Sciencemadness Discussion Board

Bad days in the lab or with glassware?

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peach - 22-1-2011 at 05:11

People who use things like SolidWorks can not only produce the CAD drawings of components, they can build them into huge assemblies, like buildings or aeroplanes, and model each element for it's stress distribution as it goes through different frequencies (looking for natural resonance), loadings and temperatures.

When you see places now that look like something out of SimCity, there's a good chance the entire plan for the railways, services, roads, municipal facilities and residential buildings has been laid out in something like AutoCAD.





[Edited on 22-1-2011 by peach]

Piranha bites

The WiZard is In - 27-1-2011 at 10:48

http://tinyurl.com/4svmllh

and :—


From: rtore00@pop.uky.edu (Professor Robert Toreki)
Newsgroups: sci.chem
Subject: Re: Piranha Solution
Date: 9 Apr 1997 14:00:06 GMT

In article <334A4298.C1C@lanl.gov>
"Rebecca M. Chamberlin" <rlmiller@lanl.gov> writes:

(snip)

> However, using it in an R&D lab is asking for trouble. A classic lab
> accident with piranha solution occurred at Cornell in 1986 or so. The
> grad students in one lab used to rotate responsibility for cleaning all
> of their glass frits by running piranha solution thru them (using "house
> vacuum") into a filter flask. One student made the mistake of leaving a
> trace of acetone in the flask. When the piranha solution hit the
> acetone, it went BLAMMO and a million pieces of glass embedded
> themselves into her face. Thank heavens she was wearing her safety
> glasses or she would most likely be blind now: the lenses in her safety
> glasses were shattered but still intact in the frames. The chemistry
> department took a photo of the glasses and used it in their "Are you
> wearing your safety glasses?" poster for years afterward. Not
> surprisingly, the student decided to leave chemistry after her
> hospitalization.

As it appears that Becky, I and others have not quite gotten the point
across, let me drive it home one more time. While you can usually tell
a conversation among chemists has gotten lame when they start swapping
lab accident stories, it is important that you **understand** that the
risk of using this solution is nowhere near the reward.

What Becky is writing about is 100% true. I saw it. It happened. It
could just as easily happen to you. Read this and then ask whether a
clean frit is worth this.

I was the first one to get to scene of the above incident. We heard a
sound like an M-80 (about a quarter stick of dynamite) from two labs
away. We got there within about 5 seconds to find her on the floor
halfway across the room surrounded by a large pool of blood. The
filter flask that she was using turned to dust; we never found a
fragment larger than about 2 mm even though it had been wrapped in
heavy black electrical tape. The metal 3 prong clamp that held the
flask sheared off at the point where it was clamped to the latticework
in the hood. A row of glass cabinets along one wall were peppered with
holes from the shrapnel. The lab had one of those 100 mm diameter
glass drainpipes running vertically on the wall opposite the hood
(about 8-10 m away) -- the pipe cracked in the middle ...we believe
that it wasn't from shrapnel, but from the compression wave of the
blast.

The student was wearing rubber gloves, a thick sweater, a lab coat, an
apron and safety glasses at the time of the explosion. The hood was
down part way and saved her from catching most of it in the face. The
arm holding the frit caught most of the damage -- the glove was
completely flayed and her arm had several hundred small bits of glass
in it as well as several fairly large lacerations. She had a wound
about 20 mm in diameter just next to her jugular vein. At least one
piece of glass went through her cheek. She (and everything else) was
also covered with hydrogen peroxide and sulfuric acid; something that
we didn't realize until much later because we had no way of knowing
what had happened. I think the bleeding stopped more because she went
into shock than from the pressure were were applying in two different
places.

She spent the next six hours having tiny bits of glass picked out of
her arm, neck and face. I'm told that you continue to have those work
their way out of your skin for the next several weeks after such an
incident -- that you sweep your good hand across the arm and cut
yourself on the glass sticking out of your own skin. This student had
some nerve/tendon damage and lost a bit of the motion in one or two of
her fingers; I can't recall if she had any hearing loss or not. All
things considered, she got off pretty lucky. And yes, she did leave
the program a short time after.

Now consider this: 10 minutes later and the rest of my research group
would have left for dinner. She was working ALONE in her laboratory,
"just cleaning up". Maybe she could have gotten to the phone on her
own...when I got there she was trying to get up, but not very
successfully. Ever try to stand up in a pool of your own blood and
sulfuric acid on a linoleum floor while dazed and injured? Me neither,
but it certainly didn't look very easy. Think about that the next time
you are working a late night alone.

The odd thing here is that if she hadn't been working alone there would
have been many other injuries in that laboratory. We found one large
chunk of glass imbedded in a bookcase over someone's desk. If the
owner of the desk had been there he would have caught this fragment
with the back of his neck. I can not stress enough how **stupid** it
is to put a desk or glovebox opposite a fume hood (or having a desk in
a lab, but that's not always avoidable). Look around your lab and see
if you have that configuration...it's scary. And the next time you see
someone without their safety glasses on, help them find a pair or make
them leave. It is one thing to be an innocent bystander, it is another
to be a stupid bystander.

BTW, the shattered safety glasses Becky is referring to were from a
separate accident at Cornell involving a vacuum line explosion, but
that's another story and I only know it secondhand. Part of their
rather effective campaign to make you think about safety.

Let me just end with the question I posed at the beginning: Were a
batch of clean frits really worth all this?

Rob


djh
----
…the Extreme Light Infrastructure ELI, designed to be the first
exawatt-class (10x18W) Laser. This gargantuan power will be
obtained by cramming a kilojoule ofo energy into a pulse only 10
fs in duration.

Mourou and Tajima
More Intense, Shorter Pulses
Science 331:41-42. 7I11

[Do to budget constraints – la laser will be use to treat toenail fungus on Weekends.]



[Edited on 27-1-2011 by The WiZard is In]

peach - 27-1-2011 at 14:03

He's right, that is a lame story.

I can guarantee I'd get laughed out of a chemistry department for not knowing my mechanisms off by heart, yet I also rinse things with water, then sulphuric prior to using Piranha.

Quote:
The student was wearing rubber gloves, a thick sweater, a lab coat, an
apron and safety glasses at the time of the explosion. The hood was
down part way and saved her from catching most of it in the face.


Classic 'pile on the safety gear and don't think' methodology at work.

The rubber gloves, apron, lab coat, and fume hood are in no way essential for using it. What they are doing is getting in the way and giving a false sense of security. I've gone as far as making that video of me with it on my hands to demonstrate the point.

If you were to pick one piece of safety gear, it'd be for your eyes - in case it splatters. Forget steamy, tunnel vision, digging in, poor protection goggles, get a face shield instead.

Quote:
you can usually tell
a conversation among chemists has gotten lame when they start swapping
lab accident stories, it is important that you **understand** that the
risk of using this solution is nowhere near the reward.


Erm... using it is perfectly worth the reward. There is not a lot else that will match it.

I notice for someone who doesn't like gore stories, but does want to ram home the risk, he didn't mention why she was using it or how to avoid it doing what it did.

Pulling Piranha straight into a freshly used piece of glass under vacuum is simply unacceptable. It is the absolute worse case example. Okay, if it was boiling it'd be worse, so it's second from the top. For a start, it may have been possible to clean the glass with something less dangerous.

But John! You'll make a mistake and regret it too some day!

Probably! And then I'll feel like a complete idiot. The one thing I'd like out of it wouldn't be people going on about blast radius's, but telling other people how to stop it happening to them; even if that means getting laughed at when I post a photo of me in hospital. I also very much appreciate help from other people, which this does not provide.

This accident would have been avoided if one of the staff (prior to handing them something that'd form high explosives in the glassware), had taken 30s to demonstrate what happens when you suck concentrated sulphuric through a damp frit.

As we see here, despite the mountain of safety gear, she was 'lying on the floor in a pool of blood'. Since she didn't have a full hazmat suit on, it's lucky she wasn't doing anything toxic.

Quote:
And the next time you see
someone without their safety glasses on, help them find a pair or make
them leave. It is one thing to be an innocent bystander, it is another
to be a stupid bystander.


Whoever let the students use it unsupervised should leave. And the person who recommended using it before anything else. And the person who suggested immediately connecting the sintered glass to the vacuum.

And the person going on about goggles rather than pointing these things out.

Something has gone seriously wrong here. Either Becky didn't care, or someone didn't care about her.

----------------------------------------
Cleaning frits

Try solvents and biological detergents first (soaking overnight)

Not working?

Rinse with water, then try sulphuric

Not working?

Try piranha (DO NOT rinse the glass with solvent between the last stage and this, for the above reason)

Alternatives?

Nital / cook the sinter (preferably with oxygen) near 500C / alkaline peroxide (it will start rotting sintered glass) / use a disposable membrane filter instead and save yourself the effort of cleaning glass frit (I am quite surprised more of these aren't used in chemistry)

READ THIS AND THE COMMENTS

Take the points about lab coats and gloves as significantly less than the one about rinsing the funnel first. He's only suggesting using the fume hood to provide a barrier between you and glass, which a plastic shield will do or not standing in the room with it.

Do not do as he suggests and connect it to the vacuum until it's at least fully permeated the frit. Better yet, let it run through once without the vacuum - as someone suggests in the comments.

[Edited on 27-1-2011 by peach]

ScienceHideout - 13-3-2011 at 15:42

Once my friend wanted to see my lab. I sail what the hell and I took him. He asked me what a certain chemical was. It was on my ring stand in a 19/22 quickfit flask with a stopper in it. I said I really need to get it down and put in on a cork ring. I asked him to hold it while I get a ring out. A few seconds later I turned to the sound of broken glass. He had an Oh, **** look on his face and the stopper in one hand, while my reagent was eating away the floor. I quickly turned and grabbed baking soda and poured it all over.

It was the corrosive dragendorff reagent.

From that point on NO ONE but me was allowed in my lab.

cyanureeves - 13-3-2011 at 17:20

today i was making sodium nitrate with cold packs and bubbling the ammonia into distilled water.it was doing great until it just stopped bubbling even though it was boiling,so i lifted the tube out of the water and some of it got sucked back into the sodium hydroxide/ cold pack mix. i got weak ammonium hydroxide now, my favorite ammonia generator (round pyrex coffee pot with narrow neck)in pieces,a smelly tool shed and no sodium nitrate.i'm going back to my old way of making ammonium hydroxide by capping a coffee pot with an inverted plastic container with a hole in the cap and a piece of 2" p.v.c. tube in it a just collect the condensate. i loved that pot!

plante1999 - 13-3-2011 at 17:46

Quote: Originally posted by ScienceHideout  
Once my friend wanted to see my lab. I sail what the hell and I took him. He asked me what a certain chemical was. It was on my ring stand in a 19/22 quickfit flask with a stopper in it. I said I really need to get it down and put in on a cork ring. I asked him to hold it while I get a ring out. A few seconds later I turned to the sound of broken glass. He had an Oh, **** look on his face and the stopper in one hand, while my reagent was eating away the floor. I quickly turned and grabbed baking soda and poured it all over.

It was the corrosive dragendorff reagent.

From that point on NO ONE but me was allowed in my lab.



you'd need a friend who shares the same passion as you. I'm lucky I have one, in some of my video on my youtube channel I have three arms .... my friend take very care of my stuf and my glassware , probably more than my.


[Edited on 14-3-2011 by plante1999]

[Edited on 14-3-2011 by plante1999]

redox - 28-3-2011 at 15:12

I had a beaker full of boiling conc. acetic acid. There was a small crack I noticed previously (but ignored), which, of course, shattered as it was heating and spilled the acid EVERYWHERE. My basement smelled like hell's vinegar for weeks.

The WiZard is In - 28-3-2011 at 17:50

Quote: Originally posted by redox  
I had a beaker full of boiling conc. acetic acid. There was a small crack I noticed previously (but ignored), which, of course, shattered as it was heating and spilled the acid EVERYWHERE. My basement smelled like hell's vinegar for weeks.

I remember a bunch and a half years ago decided to make
sauerbraten. The Joy of Cooking sez — Heat but do not boil:

Equal parts of mild vinegar and water
1/2 cup sliced onion
2 bay leaves
1/4 cup sugar

Pour this mixture while hot over the beef....

I didn't have a pot large enough to hold the eye round
so I used a plastic bag... whose seams lasted all of 3-seconds
before seperating... my kitchen smell like a deli for two weeks.

And byda --- when cleaning squid ... don't squeeze them or
you will end up with ink all over the kitchen.

Now back to science .... I would note in passing :—

Harold McGee
On Food and Cooking : The Science and Lore of the Kitchen
Simon & Schuster 1984
684 Pages



djh
----

Rötgen's [William Conrad] parents were
greatly concerned about their future
daughter-in-law. [Swiss -Bertha Ludwig]
They had seen that she was an intelligent
girl and had a good education, but they also
recognized that she was not fully prepared
to enter matrimony. Her faults, however,
could quickly be corrected, and so it was
mutually decided that Bertha should go to
Apeldoorn to learn not only the rudiments
of a German household but also how to cook
certain German and Dutch style dishes that
their son especially liked.

W Robert Nitske
The Life of Wilhelm Conrad Röntgen : Discovery of the X Ray
U of Arizona Press 1971



[Edited on 29-3-2011 by The WiZard is In]

[Edited on 29-3-2011 by The WiZard is In]

redox - 30-3-2011 at 17:07

Did you test the chemical properties of the squid ink, by any chance?

Mixell - 8-5-2011 at 14:35

Just broke my LAST beaker (the fifth one), good that they are quite cheap, although that means that I'll need to visit the glassware store again...

Jor - 8-5-2011 at 14:56

I hardly every break glassware. In my 4 years of amateur chemistry, I broke 1 erlenmeyer, about 4 beakers and a vacuum allonge. But even then, when you break something it really sucks. Beakers would not be much of a problem as they are cheap but i would hate to break 3-necks, condensors, and such glasware.

Arthur Dent - 9-5-2011 at 04:30

Yeah, it's been a while since I broke something. Occasionally, I break test tubes but these are so inexpensive that it doesn't count. I have broken a nice 500 ml beaker by dropping a tiny piece of metallic lithium in water and not stirring. The tiny piece bubbled and melted until it reached the side of the beaker and spontaneously caught fire, instantly cracking the whole beaker and melting a hole right through the glass!

Right now I have a beautiful Friedrich condenser that has a 1/2 inch crack on the water intake port, I have no idea how and if it can be repaired so right now, it's just a decoration.

I have thrown away a nice 250 ml boiling flask because I noticed there was a chip of glass 5x5 mm missing at the bottom INSIDE the vessel! :o Must be that it was heated too strongly or something...

Robert

#maverick# - 9-5-2011 at 12:45

i broke my only 3 necked RBF and a Erlenmeyer with the little vaccum port on the side in the last 2 weeks, both in careless ways i was pissed

nezza - 10-5-2011 at 08:53

Many year ago when I was at school I found out how to make nitrogen tri-iodide so I had a go at it. Made a small amount at home and left the filter paper to dry overnight on a saucer. Next morning I poked it with a stick to see if it was dry. It was and blew up in my face. It smashed the saucer to pieces and I was lucky that the only injury I got was a speck of iodine in my eye which stung like hell.

I also blew up some potassium permanganate and red phosphorus in a pestle and mortar around the same time when I
a. could get hold of the reagents easily
b. Didn't know just how dangerous this could be
Fortunately it was a very small (well under 1 gram) amount so it just went bang and didnt break anything.

So a bit of luck is always helpful with chemistry.

#maverick# - 10-5-2011 at 12:38

Quote: Originally posted by nezza  
Many year ago when I was at school I found out how to make nitrogen tri-iodide so I had a go at it. Made a small amount at home and left the filter paper to dry overnight on a saucer. Next morning I poked it with a stick to see if it was dry. It was and blew up in my face. It smashed the saucer to pieces and I was lucky that the only injury I got was a speck of iodine in my eye which stung like hell.

I also blew up some potassium permanganate and red phosphorus in a pestle and mortar around the same time when I
a. could get hold of the reagents easily
b. Didn't know just how dangerous this could be
Fortunately it was a very small (well under 1 gram) amount so it just went bang and didnt break anything.

So a bit of luck is always helpful with chemistry.

djust a bit of luck is an understatement, about 2 or 3 years back i read the anarchists cook book and made tiiodide before i knew anyrthing about chem and how sensitive the compound is, it went boom right in my face thank good i had goggles, gloves and a small amount, i was scared shitless:(

redox - 13-5-2011 at 18:16

About a week ago I bought a 10 mL volumetric flask (more as a joke) on the cheap. Three days after I got it, it fell and shattered. $4 wasted dollars. :(

#maverick# - 14-5-2011 at 20:03

Quote: Originally posted by redox  
About a week ago I bought a 10 mL volumetric flask (more as a joke) on the cheap. Three days after I got it, it fell and shattered. $4 wasted dollars. :(


May your flask and my flask rest in peace in heavens meth lab :D

Magpie - 15-5-2011 at 13:29

Today I had to change out a 4' (1.3m) fluorescent light bulb for the lab. I assumed it would have to be broken before placing in the garbage can. Never having done this before and not stopping to realize that it was under vacuum I gave it a whack near one end with a pair of channel locks. Luckily I was wearing leather gloves and had my lab goggles on as there was a violent implosion with glass flying everywhere and a white powder shooting out the open end, pointed away from me. Checking with my son, who has broken many such bulbs at his business, he said that he places them in a garbage bag before breaking. He just assumed that I knew that so hadn't mention it beforehand.

Bot0nist - 18-5-2011 at 05:19

Late last night I was setting up to run a 10g synthesis of TNP, a reaction I have done many times safely. I had an oil bath set up on my table on a towel and it was heating up to 85c. While the bath was warming I was diluting my 98% H<sub>2</sub>SO<sub>4</sub> to 40ml of 92%. During the dilution I somehow pulled the cord to my oil bath and the liter of warm oil hit the floor. Let me tell you that a liter on the linoleum look like the gulf oil spill, so I rushed to get towels.

While I was sopping up the oil I noticed an acrid burning smell and then noticed that the 30 or so milliliters of the warm H<sub>2</sub>SO<sub>4</sub> had spilt onto the towel on top of the table. What was left by the time I noticed was a pile of smoking black carbon. After neutralizing and cleaning up the mess I was left with an ugly blemish on my table the size of a dinner plate. Good times!

Bromine

The WiZard is In - 26-5-2011 at 10:37

FOUR INJURED IN OHIO UNIVERSITY CHEMICAL BLAST
400 Students Routed by Bromine Fumes.
Chicago Daily Tribune (1923-1963) - Chicago, Ill.
Date: Feb 11, 1931
Start Page: 16
Pages: 1
Text Word Count: 405
Abstract (Document Summary)

[Special.]--An instructor was seriously burned, two graduate
assistants and a co-ed overcome, and more than 400 students
routed from the chemistry building at Ohio State university today
when a five pound bottle of liquid bromine exploded, when it fell.

---
Amazing how many thing explode.

Exploding bromine too!

The WiZard is In - 26-5-2011 at 16:01

From the NY Times

Attachment: Chem Bromine Ohio NYT.pdf (16kB)
This file has been downloaded 549 times


plante1999 - 26-5-2011 at 16:12

so... bromine can explode , I have dificulty to see how it can explode , it dont have instable bonds....

[Edited on 27-5-2011 by plante1999]

That Devil Bromine - redux

The WiZard is In - 26-5-2011 at 16:16

From the NY Times

Attachment: Chem Bromine Brookhaven.pdf (54kB)
This file has been downloaded 556 times

Attachment: Chem Bromine Woman chemist.pdf (20kB)
This file has been downloaded 574 times

Mailinmypocket - 31-5-2011 at 15:41

I have been unpacking my chemistry equipment while getting back into the hobby lately, last night out came my box of "nicer more specialized" glassware...first thing that goes flying on the floor is my nice 100 ml weighing bottle with ground glass stopper and all... Thouroughly insulted... I dropped what i was doing and decided to browse Sciencemadness while having a beer lol ... I guess it could have been a condenser or a retort... but....still :( it was my only one.

dish.jpg - 21kB

redox - 6-6-2011 at 03:19

Yesterday my really nice (and expensive) 14/20 200 mm vigreux column hooked on my lab coat as I stood up, one end of the column rose about an inch, and fell back to the table, breaking. :mad:

Arthur Dent - 6-6-2011 at 04:31

Outch. a vigreux is always a painful sight to see shattered...

An odd breakage happened this weekend as I was heating a solution of copper sulphate in a beaker. I usually put a sheet of aluminum paper over the element of my outdoors electric heater. As the solution was boiling gently, it suddenly overheated and upon cooling, I noticed that some of the aluminum paper had become stuck on the bottom of the beaker, after washing thoroughly the beaker, and dipping it in cleaning solution to remove the aluminum stains, there were several small cross-shaped cracks where the beaker had contacted the aluminum-covered element. Sigh.

So no more direct contact with glassware anymore, from now on, sand-bath all the way.

Almost had another breakage, I have this nice 600 ml widemouth erlenmeyer that rolled off my table and landed loudly on my hardwood floor. Didn't break! Phew. I inspected it for cracks and it appears to be ok. I use that flask for my gold-dissolving experiments, because you can easily drop a Pentium broken in half in it.

Robert

bob800 - 6-6-2011 at 12:33

Quote: Originally posted by Arthur Dent  
So no more direct contact with glassware anymore, from now on, sand-bath all the way.


If you're simply heating a beaker, you can just use a piece of wire gauze. I use them to heat beakers over flames, and I've never had a breakage!

Magpie - 10-6-2011 at 12:27

Today I was in the middle of a synthesis of SO3 from NaHSO4. I don't turn the hood fan until T=550C. I was just about ready to do that when I looked out the window. Who did I see but the neighbor's son who occasionally visits for a day of chores on Fridays. This caused me to shut down this day-long synthesis. Said son is a millwright and would instantly recognize the sound of my blower. He knows me and would very possibly start asking questions. I have to chalk this one up to "failure to adequately plan." But looking on the positive side, I did see him in time to take corrective action.

LanthanumK - 10-6-2011 at 12:50

Some gunk from a chemical cold pack crystallized in the bottom of my only beaker. It was moderately hard but was still like an extremely viscous liquid. I was starting to pry it up with my knife when I punched a little hole in the bottom of the beaker. :mad: I also burnt sulfur and ascorbic acid in separate test tubes and tried to scrape them out--same result as above.

redox - 21-6-2011 at 18:14

Quote: Originally posted by LanthanumK  
I was starting to pry it up with my knife when I punched a little hole in the bottom of the beaker. :mad:


I do this also! I lightly dropped a metal spatula into a 25 mL graduated cylinder, and it just fell right through the cylinder. :(
Granted, it was a very cheap cylinder, it was my only one of that size.

A bucket of sand .. my Kingdom for a bucket of sand!

The WiZard is In - 22-6-2011 at 06:22

Found on the depths of my hard drive.

From: herodotus <paiuteNOpaSPAM@my-deja.com.invalid>
Subject: Anecdote from 1st year grad school
Date: Monday, June 05, 2000 9:49 AM

Down the hall, outside the undergraduate lab was a 5 gallon drum
of sand, the D-type fire extinguisher for quenching metal fires
and such. It had apparently never been needed and was covered
with a scattering of butts and papers. One humid summer day we
decide to clean out our THF still. The 5L pot was about a
third-full of the whitish-blue crust of sodium benzophenone ketyl
debris entraining God knows how much unreacted sodium. We remove
the THF in a hood and carefully begin to quench the residue with
alcohol. Sure as shit, it bursts into flames pretty soon as we
get bored with being cautious and pour the alcohol in too
quickly. I am prepared. I hose the pot down with a CO2
extinguisher and put the fire out. We relax. But then I notice
that the CO2 has cooled down the flask, and it is condensing
quite a bit of moisture from the room air. It builds up and
trickles down into the pot. FOOM! I hose it down again and the
fire goes out. But the glass is cold again. FOOM! I realize that
this cycle will repeat until I run out of CO2, so I scream at a
labmate to run down the hall and grab the bucket of sand. I go to
the door in time to see him carrying the bucket back with great
difficulty. It turns out to weigh close to a hundred pounds, and
he is a skinny guy. He manages to drag and hump the thing into
our lab with his adrenaline-enhanced strength. He puts it down by
the hood, and I plunge my hand in to gather up some sand, as the
flask has just FOOMed! again. Crack! My fingers bend back
unnaturally. The contents of the bucket have seized up over time
into an inpenetrable mass, the sand cemented together by years of
spit, dregs of sodas, and other things I do not want to know
about. We can't dig enough sand from the bucket to put atop a
silica gel column, let alone put out a fire. By now we know that
fate is against us, so we let the flask burn for a while. The
fire is small. Eventually we scrounge up a real D-type from
another lab and smother the thing.

As we later realized, this is the type of valuable educational
experience we would never have gotten at Harvard.


djh
----
The people of those foreign countries are very,
very ignorant. They looked curiously at the costumes
we had brought from the wilds of America. They
observed that we talked loudly at table sometimes.
They noticed that we looked out for expenses and
got what we conveniently could out of a Franc, and
wondered where in the mischief we came from. In
Paris they simply opened their eyes and stared
when we spoke to them in French! We never did
succeed in making them understand their own
language.

Mark Twain
20 November 1867


[Edited on 22-6-2011 by The WiZard is In]

Sand or kitty litter?

Arthur Dent - 22-6-2011 at 08:02

Quote: Originally posted by The WiZard is In  
The contents of the bucket have seized up over time
into an inpenetrable mass, the sand cemented together ...


I had a bag of sand for emergencies, which is kept outside in my shed. but I realized that moist, heavy sand is much less efficient and easy to manipulate than clean, free-flowing dry sand, so I bought several 2l plastic containers with a hermetic lid and I filled them with sand that I thoroughly washed and dried in the oven.

I also keep similar containers filled with cat litter, if I ever have an emergency, i'll probably see very quickly which product is more efficient/less reactive in case of a tenacious fire.

Robert

Performic acid

The WiZard is In - 1-7-2011 at 08:47

Chem. Eng. News, 1952, 30 (29), p 3041
DOI: 10.1021/cen-v030n029.p3041
Publication Date: July 21, 1952

Abstract

Chemist Loses Hand in Performic Acid Explosion

Five milliliters of performic acid exploded recently at Laval
University, Quebec, Canada, tearing off the right hand of a
graduate student and smashing all glassware in a radius of two
to three feet. Numerous glass slivers were driven into his skin
and into one of his eyes.

According to information from the student, A. Weingartshofer-
Olmos, and Paul A. Giguère, professor of physical chemistry at
Laval, a small receiving flask containing the 5 ml. of
approximately 90% performic acid was being removed from the
still when it detonated for no apparent reason. The acid had
been prepared by the addition of 25 grams of 99% hydrogen
peroxide to 20 grams of 99% formic acid in the presence of 6.5
grams of concentrated sulfuric acid as catalyst. After two hours
for reaching equilibrium, the mixture was distilled under
reduced pressure (5 to 10 mm. Hg) at 30° to 35° ... [$$$$]


----
Unless perfomic acid has a phenomenal density - 5ml ain't much
weight. A lesson for the assorted fools here who dismiss all
safety information on primary explosives.



Arthur Dent - 1-7-2011 at 09:24

Quote: Originally posted by The WiZard is In  
Unless perfomic acid has a phenomenal density...


One could say that it "performs" admirably well as an explosive...
...podom bom...

As for defunct glassware, my favorite "drying dish" (a 10x10" Pyrex baking dish) literally split in half because of a dumb mistake of mine. I was gently heating some solution to dessicate it and instead of leaving the dish on the heater element, I put it on the concrete floor of the balcony to cool down. The temperature difference was too great and it just went "klink... KLANK!!!" and was effectively split into two perfect halves. Thankfully, there wasn't any liquid left, just a dry salt. Oh well, I paid $1 for it at a thrift shop... ;)

Robert

[Edited on 1-7-2011 by Arthur Dent]

barley81 - 1-7-2011 at 10:30

I discovered that my first erlenmeyer flask ever from four years ago has a 5mm crack! Must have been from the time where I put dry ice and ethanol in it... Oh well, it was only $4 and I have others now.

Lambda-Eyde - 6-7-2011 at 12:24

This has been such a shitty day for chemistry. The week started out nicely with a trouble-free nitrobenzene synthesis. But today wouldn't turn out to be that nice. First I cough my ass of trying to transfer 15 ml of bromine to an addition funnel. Then I break my only 50 ml measuring cylinder. :(

Then, while doing a bromobenzene synthesis, I first realize that I haven't greased the joints: bromine vapour and HBr leaks all over the place, and I have to evacuate the lab and let the fan do its job for a while. Then, after sealing it up and making sure all the joints are actually in place (there was a relatively large gap between the liebig and three-neck adapter) everything proceeds nicely...Until I leave the setup for ten minutes (tops). When I return the liquid in the round bottom flask appears to be refluxing vigorously. "Hm. Vogel says the solution needs to be warmed. Makes no sense that it's refluxing from the reaction heat then?" Turns out it wasnt - the liquid from the HBr absorber had sucked back and poured through the condenser, ruining my reaction! :( I did put in a checkvalve, but I didn't realize at the time that it wouldn't react to such a slow sucking (sometimes I'm so stupid and short-sighted I amaze even myself). Then, while sealing the apparatus up, I break one of my three yellow NS14 keck clips to top it all off... So, summary: wasted a bit of bromine and benzene (my two most valued reagents), got a bad cough and broke a keck clip. At least I got some invaluable experience.


TO DO-LIST:

* Build a fumehood efficient enough to safely boil a liter of cyanogen bromide in it
* Buy a coiled or double surface condenser, a 200 mm 19/26 liebig just isn't suitable for anything involving bromine
* Buy some washbottles
* Buy sodium thiosulfate
* Buy some metal keck clips for use with high temperatures and hydrogen halides
* Hang up a poster in my lab saying "GREASE ALL JOINTS / ADD BOILING CHIPS / PREVENT SUCK-BACK" or something along those lines.


Now I'm just looking forward to monday, when I will pick up some exclusive glassware at the glassblower. Can't wait! :)

Retard-3000 - 9-7-2011 at 00:56

Yesterday i was trying to make a concentrated ammonia solution by bubbling ammonia gas through water. I did this using a simple setup that consisted of a stoppered 100ml flask that had pvc tubing leading into cold water. I used ammonium chloride and sodium hydroxide to produce the ammonia, about 2 minutes into the reaction the water that i was passing the ammonia gas through got sucked back into the flask containing the NaOH and NH4Cl :o, at this point i knew something was going to go wrong so i ran out the room slamming the door behind me when all of a sudden . . . BANG!, the rubber bung gets blown off the flask and sodium hydroxide and ammonium chloride went everywhere, not to mention the amount of ammonia gas that was flooding my room, cleanup took at least 2 hours :(. At least next time i know not to do this experiment inside and to use another flask to lead the ammonia gas into the water so that incase another suckback does occur it won't get out of hand again!

Also does anyone know why this suckback occured ? I was thinking maybe due to the dissociation of sodium hydroxide being exothermic it heated the air/nh3 inside the flask and when it cooled down a little a partial vacuum was created ?

barley81 - 9-7-2011 at 03:55

Well, next time you do this, you should:
Not be doing it in your room.
Use a suckback trap.

Ammonia gas is very soluble in water. See this experiment, the ammonia fountain:
http://www.youtube.com/watch?v=sLpITPAqdUI&feature=relat...

cyanureeves - 9-7-2011 at 05:18

i always thought it was caused by absence of oxygen and the void tries to grab it from the atmosphere but its probably the other way around. the oxygen tries to go into the void or maybe i am about to learn something new about this occurence that broke my favorite vessel. at the moment i am waiting on the gentlemen going back and forth on the ammonia and aluminum thread to come up with something concrete because i want to make an ammonia generator using an aluminum joggers bottle and i dont want to blow up. i can sacrify aluminum but glass is priceless almost.i dont want to waste my hydroxide so i am using baking soda and ammonium nitrate and heat. oh! you already know about the oxygen thing and you want to know how it happens.

[Edited on 9-7-2011 by cyanureeves]

Mixell - 9-7-2011 at 05:30

Its not about a specific element, its the pressure of the gas (or gas mixture) that determines if the vessel will explode or implode.
The air around us puts a very strong pressure on every object, the only thing that keeps objects, say glass, from imploding is the inner force applied by the pressure. For instance an erlenmeyer got the same mix of gases inside and outside of the vessel, but when you close it, and some reaction that produces heat/gases occurs, the inner pressure grows and can apply enough force that the vessel will explode (overcoming the force applied by the outer pressure and the glass strength). If the reaction takes up heat or uses gases from the air (without releasing any other gases) then the inner pressure and the strength (molecular bonds) of the glass may not be enough to equal to the force applied by the outer pressure and the vessel will implode.

Boy Hurt In Chemical Blast .Packed Rocket Pipe Lets Go

The WiZard is In - 4-8-2011 at 13:44

http://tinyurl.com/3cgzenv

Later we will make an even stronger [rocket] fuel....!

The WiZard is In - 5-8-2011 at 06:30

Darwin never sleeps.

Teacher Killed In Explosion Of Pipe Rocket .‎

Ocala Star-Banner - Dec 5, 1957
FLOYDADA, Tex. A rocket made from a piece of pipe blew up during a school ...
a member of the class who was only a few feet from the explosion but escaped ...

http://tinyurl.com/4x83o86

If the teacher previously worked at an AEC Research Center I assume he swept its floors.

Several more reports from Google.com/news
http://tinyurl.com/4xv4vpm


[Edited on 5-8-2011 by The WiZard is In]

quicksilver - 5-8-2011 at 08:24

Personally speaking - I would like to thank W.I.N. for his posts and offer a small bit of history to clarify my thinking.

I have been reading material for this gentleman for quite a bit over a decade now. He had been posting some difficult to procure items [to find] back in the days of UseNet (news groups) well back into the 1990's. Some of the material was extremely difficult to find back then.
We face a situation where our collective interests are being restricted in a variety of ways. As tragedies from disturbed individuals result in a knee-jerk fear reaction from the public. More and more of this information will become much more difficult to obtain. Even well back before these horrors, were perpetrated on the public, the difficulty in finding some of this material was obvious to hobbyists and interested persons. Often it had been remarked that his sourcing was of great value as some of the material simply became frozen out of university libraries as well as the US Library of Congress (for common reading).

One of the the MOST valuable items in any collective interest or hobby is the knowledge regarding it's idiosyncrasies. Without it, there is limited means to move forward no matter what level of expertise weighs in the individual's background. The amount of background material available had been uncommon & with more and more politics entering this subject simply the pursuit of background material, it will become much more rare in it's availability.

Very realistically; we may not have another chance at some of this. The Governments of some nations have almost (& in some cases, fully) restricted certain books and papers. Some many years back the Government Printing Office of the US was the method to obtain the full hard-bound PATR. This is no longer so. In fact I could list several sources which have totally dried up. The collections of Urbanski and Federoff (when available) sell for $250 per individual copy, with collections (depending upon condition) meeting rare book prices.

SEVERAL individuals have made available scanned copies of various publications & I would like to thank them all as they preserve an aspect of knowledge that may be eliminated in the not too distant future!
This is not simply opinion. Collecting material on various aspect of subjects such as energetic chemistry has entered the "rare book" arena; check for yourselves on titles that are not part of modern industrial usage. You may be very surprised. Please keep an open mind. Contributions to a knowledge base should be appreciated as some may not be available in the future.

watson.fawkes - 5-8-2011 at 08:26

Quote: Originally posted by The WiZard is In  
Teacher Killed In Explosion Of Pipe Rocket .‎
From the article:"when he struck a match to the opening at one end of the rocket".

Well, that explains that.

The WiZard is In - 5-8-2011 at 08:37

Quote: Originally posted by quicksilver  
Personally speaking - I would like to thank W.I.N. for his posts and offer a small bit of history to clarify my thinking.

Very realistically; we may not have another chance at some of this. The Governments of some nations have almost (& in some cases, fully) restricted certain books and papers. Some many years back the Government Printing Office of the US was the method to obtain the full hard-bound PATR. This is no longer so. In fact I could list several sources which have totally dried up. The collections of Urbanski and Federoff (when available) sell for $250 per individual copy, with collections (depending upon condition) meeting rare book prices.


W.I.N. steps to the podium — bows to the applause of the audience.
Notes that PATR-2700 ("Federoff") can be DL's
from www.dtic.mil. Exit's stage left.

Urbanski has been reprinted. however, even these copies
dobe $$$$$!

Hydrogen and Fluorine

The WiZard is In - 7-8-2011 at 11:14

Erying and Kassel(Cf. Ref. 35) describe experiments in which
the reaction between hydrogen and fluorine was inhibited…..
In one experiment, they admitted the hydrogen and then a
quantity of fluorine much larger than usual, but there was a
very violent explosion. The flask was shattered, a towel which
had enclosed the flask was cut into shreds, and a protective
screen made from glass containing wire was cracked in many
places. The experimenters presume that the explosion was
started by sulfur, talc, or other catalytic material from the
rubber tubing of the nitrogen supply line. They point out that
for ½ hour before the explosion, there must had existed a
mixture of hydrogen and fluorine varying in composition
between 100 per cent hydrogen and 100 per cent fluorine
without appreciable reaction.

35. Erying, H. and Kassel, L.
The Homogeneous Reaction Between Hydrogen and Fluorine.
Journal of the American Chemical Society,
55:2796-2797, 1933.

In:—
Accession Number : ADA800192
Title : The Properties of Fluorine, Oxygen Bifluoride, and
Chlorine Trifluoride
Descriptive Note : Memorandum rept.
Corporate Author : CALIFORNIA INST OF TECHNOLOGY PASADENA JET PROPULSION LAB
Personal Author(s) : Doescher, Russell N.
Handle / proxy Url : http://handle.dtic.mil/100.2/ADA800192
Report Date : 06 SEP 1949
Pagination or Media Count : 73
Descriptors : *LIQUID PROPELLANTS, FLUORINE, CHLORINE
TRIFLUORIDE, LUBRICANTS, FLUORINE COMPOUNDS, FUELS
Subject Categories : LIQUID ROCKET PROPELLANTS


djh
----
Todays factoid —

Quartz burns with
a brilliant light in
oxygen bifluoride.



[Edited on 7-8-2011 by The WiZard is In]

smaerd - 10-8-2011 at 09:56

Broke a buchner funnel the other day. I set it down inside of a quart mason jar so it was held up-right and the contents wouldn't spill. It tapped and I mean tapped, the inside of the jar. *clunk* the bottom part is inside the jar and the top remains. Nothing major, but another small impedance.

edit - next time I will use a steel ring extension on a clamp.

[Edited on 10-8-2011 by smaerd]

Arthur Dent - 10-8-2011 at 12:41

Quote: Originally posted by smaerd  
Broke a buchner funnel the other day.


Was it one of them fancy fritted glass ones or the large white ceramic type?

Mine rolled off the table a while ago and the trash basket broke its fall thankfully. Yeah I was lucky because these puppies are expensive!

Robert

Mildronate - 10-8-2011 at 12:52

I broke 2L Beaker :(

smaerd - 10-8-2011 at 13:22

thankfully it was ceramic. It served it's worth, I think I got it for 5$ and it was used probably hundred plus times. Although it is always a let down when something breaks.

Jack in the box

The WiZard is In - 16-8-2011 at 06:23

ARMED SERVICES EXPLOSIVES SAFETY BOARD
Nassif Building
Washington, D. C. 20315
OPERATIONAL INCIDENT REPORT NO, 111
Detonation in "Catch Box"

Description:
As part of a routine safety inspection, a technologist lifted the
lid of a catch box to check the box and contents. While he was lowering
the lid, an explosion occurred in the box, hurling the 38-lb. aluminum
lid (28" x 54" x 1/4") into his face.

It is believed that non-explosive intermediates combined with the
contents (lead salts) of the catch box producing explosive material one
of which was lead azide. The friction of closing the aluminum lid
detonated some of these crystals.

Preventive Measures:
1. Catch boxes will be eliminated from laboratory installations.
2. All chemical wastes will be destroyed chemically before being
ditched.

(REPORTED BY MANUFACTURING CHEMISTS' ASSOCIATION, INC.)
Reference Number of thts Report: 01-111
Duplication of this report is authorized.

MeSynth - 16-8-2011 at 09:57

My first bad day was when I was concentrating sulfuric acid in the back yard in my first set of newly purchased glassware when I heard the door bell ring. I look into the house through the window to see that it was the pest control guy. I freaked out and blew out my bunsen burner, grabbed the flask with a towl, and then grabbed everything else I could see and ran inside the house with it. As I ran into the house I forgot to grab an empty flask that I had out there for some reason and my foot hit it. When it slid away it tipped over and a large portion of the lip broke off and sent a crack down the side. After laying down the stuff I was using inside the house I ran out and grabbed the broken flask and the chunk that broke off. Soon after I shut the door the guy comes around and sprays the house. My first sad moment in chemistry.

redox - 16-8-2011 at 17:34

Quote: Originally posted by MeSynth  
My first bad day was when I was concentrating sulfuric acid in the back yard in my first set of newly purchased glassware when I heard the door bell ring. I look into the house through the window to see that it was the pest control guy. I freaked out and blew out my bunsen burner, grabbed the flask with a towl, and then grabbed everything else I could see and ran inside the house with it. As I ran into the house I forgot to grab an empty flask that I had out there for some reason and my foot hit it. When it slid away it tipped over and a large portion of the lip broke off and sent a crack down the side. After laying down the stuff I was using inside the house I ran out and grabbed the broken flask and the chunk that broke off. Soon after I shut the door the guy comes around and sprays the house. My first sad moment in chemistry.


Ow, it always hurts when glass breaks. :( What kind of flask was it? A cheap erlenmeyer? Or a 3-neck 12 liter RBF?

overload - 16-8-2011 at 22:29

Quote: Originally posted by redox  
Quote: Originally posted by MeSynth  
My first bad day was when I was concentrating sulfuric acid in the back yard in my first set of newly purchased glassware when I heard the door bell ring. I look into the house through the window to see that it was the pest control guy. I freaked out and blew out my bunsen burner, grabbed the flask with a towl, and then grabbed everything else I could see and ran inside the house with it. As I ran into the house I forgot to grab an empty flask that I had out there for some reason and my foot hit it. When it slid away it tipped over and a large portion of the lip broke off and sent a crack down the side. After laying down the stuff I was using inside the house I ran out and grabbed the broken flask and the chunk that broke off. Soon after I shut the door the guy comes around and sprays the house. My first sad moment in chemistry.


Ow, it always hurts when glass breaks. :( What kind of flask was it? A cheap erlenmeyer? Or a 3-neck 12 liter RBF?


lol! like I would have a RB 12 liter 3-neck F just sitting around! XD it was a 500ml erlenmeyer. I was so new that I actually believed that I could fix it with only a propane blow torch.

asilentbob - 18-8-2011 at 03:27

Whenever we broke or chipped any glassware in the lab I did undergraduate research in we would slam it down into the broken glass receptacle... Results in a more densely packed package lol.

Mercury perchlorate

The WiZard is In - 20-8-2011 at 07:58

Pitt grad student burned in chemical explosion
Thursday, August 18, 2011
Pittsburgh Post-Gazette
http://www.post-gazette.com/pg/11230/1168173-53.stm#ixzz1VaI...

A University of Pittsburgh researcher suffered minor burns in
a chemical explosion Wednesday morning at a science building
on campus.

The graduate student, a 30-year-old man, was working in a
room on the 11th floor of the Chevron Science Center when a
beaker containing mercury perchlorate hydrate broke, Pitt
spokesman John Fedele said.

He suffered burns on his face, chest and arms and was taken to
a hospital, where he was in stable condition. The student was
wearing appropriate safety equipment, Mr. Fedele said.

Police and emergency crews evacuated the building on Parkman
Avenue, as is standard procedure in such incidents, Mr. Fedele
said. He was unsure how many people were inside.

A hazardous materials team was also called. The building was
not damaged, and no one else was hurt.

The university is not in session; students are returning to
campus to start classes Monday.


---
Mercury perchlorate? Could be, however, magnesium perchlorate a common desiccating agent seems upon my
mind as more likely.

MeSynth - 20-8-2011 at 11:46

Quote: Originally posted by The WiZard is In  
Pitt grad student burned in chemical explosion
Thursday, August 18, 2011
Pittsburgh Post-Gazette
http://www.post-gazette.com/pg/11230/1168173-53.stm#ixzz1VaI...

A University of Pittsburgh researcher suffered minor burns in
a chemical explosion Wednesday morning at a science building
on campus.

The graduate student, a 30-year-old man, was working in a
room on the 11th floor of the Chevron Science Center when a
beaker containing mercury perchlorate hydrate broke, Pitt
spokesman John Fedele said.

He suffered burns on his face, chest and arms and was taken to
a hospital, where he was in stable condition. The student was
wearing appropriate safety equipment, Mr. Fedele said.

Police and emergency crews evacuated the building on Parkman
Avenue, as is standard procedure in such incidents, Mr. Fedele
said. He was unsure how many people were inside.

A hazardous materials team was also called. The building was
not damaged, and no one else was hurt.

The university is not in session; students are returning to
campus to start classes Monday.


---
Mercury perchlorate? Could be, however, magnesium perchlorate a common desiccating agent seems upon my
mind as more likely.


This happens if your not concentrating on what your doing. Say you take a beaker containing a liquid and are about to pour it into another beaker with another liquid in order to start a reaction. If you begin to pour the liquid while your thoughts are on the reaction and the reaction products instead of on the preplanned act of pouring the beaker you are increasing the chances of you dropping the beaker or catching it on something and spilling some of the contents ect.

Mixell - 26-8-2011 at 07:58

Broke a 1L beaker while cleaning it, and later managed to get a bit of nitric acid into a cut that was made when I was collecting the beaker shards...

Endimion17 - 30-8-2011 at 07:53

Quote: Originally posted by Mixell  
Broke a 1L beaker while cleaning it, and later managed to get a bit of nitric acid into a cut that was made when I was collecting the beaker shards...



HA-HA!

j/k :D I know how painful that is.

Few days ago I was trying to fix a glass stopcock. The plug was stuck. I've tried gently heating, bathing and cooling in oil, creating a temperature difference between the shell and the plug, but nothing helped.
Since nothing helped, I applied force using this thing (I don't know the English term) and a pair of aluminium sheet covered steel pipes with proper diameters, according to the plug and sheet.
At first, I used the temperature difference, too. Froze the stopcock and used force while heating the sheet.
But the damn thing didn't let go so I used plain brute force. Eventually, the sheet partially shattered and some parts fell off. Most of the sheet was still on the plug and was holding so strongly I had trouble removing it with pliers. It was indeed jammed for good. The smell was organic, akin to resin or even tar.
I have no idea what the hell previous owner used to "lubricate" this. Might as well used superglue. :mad:

alway wear clean socks to work - you never know what can happen

The WiZard is In - 30-8-2011 at 11:21

Acid?! I would have thought alkali.

SO: Textbook of Military Medicine



Attachment: Acid foot.pdf (200kB)
This file has been downloaded 477 times

#maverick# - 30-8-2011 at 12:54

what the hell is it with me and breaking volumetric flask broke another one this time a 1 liter one i iz sad

Freezer And Oleum

Damitwhy - 30-8-2011 at 18:23

After many hours of experimental heating of Sodium Pyrosulphate to obtain Sulphur Trioxide and realising product would solidify in the condenser when it was too cool, produced A pretty good result of fuming Sulphuric Acid...

As I'd been at it from 10pm till 9am I made the silly mistake of Glass Stoppering the receiving flask and popping into the Freezer under the fume hood :( awoke that afternoon to evaluate my full nights work only to find the Fuming Sulphuric Acid wouldnt fume any more and its volume had increased...

I've learnt the Freezer is much to damp an enviroment for Oleum :mad:

Bot0nist - 30-8-2011 at 19:14

That sucks man. Did you do a titration before and after storage? Did you lube your glass stopper joint with silicon or H<sub>2</sub>SO<sub>4</sub>? Maybe in a sealed bag with a good desiccant in the freezer would help.

Killer shard

simba - 2-9-2011 at 17:28

So the other day I was gonna do some quick experiment, and was setting up everything to get it started.

I picked up my sep funnel and noticed I forgot the base and clamps to hold it up, but then I was in a hurry and didn't want to go get them, so I just fitted the sep funnel in a hole on my sink and thought it would hold it up well.

After a few seconds...crack. It broke, and a shard flew on my forearm cutting my wrist. Needless to say it was a bloody scene, I quickly wrapped some piece of cloth around my arm to stop the bleeding and ran to my neighbour's house, which is a nurse, and then she took care of me. :)

The only good thing about the story is that I didn't have to go work that week. ;)

resveratrol - 23-9-2011 at 18:05

i remember one time in undergrad organic lab, i had just recrystallized something from toluene I think...I poured the crystallized solution into a bucchner filtration setup (i had let the flask fill up over the course of the lab without dumping it mind you).

I wasn't giving full attention to what I was doing, and the level of solvent in the flask had risen to the level of the gas inlet (where the vacuum pump was connected), so the vacuum pump started sucking up solvent - which would be okay if it weren't for the fact that the excess fluid cache on the side of the pump was taken off (for some reason)....so the unit sprayed solvent ALL over me. luckily it wasn't acidic, and it smelled kind of pleasant.

Chordate - 23-9-2011 at 23:48

I broke TWO 14/20 short path distillation heads with ground glass thermometer joints in the same day last week, they were on the shelf next to each other and I grabbed one, knocked the other off the shelf, instinctively lunged to grab at it and dropped the first one in my hand. They both hit the ground and broke simultaneously. Ouchie.

I decided that it was a bad omen and scrapped all my work that day. It still stings.

bbartlog - 24-9-2011 at 04:44

A chicken broke my 2-neck 2 liter RB flask. Normally I put all the glass back on shelves or in cabinets when I'm done, but in this case I left the empty flask sitting out on a roll of tape (a fairly stable base, absent other factors). But since some of my chickens have started roaming around inside the pole barn that I use for chemistry, this proved unsafe, and one of them apparently knocked it to the floor and broke it.

Arthur Dent - 25-9-2011 at 13:10

Quote: Originally posted by bbartlog  
A chicken broke my 2-neck 2 liter RB flask.


If that would happen to me, there would be some barbecue sauce and cole slaw in the future of that bird. :mad:

Robert

bbartlog - 25-9-2011 at 15:46

Well, the individual perpetrator can't be identified, and I'm not going to roast a flock of fifty laying hens to avenge one broken flask. But they will eventually get sent to the western end of my farm, where they will no longer be able to trouble my lab space.

mr.crow - 17-10-2011 at 10:58

I keep forgetting about those stupid little stirbars and they wind up in the drain >: (

Arthur Dent - 17-10-2011 at 11:07

Well, if the pipes are made out of cast iron, maybe they're still there and you could retrieve them with a magnet tied to a string. But most drain pipes are black PVC, so I guess they're swimming with the fishes... ;)

Robert

Neil - 17-10-2011 at 11:33

Check your drain trap.

mr.crow - 18-10-2011 at 06:54

Fortunately most of the time they get caught in the drain, only one has actually been flushed.

I should get into the habit of using the HDD magnet to hold it in place. Or get a stirbar retriever to take it out first.

UnintentionalChaos - 24-12-2011 at 19:19

Don't ever shake a flask with a stirbar in it...I had a rather large stirbar in a 1L, 4-neck RBF and one good shake while cleaning put it cleanly through the side wall. I almost cried. That was my fanciest flask and one of only 2 1Ls that I owned. I picked up a 3-neck 1L on ebay though, to replace it, so all is okay...just cost me $30.

DJF90 - 25-12-2011 at 14:49

Same thing goes for a sep funnel. Always pour your reaction mix from the flask to the sep funnel through a plastic funnel with a narrow enough aperture to catch the stirbar - result: no breakages upon shaking.

UnintentionalChaos - 26-12-2011 at 11:09

Quote: Originally posted by DJF90  
Same thing goes for a sep funnel. Always pour your reaction mix from the flask to the sep funnel through a plastic funnel with a narrow enough aperture to catch the stirbar - result: no breakages upon shaking.


You can also just use a hard drive magnet to stick the stirbar to the flask wall when you pour.

Magpie - 26-12-2011 at 12:22

make yourself one of these:

http://www.sciencemadness.org/talk/viewthread.php?tid=13156&...

White Yeti - 31-12-2011 at 10:30

Quote: Originally posted by Magpie  
make yourself one of these:

http://www.sciencemadness.org/talk/viewthread.php?tid=13156&...


Link not works...

Magpie - 31-12-2011 at 14:03

Quote: Originally posted by White Yeti  

Link not works...


The link works for me. It takes me to a thread, where upon scrolling up I find my post with the picture of my stir bar retriever. If you still can't find it let me know and I will quote the whole post in response.

White Yeti - 31-12-2011 at 17:37

Quote: Originally posted by Magpie  
The link works for me. It takes me to a thread, where upon scrolling up I find my post with the picture of my stir bar retriever. If you still can't find it let me know and I will quote the whole post in response.


The link still doesn't work (for me at least). It takes me to a default page "the item you have requested cannot be found" type thing.

Lambda-Eyde - 31-12-2011 at 18:05

It works for me. What browser are you using? I'm using Opera v. 11.50.

Magpie - 31-12-2011 at 19:11

Quote: Originally posted by Magpie  
Finding that I often wish I had one of these but am not willing to pay the $20 + postage, I made one of my own. Here's how:

* Buy 2 feet of 0.17"ID polyethylene tubing ($0.34)
* Buy one 3 foot piece of 1/16" steel rod (~$2)
* Buy one 3/16"OD x 1/2" long cylindrical neodymium magnet ($0.27) (Note 1)

1.Heat about 3/4" of one end of an 18" piece of poly tubing in boiling water to soften it, then force fit the magnet into it, leaving about 1/4" of the end of the tube open.
2. Fuse this end of the poly tube by heating it on a stove, working the end to a seal. Try not to overly heat the magnet as it will lose its magnetism if heated to 80C. (Note 2.)
3. Cut the steel rod to fit in the poly tube leaving about 1/2" of the tube end open.
4. Fuse the open end of the poly tube as before.

Notes
1. The economics are hurt here if you have to pay postage on the magnet like I did. This came to about $5.
2. It might be better to buy an undersize magnet, say 1/8"OD instead. That way you could slide the magnet in later after fusing the end to a seal, and wouldn't have to risk heating the magnet. These Nd magnets are tremendously strong.
[Edited on 23-1-2010 by Magpie]


stir bar retriever.JPG - 101kB

White Yeti - 31-12-2011 at 21:23

Quote: Originally posted by Lambda-Eyde  
It works for me. What browser are you using? I'm using Opera v. 11.50.


I'm using Safari version 5.0.5.

White Yeti - 12-2-2012 at 14:23

Speaking about bad days with glassware, I was messing around, minding my own business when this happened:
IMG_0391 downsize.jpg - 119kB
I know soda lime glass crack under the slightest temperatire changes, but I ramped up the heat extremely slowly, bringing the water to a boil in 40 minutes. The whole bottom usually doesn't blow out when I'm this careful, it's the first time.

I guess the glass had some internal stress to begin with, oh well bad luck I guess.

I gotta get me som'o those polarizers next time:)

entropy51 - 12-2-2012 at 15:04

Quote: Originally posted by White Yeti  
Speaking about bad days with glassware, I was messing around, minding my own business when this happened:
That doesn't look like glassware. It looks like a pickle jar. They are not known for their heat resistance.

Arthur Dent - 13-2-2012 at 04:55

Quote: Originally posted by entropy51  
That doesn't look like glassware. It looks like a pickle jar. They are not known for their heat resistance.


Indeed, I use plain old mason jars to store chemicals, mix them or react them if they are only mildly exothermic, but I have stopped using them to heat/boil/react stuff in them if it might be a bit too intense. I have had jars fracture simply because I have removed them off the hotplate or water bath.

It is safer to boil or heat stuff in a proper borosilicate vessel, using mason jars or mayonnaise pots to heat/boil/react stuff is at your own risk, and if the vessel breaks, you lose your chemical you've worked on and run the risk of ruining your heating device at the very least.

Robert

MrHomeScientist - 13-2-2012 at 06:42

The other day I had a small incident in the lab. I performed the gas test for hydrogen on one reaction that was running, which consists of holding a lit splint to the test tube and listening for the pop. After the test, I blew out the splint and went to snuff out the glowing end on a piece of filter paper lieing nearby. I've done this many times without incident, but this particular paper immediately started crackling and burst into flames! I ran it over to the sink to extinguish it, and luckily nothing was damaged. The filter paper had been used earlier to filter nickel hydroxide from a solution containing potassium nitrate, and so had some residue on it. I think the KNO3 was the culprit.

White Yeti - 13-2-2012 at 17:55

Quote: Originally posted by entropy51  
That doesn't look like glassware. It looks like a pickle jar. They are not known for their heat resistance.


Yes, but believe it or not, I tested one of these out one time to find the limits of these jars, and I was able to bring water to a boil (quickly) and sustain a boil for more than 20 minutes without it breaking.

I suppose you can get lucky sometimes. For the record, I never boil anything of considerable value in jam jars. In this case, I was extracting urea from fertiliser. I was boiling about 100mL of water mixed with approximately the same volume of fertiliser and ramped up the heat really REALLY slowly. I've had some instances where the glass gave a warning, cracked but didn't break completely. I was hoping for that, but instead the whole bottom blew off without warning.

Halcyon - 15-2-2012 at 05:02

In my first high-school science class, the teacher made a huge point of how expensive the measuring cylinders were and how careful we had to be. One dude knocked over a 250ml, I turned to point and laugh, and stole his thunder by knocking over a 500ml one.

FML, that day.

neptunium - 15-2-2012 at 14:02

i hate glass and glass hates me back! i was cleaning a round bottom flask after a distillation when this happen...

picture0001.jpg - 44kB picture0002.jpg - 62kB

bad day indeed...

[Edited on 15-2-2012 by neptunium]

White Yeti - 15-2-2012 at 14:22

:o:o:o:o

Hope to God it doesn't get infected.

[Edited on 2-15-2012 by White Yeti]

neptunium - 15-2-2012 at 14:24

this was last year in June ...went to the hospital no infection thanks! i am fine now...but it was a bloody mess

Bot0nist - 26-2-2012 at 19:11

Broke my 14/20 claisen adapter. I blame the Teflon tape I used. I have just read about it's problems with thermal expansion. As soon as the thermometer read >100&deg;C it popped right off.



EDIT;
Damn neptunium, that's nasty.

[Edited on 27-2-2012 by Bot0nist]

Endimion17 - 26-2-2012 at 19:25

Holy crap, neptunium! :O

Any severed nerves? Any cool looking scars? :D
These kinds of photos are actually good to look at - one becomes aware of the dangers of handling glassware. I think we all tend to ignore that fact because glassware is smooth and cool to play with. This is an eye opener for some, a good reminder for others.


Bot0nist, was that one layer of tape or more? Was the tape covering the lower or the upper part of the joint?

[Edited on 27-2-2012 by Endimion17]

Bot0nist - 26-2-2012 at 19:33

Quote: Originally posted by Endimion17  


Bot0nist, was that one layer of tape or more? Was the tape covering the lower or the upper part of the joint?

[Edited on 27-2-2012 by Endimion17]


Only the top <sup>1</sup>/<sub>4</sub> was wrapped. One and a half layers.

AirCowPeaCock - 26-2-2012 at 19:55

That's a shame Bot0nist, I broke a 250ml 24/40 flask a few days back--I flipped because it was totally my fault. The next day I got my glassware kit--and it was all a-ok :)

inspector071 - 26-2-2012 at 20:50

I broke a 500 mL retort after my 2nd nitric acid distillation with the thing about a week ago. There was a solid cake of potassium sulfate left and I was trying to break it up so I could get back to distilling some more nitric acid. The cake of course thumped up against the glass, which I over-estimated the strength of, and promptly broke. Next time, I'll be more patient and let the potassium sulfate dissolve in hot water. Looking back, I would have been better off just buying a 500 mL distillation setup.

Mirage - 26-2-2012 at 21:12

I was just doing a simple steam distillation, and as I removed the hotplate from underneath the erlenmeyer flask, the whole setup fell over! I had my ring stand twisted the wrong way! Everything proceeded to fall to the damn tile floor, and smash. My steam distillation head with vacuum takeoff smashed, my heavy wall Erlenmeyer, and the bottom portion of my fancy coil condenser. NOOOO! Everything was Chemglass! Expensive! Luckily my receiving flask was fine as well as my vigreux.

Mirage

Bot0nist - 26-2-2012 at 21:15

Damn, that sucks. Happened to me once too, but I had a liter hot oil bath hit the floor with my glass! What a mess.

Sedit - 26-2-2012 at 23:42

Quote: Originally posted by neptunium  
i hate glass and glass hates me back! i was cleaning a round bottom flask after a distillation when this happen...



bad day indeed...

[Edited on 15-2-2012 by neptunium]



.....Holy fuck dude.... and you stopped to take a picture, are you serious?:P

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