latch (PANIC!)

Luckily, it doesn't look like my rifles were attacked but I'll give them a good clean and oil tonight anyway, just to be sure.

Below are some pics of the offending guncotton, the jar lid that the NO2 ate through and the damaged latch and primers.

Only powders, primers and ammo will be stored with the firearms from now on.

DSC_3227.jpg - 1.9MB DSC_3226.jpg - 2.7MB

DSC_3219.jpg - 1.6MB DSC_3232.jpg - 2.6MB

DSC_3233.jpg - 2.3MB

mr.crow - 17-3-2017 at 16:12

Not lab related but certainly a bad day and chemical related. I recently moved into a new place and the previous owner had apparently spilled a whole jug of laundry detergent under the washer and dryer. I literally had to scrape lint, dust and pube encrusted soap off the floor with a chisel. Today my fingers are super dry and sting like crazy. Not fun.

Σldritch - 23-3-2017 at 13:26

While on my accident streak I had an accidental detonation. I was trying to make nitrite by the reduction of nitrate with sodium sulfide... Again, and it detonated spraying sulfur smelling goop on windows and walls, luckily it did this relativly safely outside so no real damage was done, it didnt even crack the crucible but i think it is time to give up on this synthesis.

Im going to try the electctrolytic oxidation of ammonia instead. :(

mayko - 1-10-2017 at 07:15

I've been doing some experiments with corn syrup and have managed to get it everywhere and all over everything. It doesn't take too much to clean it up, but it has a tendency to cement stuff to the countertop. Most things I've been able to dislodge, but one petri dish was so firmly stuck that it broke rather than come loose. There's still glass glued to the counter top that I haven't been able to get loose :(

Σldritch - 2-10-2017 at 12:13

Im was finally sucessful with the nitrite but i broke my glass thimble placing it in the sink on top of the drain so it fell over...

Here is another one: :(

MrHomeScientist - 13-11-2017 at 09:23

Sort of a cross-post, but I thought it belonged here too.

Last night I was doing an experiment on making boron from boric oxide, by mixing the crushed oxide with Mg powder and heating in a small propane furnace. Just a few minutes into heating, I was poking at it with a graphite rod to try mixing things around. It suddenly reached the activation temperature and I was met with a wooshing sound, a blinding white light, and very hot boron flying out of the furnace. While I was right next to it. The tabletop was scorched in several places and my shirt now has a burn mark on it. Luckily, I was doing this outside and was wearing a face shield and welding gloves. I should have also been wearing my welding jacket, apparently. That really surprised me because the reaction shouldn't produce any gas, so I don't know why it would "explode" like that. Always be prepared for the worst!

The upside is it looks like this method worked beautifully, and I have lots of black B powder drying on the filter paper now. Should make for a fun YouTube video!

The Volatile Chemist - 18-11-2017 at 21:09

Well I guess I don't have too much to complain about, but I dirtied half my glassware for a phenolphthalein synth that failed simply because I neglected to add sulfuric acid. I did get a very little product in solution, which was a nice proof of concept, however, and I also silenced a nagging that I'd had, that sulfuric acid, when used as a catalyst in reactions involving the release of water, could hardly be necessary. So, all in all, not too bad, but I have to prep some phthalic anhydride all the way from di-n-butylphthalate, so it'll be a while before I can retry the experiment.

CharlieA - 19-11-2017 at 18:11

I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D

NEMO-Chemistry - 19-11-2017 at 18:53

Quote: Originally posted by CharlieA  
I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D


You normally get that when the person stops paying for the server. In this case i had a peek at the history and I think it never got passed the under construction stage.


TheNerdyFarmer - 20-11-2017 at 06:09

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.

The Volatile Chemist - 20-11-2017 at 09:23

Quote: Originally posted by NEMO-Chemistry  
Quote: Originally posted by CharlieA  
I attempted to look at your write-ups, but both links gave me an "account suspended" screen. What am I doing wrong? (I will admit in advance to being severely computer-challenged.):D


You normally get that when the person stops paying for the server. In this case i had a peek at the history and I think it never got passed the under construction stage.


Well if you look long enough back you'd find it did indeed have a website there - though you'd need to look at the ptp.x10.mx link for that. I just use it as a placeholder for the moment, until I have something to actually put there. These days I don't really do big writeups. But when I make some progress on a PDF of amateur-accessible syntheses and the characterization of compounds, I'll put it up there along with the indices.

Ironically, when you checked, the website had just gone suspended. It should be unsuspended now (free host, just have to make sure I log in monthly).

[Edited on 11-20-2017 by The Volatile Chemist]

Vosoryx - 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.

Lab without heating mantle

KiWiki - 2-12-2017 at 14:40

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... :(

CRUSTY - 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.

Geocachmaster - 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!

JJay - 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.

WangleSpong5000 - 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]

NEMO-Chemistry - 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....

WangleSpong5000 - 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]

NEMO-Chemistry - 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.

WangleSpong5000 - 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]

NedsHead - 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

WangleSpong5000 - 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.

nitro-genes - 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. :)

WangleSpong5000 - 28-12-2017 at 08:43

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

nitro-genes - 28-12-2017 at 08:56

Wasn't sure which would be grinding which either, it put up a descent fight though.

j_sum1 - 9-3-2018 at 20:06

"Tink"

The noise no one wants to hear.

IMG20180310135423.jpg - 774kB

Mabus - 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.

JJay - 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.

Mabus - 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.

AvBaeyer - 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.

AvB

DrScrabs - 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.

mayko - 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.

j_sum1 - 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.

violet sin - 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.

zed - 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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