Sciencemadness Discussion Board - What is the most ignorant thing you have ever done while conducting an experiment?

What is the most ignorant thing you have ever done while conducting an experiment?

Pages: 1 2

saps - 1-4-2005 at 14:29

What is the most ignorant thing you have ever done while conducting an experiment?

EbC: spelling

[Edited on 3-10-2005 by chemoleo]

Chris The Great - 1-4-2005 at 15:53

I'd have to say my entire distillation of acetone peroxide dissolved in acetone, with a flame, in mayo jars, with plastic components and high pressure.

That, and when I stuck my finger into a reaction involving fairly concentrated HCl to see how hot it was.........don't ask me why, I can't remember. It hurt a fair bit.

Magpie - 1-4-2005 at 20:10

This is really not a chemistry experiment but related:

When I was young I induged in my share of k3wlish acts (we all have a little k3wl in us

). I was firing marbles at a target with a pipe cannon charged with gunpowder. I did this right beside my house in a residential area as you could do that in the late '50s. This got boring so I decide to leave the ramrod in and fire it as the projectile. After lighting the Jet X fuse I ran around the sleeping porch on the back of the house. Just as I rounded the corner the cannon itself caught me in the calf. It had broke loose of its mounting and passed through both walls of the porch before intercepting me!

I could tell of other escapes but I'm not sure what the statute of limitations is on acts of k3wl.

PainKilla - 1-4-2005 at 21:16

I think that would be having Caro's acid shooting all over me. I made a batch to see if would do something (dont remember what) and rode over with it to my freinds. It was summer time around noon and apparently from what I can guess my caro's acid decomposed somewhat and the rubber stopper shot off and landed all over my neck just as I got to his house.

I just ran in and poured baking soda over my neck lol. He was like wtf. Needless to say.... Bike + bad stuff --(light/hot)-> bad.

Luckily, my skin only started to lightly burn. And it was red for a long, long time. I can imagine concentrated h2so5 landing in your eyes. MMM....

Armstrong's Mixture

MadHatter - 2-4-2005 at 00:36

31 years ago. Mixing red P and KClO3 together in a mortar and pestle. Blew my
eyebrows off !

sparkgap - 2-4-2005 at 05:45

Didn't you guys spin those tales in Whimsy a long time ago?

I forget which thread, however.

sparky (^_^)

froot - 2-4-2005 at 06:23

Anyone filled a sep funnel with nasty chemicals while forgetting to CLOSE the stopcock? More than once??

Try it, its a good way to learn damage control. I'm quite good at that now.

Mr. Wizard - 2-4-2005 at 11:54

I mixed some calcium metal filings, that were very course, with some sulfur and lit it with a match. You can't pull your fingers back quickly enough. I had white soot all the way to my knuckles and blisters too. I'm glad I got tired of filing and only had a small pile of calcium. Other dumb tricks involved setting my bed on fire with a Tesla coil; the spark went to the bed springs, and shocking myself with the capacitors when I forgot I had widened the spark gap to "shut it off". I also made an arc furnace and melted nails, dirt, salt etc, while looking through some dark sunglasses. I can still see the image, how convenient that I don't have to rely on my memory. Sunglasses don't work as welder's goggles. The dumbest trick was heating Potassium Perchlorate with concentrated Sulfuric to distill off the Perchloric acid. I had added the acid and was adjusting the asbestos pad under the flask so the bunsen burner wouldn't hit the glass directly. The explosion happened as I was under the level of the flask and parts of the glassware ended up in the ceiling. The chemistry teacher, who had approved this madness came in from the other room as white as a ghost. Amazingly nobody was hurt. The second dumbest trick was making up an ammoniacal silver solution (not an approved experiment ;-) late one afternoon while at the college lab. I thought it was in a safe condition so I locked it up for the weekend. Next lab session, I opened my glassware drawer to see glass shards everywhere. Whoops! I came back after everyone else had left and carefully cleaned up the mess. It only cost me the price of the lab glass I had checked out, which was expensive to a poor student. Live, learn, and tell those who will listen.

Two eyes, one face, and ten fingers per customer; don't lose them.

garage chemist - 2-4-2005 at 12:46

Long ago, when I only had my chemistry set, I tried to nitrate resorcinol with 30% HNO3 which I had boiled down to about 50%.
I added some resorcinol to the HNO3 (without H2SO4!) and it dissolved rapidly. I added quite a lot, about 2g to 4ml of HNO3. Nothing happened, so I heated it. Suddenly, it turned black and began increasing its volume. The black sludge became bigger and bigger and poured down the sides of the test tube and on my desk ( worked in my sleeping room). It began spewing large amounts of red gas which made me cough (I didn't know about its dangers then) and I left the room. A few minutes later, I came back and it still boiled and red gas was being produced. I had a very sore throat and lung pain for over a week and the burn mark is still visible on the desk.

vulture - 2-4-2005 at 13:06

Dumping >10g of questionable quality cellulose into 100ml of HNO3 DCM extract. Mighty fine runaway that was...

I have a bad habit...

Hermes_Trismegistus - 2-4-2005 at 17:23

The same as froot's

I tend to leave the stopcock in the open position, then commence to pour very carefully, whatever liquid I am washing, into the top of the sep funnel, and from thence, into my lap.

[Edited on 3-4-2005 by Hermes_Trismegistus]

chloric1 - 2-4-2005 at 18:32

When I was making ammonium chloride a few years back from janitor ammonia and muriatic acid, I left it on the burner too long and too hot and filled my entire house with sla ammoniac fog!! My roommate thought I was burning the house down!

Mr. Wizard - 3-4-2005 at 12:38

Chloric, have you noticed how it fogs the windows up for weeks after you get an ammonium chloride smoke?

BTW a straw broom soaked in NH4OH is a useful way of finding Chlorine leaks when you are in a protective suit and looking for the leak. You get the same white cloud, but I'm not sure what the white cloud is. Anybody want to suggest one. Maybe a mixture of NH4Cl and Hypochlorous Acid?

Silentnite - 5-4-2005 at 08:44

Ah I just had a fun one last night. Making a standard batch of AP, but I had some stuff setting in the back that I was letting ferment for the DPPP experiment. HCl, and Acetone. Nice dark red and all that. Well I added the H2O2 to it, and started a very bad runaway reaction. All of the liquid boiled away, and the house filled up with a smoke like gas. Which I have since come to find out was Chloroacetone. I believe anyways. So I gassed my family out.!

Thankfully I was the only one truly affected by it. And that fact alone got me off the hook with my family.

Ah the misspent times of youth. :cool:

uber luminal - 5-4-2005 at 18:50

I wouldnt call it ignorant, I would call it redundant education.
Arc melting screw ups:

1. moved my arm too close to the upper metallic shell, while arc melting a sample. A wingnut was about 3 inches from my wrist when the electricity decided my arm was a greater drop. left a sizable scar on my wrist and scared the piss out of me.

2. the dumber thing. finished melting a Al, Mg, Zn alloy puck. To help cool things off faster, sometimes I take the chamber to 1 atm of Ar. (typically most melts are done under a -15atm vacuum). So I flipped the Ar valve and for some reason stopped paying attention. BOOM! one of the O-rings burst, spewing out smoke and a fire errupted inside the chamber. (could have been worse)
3. Even dumber. After the above event, I sparked out the inside of the chamber to burn up the remaining mg/zn dust and cleaned it out with ethanol and towels. Then used the same ethanol towels to wipe up the floor where the smoke had shot down onto. I never sparked the dust on the floor so it was still active. I almost threw it away and probably would have started the trash on fire, but instead I noticed the little crackling patterns of red dancing around burning up the active dust and lighting the kimwipe on fire in my hand.

4. my favorite. just finished arc melting a Tungsten-Ni button. Usualy wait about 4-5 seconds before sliding the #11 shade off the port hole, but I guess that wasnt long enough. I quickly looked away from the demon light but I was still blinded for a short time (longer than I am blinded when accidentaly striking an arc without a shade). This was the brightest thing I had ever looked at. Imagine looking at a lightbulb filliment 1 foot away, which was the size of a (AA) battery while it was white hot. that has got to be the most ignorant thing I have done.

Polverone - 5-4-2005 at 21:34

Uber luminal: you need to post pictures of your arc melting setup and regale us with more entertaining tales of alloy-making.

Here's something I did that was profoundly ignorant but not dangerous:

When I was seven years old, I was reading some science books from the library and trying whatever I could with household products snatched from the kitchen and the laundry room. I read about grain elevator explosions, and read that flour could behave in the same way on a smaller scale. Not really understanding the "dust explosion" concept, I wrapped some flour up in foil with a piece of string as fuse, added a dash of rubbing alcohol for good measure, lit the string, and ran away covering my ears. The expected bang never materialized. First I was fearful that it was just waiting to go off, then I was sad that it did nothing. When my dad got home he demonstrated a couple of real firecrackers for me, which cheered me right up and made me more determined to crack the mysteries of explosives.

A couple of years later, when I had a little lab in the garage, I was suddenly thrown into terror by a hissing noise I heard as I was mixing a pyrotechnic composition. Jumping away from the bench, I saw that a bag of sand had tipped over underneath the bench and was spilling its grains with a soft hiss.

Around the same time I read in some book about people making explosives with sugar and tropical bleach (special calcium hypochlorite grains). Not realizing that tropical bleach was a lot different from the stuff in the laundry room, I tried mixing Clorox and sugar outdoors and never saw anything interesting happen.

I discovered stronger (hair-bleach) hydrogen peroxide around the 5th grade. I enjoyed making it bubble with all sorts of things. Cobalt chloride worked well. Cobalt carbonate, made with a mixture of sodium carbonate and cobalt chloride, worked much better. I realized only a couple of years ago that it was probably the pH change, rather than the cobalt carbonate per se, that made the mixture work better.

When I was six I used to play with a bright red towel that my dad used when washing cars. I could set gray pebbles on it and after some staring they would start to look green, like the whole world did when I looked away from the towel. At first I thought the towel was somehow making the little rocks more green.

Also when I was seven, my best friend was fascinated by dinosaurs and fossils. I thought that if animals falling dead normally could leave fossils over millions of years, we might be able to do it in just a few months if we helped things along. So I took chicken bones from the trash and placed them at the bottom of a bucket filled with mud. The fossilization didn't seem to work, so later we just added urine and plant matter to the bucket until we had a putrid mess.

When I was eight, I burned a pit in a large desk and filled a classroom with smoke while trying to demonstrate the power of oxidizers for "Show and Tell." I was going to put KNO3 in a soup can and insert a burning wooden splint. I forgot the soup can, and instead of aborting I decided I could use a big heap of KNO3 on top of several layers of foil. I paid too much attention to the audience and melted right through before I noticed anything was wrong. In the same classroom, I later set everyone to choking and holding their noses while demonstrating the exothermic union of sulfur and iron. Don't ask me why neither I nor any of the adults watching me thought to do these little demos outside.

In math classes, in too many instances to remember, I found little formulas or shortcuts that were easier for me to use/think about/remember than what the teacher was actually saying. When it came time to do homework and tests, I got marked down because I wasn't showing my work properly. Later I went to finding and writing down the answer first, then scribbling the right sorts of things above it to "show my work." It was a rare instance where external, rather than internal, ignorance proved a problem.

When quite young, I thought that sexual pleasure must come from some sort of chemical exchange between partners (given that I read a lot about chemistry and very little about the body). There were chemicals excreted by the penis that could stimulate the vagina (I had no notion of the clitoris) and vice-versa. It was so perfectly logical! The penis would be inserted and then both people would lie motionless there with goofy smiles on their faces, enjoying the chemicals they were exchanging. I didn't have any notion of orgasm either. When I discovered the self-induced orgasm, I felt like I had uncovered a great secret and wondered if it had anything to do with sex. But how could it, when my hand surely couldn't excrete womanly pleasure-chemicals?

Darkblade48 - 5-4-2005 at 21:41

LOL, Polverone, the last story is the best

sparkgap - 5-4-2005 at 21:48

After seeing your post, Polverone, methinks this should be a Whimsy thread.

Your second to the last anecdote was cool. :cool:

I had the same problem also. My untainted mind was thinking at the time, "Why aren't they teaching this stuff when things could be so much easier?" I found the sobering truth years later.

That last one, however, was hilarious!

But hey, IIRC, there are chemicals in semen that stimulate some "noticeable reactions" in women.

sparky (^_^)

Esplosivo - 6-4-2005 at 02:55

Quote:

Originally posted by sparkgap
But hey, IIRC, there are chemicals in semen that stimulate some "noticeable reactions" in women.

You are probably speaking about prostaglandins which induce contractions of the uterus and fallopian tubes, which might case pleasure, in women obviously.

My first most dangerous 'synthesis' was the production of ammonia. I was still 12 and had read that on mixing any ammonium salt with calcium oxide and heating gave ammonia gas. I started looking aroun and got my hands on around 500g of NaOH prilled which according to certain other references said it would also work since all that is required is a strong base. Well I crushed Ammonium sulfate and NaOH and placed them in a soft-drink glass bottle, those with a narrow neck. To the neck I connected a pipe which led to an inverted funnel in water. On heating only a small quantity of ammonia was generated. I thought, well hell why not add some water to the mixture. That was it. I added approximately 150ml of water into the bottle at one go. Conc. ammonia and NaOH soln sprang out at me from the bottle. I was drenched in it. Had to go to hospital because a small injury on my eye but that was it, I was very lucky. The other injuries quickly healed, except a very small unnoticable patch of hair.

The other dangerous experiment was due to my adventurous way to go about chem when I was young. On my old school books I had found out that strong oxidizing agents under acidified conditions could oxidize various compounds, such as alcohols. The only oxidizing agent I had was hydrogen peroxide, so I used that, acidified with dilute sulfuric acid. I first tried ethanol and I noticed no rxn. I then tried propanone just for fun, since I knew it wouldn't be oxidized being a ketone. But wonder of wonders a white precipitate occured. I was amazed and thrilled. I started 'mass producing' the stuff, and had as much as >50g of it, if not more. I went about to test what the hell this stuff was, by NaOH etc.... All of the tests gave a negative result until I heated the stuff on a spoon! Damn it did it give me a fright (and thanfully on that).

Those were the most dangerous experiments I have done although there are others. Btw polverone, those stories of yours are great

[Edited on 6-4-2005 by Esplosivo]

Mr. Wizard - 6-4-2005 at 07:39

This may not be exactly the right forum, but if any of you haven't stumbled upon this site before, it might make a humorous read:
http://www.armory.com/~spcecdt/pyrotech/doap/

Maybe in the K3wl category, but those without sin can cast the first stone. This guy makes plenty of mistakes.

neutrino - 6-4-2005 at 13:55

Explosivo: You meant ammonium sulfide, right?

Well, I might as well add my 2 cents. I can think of two things right off the top of my head.

One day, I had to boil down a solution of an alcohol containing a lot of dissolved magnesium sulfate. So, I put the thing in a flask and heated that over an open flame. I didn’t have any boiling stones at the moment, so I decided to just let the thing boil on its own. Well, it went without problem at first. As the salt precipitated, though, it coated the rough surfaces present and…well, the flash boiling shot ~150mL of EtOH out of the flask. 3 foot flames aren’t fun indoors.

Recently, I was playing with my Bi crystals and noticed that I always had 50mL of liquid Bi left over that I wanted to put into a form that could be easily remelted. So, I made a plaster mold for this purpose. Unfortunately, I hadn’t counted on the rapidity with which plaster dehydrates at this temperature and quickly got a small steam explosion. I’m currently waiting for the burn on my wrist to heal… Lesson to be learned here: always dehydrate the inside of the mold before pouring liquid metals into it.

silly thing you done

aldol - 6-4-2005 at 14:38

i was once distilling benzyl chloride not long started heating and forgot to put in the boiling stones in didn't think it was as hot as it was when i dropped the boiling stones in i blew the benzyl chloride
right out out one of the necks.

its then called run lab run like all fuck !

Again with the stories - LOL

JustMe - 6-4-2005 at 18:11

Dropping a few drops of absolute alcohol onto a petri dish containing liquid Chromyl Chloride. Whoooosh! Big flame!

That was just the stupid part, the (temporary) ignorant part was attempting to put out the flames with water. Ke-bang! Fortunately the chemicals were on the other side of a small concrete barrier.

Ramiel - 6-4-2005 at 19:09

These are all good stories.
One of the most dangerous thing's i've done is to load firecrackers into a metal pneumatic spudgun... but that's not reall chemistry. Oh my good lord, how awesome is it to have your very own artillery piece!

Even Mister Policeman asked if he could have a go! I love my country.

The stupidest thing I've ever done is to boil sulphuric on a metal hotplate. stupid stupid stupid.
Later that week, I was boiling (this time WITH boiling stones) ~93% H2SO4 over a bunsen - boiled to aezotrope, then let it cool for 'a bit', because I was afraid of the acid absorbing atmospheric moisture too much... I came out later, and picking it up with oven mitts (stupid again!), ferried it over to a cork board for decantation into my glass stoppered 1L flasks. I decanted it straight into the flasks - bad idea. The first one litre flask cracked off completely at the base at about 3/4 capacity.
My beautiful brick porch!
My beautiful soft, fleshy feet!!
I at least had the common sense to have a couple of kilos of bicarbonate sitting around.
That would have to be the most careless thing I've done. :cool:

Esplosivo - 7-4-2005 at 04:38

No neutrino, I did mean ammonium sulfate. It reacts with bases to give off ammonia, although in a solution most is absorbed by the solution the reaction is taking place itself so that little gas is released, especially due to the very high solubility of ammonia in water.

neutrino - 7-4-2005 at 12:57

Sorry, I was thinking H2S for some reason.

Reverend Necroticus Rex - 15-4-2005 at 03:21

When I was a good few years younger than I am now, I did my fair share of dodgy experimentation, I used to enjoy using a mixture of equal proportions of sodium chlorate and sulfur piled up on hte ground, to blow up large propane cylinders, not knowing not to mix chlorates with sulfur at the time, I remember that I kept a 10 kilogram bucket of ready-mixed NaClO3/S under my bed

I am quite lucky that it didn't go off on me when I was sleeping really, by some act of a higher power, it didn't ever ignite of its own accord, I shudder to think now, how close I came to a nasty accident.

I once also kept a bottle of Mn2O7 in my lab, not knowing quite how nasty it was, Read up on the web about its properties, searching for things to do with it, then promptly disposed of it after learning it was likely to explode in a malodorous cloud of ozone at a moments notice.

The most unpleasant thing that happened to me, a year or so ago, was trying to directly chlorinate acetone in a shot glass, of course, it flash boiled, spraying my lab with about 200ml of chloroacetone in varying stages of chlorination, sending me scurrying out of the lab with hands over my face and generally cursing and swearing about the stinging in my eyes.

OMG

chloric1 - 15-4-2005 at 09:51

The chloracetone thing sounds really painful. But the chlorate/sulfur cocktail is definately on my scary list. Especially 10 KG!!

Greenhorn - 4-6-2005 at 07:57

Just a few days ago, while letting a solution of acetone and nitrocellulose dry in a glass jar, I lit the gasses inside and then put my hand over it to put it out. It would have been fine (I later did it many times and it was fun), but I was startled by the sudden drop in pressure inside the jar, and I waved my hand and broke the jar on the floor, along with the acetone jelly.

That's not the most ignorant or stupid thing I've done, but it's the most recent.

Jome - 4-6-2005 at 10:37

I prepared a pyro composition consisting of a stoich ammount of 2,5micron zinc mixed with sulfur. It was about 15 grams. Then I lit it by a match while my face was only about 35cm away (one foot)

Pyridinium - 4-6-2005 at 12:22

As a teenager I re-discovered an unstable yellow liquid formed by two elements.

I also discovered you should never, ever let it touch wood ashes.

Ears rang for several hours. Lucky that's all that happened...

Edited for brevity: I have a couple other 'ignorant' stories too, but this one should be enough.

Edited to remove a couple details for the sake of Kew|s' safety who might be reading this.

[Edited on 5-6-2005 by Pyridinium]

uber luminal - 4-6-2005 at 22:23

I think drawing attention to it like that in itself makes you just as kewl.

neutrino - 5-6-2005 at 04:02

What's wrong with confessions? He seems to be refomed.

Pyridinium - 5-6-2005 at 07:02

Neutrino: damn right. After a couple experiments with it I moved on to much safer things.

Luminal: I wouldn't quite say that. After all, I didn't go "d00d when 1 waz |1k3 15 I herd u cud m1x A w1th B and it would det*n8!!!! So 1 D1D i+!!!!!"

Maybe the wording was bad in my post but I think you get the idea.

Teenage years are fraught with k3w1.

Edit: ah why not, here's another story... years back I knew a grad student who, when she was a couple years younger, was working in her company's lab and decided to have some fun. It seems she forgot- some materials vigorously decompose H2O2. And it wasn't 3%, I'm guessing.

The gas was evolved so rapidly that it blew the top off the thermos she put it in, making a hole in the drop ceiling.

Not sure how she explained that one away to her boss.

Now that... THAT was k3w1.

[Edited on 5-6-2005 by Pyridinium]

Nerro - 5-6-2005 at 13:35

The first ever thing Itried to make was AP. (back when the kewl in me still had a say in things). I mixed 3% H2O2 with a lot of 10% muriatic acid and a splash of acetone. A week in the fridge yielded nothing so I tried again with something stronger... 100mL acetone, 25mL 30% HCl and 60mL 35% H2O2. I stirred it with a wooden spoon (yesyes

) and then put in in the fridge and forgot it. After a week I had 100g of AP :S I ignited a gramme of it and got pretty freaked out by the thought that I had 99g more of that stuff. I took the glass jar to the river and dumped most of it. 30g of it were poured into a 1m deep hole in the ground and ignited. Wow. I haven't made AP since it scares me. I figured I'd be better of concentrating on safer chemistry. A nice byproduct of all this being that I'm now so interested in chemistry that I'm going to study it in University

[Edited on 5/6/2005 by Nerro]

Pyridinium - 5-6-2005 at 16:25

Quote:

Originally posted by Nerro
I haven't made AP since

That stuff is a horror show from what I've read. Never tried making it myself (never plan to either!!).

Hey, glad to hear it got you interested in professional chem though.

Chemistry is so interesting... it's just too bad some of those atoms don't like to hold hands.

Edit: I almost overlooked a gem on here:
"i was once distilling benzyl chloride not long started heating and forgot to put in the boiling stones in didn't think it was as hot as it was when i dropped the boiling stones in i blew the benzyl chloride
right out out one of the necks."

... I did the same ignorant thing a long time ago. With hot HCl. Bad, bad mess.

[Edited on 6-6-2005 by Pyridinium]

uber luminal - 23-6-2005 at 18:01

I'll add one to the list. Today I was etching with conc HF solution. I wear the typical 2 layers of gloves, lab coat, chemical goggles etc. My outermost layer of gloves are the big pvc ones. in my case they are a little big on my fingers, so they flop around a little.

Ok, so I should mention that I was wearing shorts, exposing my legs below the lab coat. My gloves had touched the HF solution a few times today. I was working and felt some random wetness on my leg. I thought maybe I could have flicked a loose glove end and spattered some solution on my leg. Paranoia goes to work. I quickly check the area for wet spot and feel for wetness by rubbing my fingers against it, and looking at my fingers to see if its wet. Duh! How ignorant can you be, to forget your wearing these big black smelly gloves, which can cross contaminate things... like acid to your skin. Ugh. So then I spent the next 10 seconds looking for the Calcium glut. cream, which someone had considerately put in a hard to reach place. Since 10 sec is really too long, I am really hoping that, while I was working, the gloves would have been rinsed enough times that I am not going to have a buildup of CaF in my blood stream.

I guess the moral of the story is... dont wear shorts when working with poisonous liquids?

EtherBunny - 28-8-2005 at 14:36

I hope I don't get lynched for digging up old threads, but I have to add my own chemical disasters here.

Most of them are your typical run-of-the-mill idiocy, such as having condenser hoses blow loose at the flanges and fountain water all over one's experiment, but I have done a few ignorant things.

I had the temperature of a pentyl acetate distillation reach 300 degrees once. I'm not sure how it happened, but I was convinced that I'd hit the flash point of the stuff and blow the whole thing, until I realized that I was reading the thermometer's Fahrenheit side.

Also, never leave experiments unattended. This, of course, is something we all learn in junior high or the like, yet we all do it eventually. And something always goes bad. Like my 4-methylcyclohexanol dehydration. I set up some apparatus, dumped in a mixture of concentrated sulfuric and phosphoric acid, and heated the daylights out of it, hoping to distill out 4-methylcyclohexene. Of course, in the mean time, I left the reaction to go to the bathroom and (I believe) for a walk. I came back to a stinky, acrid, smoking black mess which smelled somewhere between cow manure and a burnt fan belt.

The people in my organic synthesis labs used to do some pretty dumb things. Because they wanted to get out of the lab as fast as possible, their attempts at "experiments" were positively lackadaisical. Thus, all sorts of glassware breakage and mercury spills occurred, and all numerations of disgusting concoctions were formed. Common sense also went straight out the proverbial window.

For example, several labmates decided it would be a good idea to clean out a packed silica gel column by hooking it up to a compressed air hose. It made an uproarious noise, but an incredible mess.

A friend of mine managed to somehow screw up one of the student NMRs by getting a tube stuck in one of the probes. Instead of ejecting the thing out the rest of the way or calling for help, he reached in and *yanked* it out of the probe, snapping it off inside the machine. The NMR supervisor was NOT happy about that one, but my friend considered it a great accomplishment, even bragging about it the next day!

Lambda - 28-8-2005 at 15:24

This is one of my relatively innocent mishaps in the lab:

Originaly posted on 14-8-2005 at 06:23 PM by Lambda: These damn warts !:
https://sciencemadness.org/talk/viewthread.php?tid=4311&...

EtherBunny, it is interesting to read about mishaps in the laboratory, for these adventures can be very informative, and above all, hopefully prevent the same or even worse from happening to others.

About Fahrenheit:

They should make a statue of this man, put in on a stand, and let it be. This temperature scale should be abolished from science, for it creates to much confusion as you now know. Procedure translations, can be dangerously misconducted due to all this confusion.

About the bathroom:

Generally speaking, my experiments cause so much excitement, that I make it a rule to first viste the bathroom before any labwork is conducted, unless I want to end up on a "wet spot".

[Edited on 29-8-2005 by Lambda]

Duster - 28-8-2005 at 18:42

Not strictly chemistry as much as pyrotechnic, but nevertheless I have had a mishap (*cough* or two...) with the famous KNO3 and sugar smoke mix...

I uh... have a full photo album of both accidents, and what not but pictures havent been part of this thread thus far...

I dont know if that counts as kewl or just stupid (both?) but aside from that I havent done too much... or any "kewl" stuff I dont think... Ive put firecrackers in potatos and threw em like grenades... And potato guns, oh potato guns...

I can say I have been awfully close to some bad things that were about to happen, but somehow or another everything settled down...

The_Davster - 30-8-2005 at 16:25

Got a new screw up for y'all. I was about to attempt a prep of chloropicrin from silver fulminate and chlorine gas as it mentions in the chloropicrin file on the FTP. I add around .1 to .2 g of silver fulminate under water to a large testtube, a bit more water is added. So I go to place the glass tube to bubble the chlorine in, I (stupidly) drop it right down the test tube and *BANG* the bottom of the testtube is blown to bits and glass flys around the lab. Luckily I was holding the top of the testtube which did not even crack. I am just glad I was not holding it by the bottom of the test tube

I worry about how loud this was, as I was working right next to an open window.

Lambda - 30-8-2005 at 16:40

Rogue chemist, I avoid Silver fulminate like the plague. This stuff is just to sensitive, appart from the fact that crystalisation during preperation can also detonate. I would hate to imagin, what might have happend if your mother batch went "bang". Probably it wasn't a pissy 0.2 grams batch, no,.... much and much more.

[Edited on 31-8-2005 by Lambda]

The_Davster - 30-8-2005 at 17:17

Well the mother batch was around 0.6g, and it was 3 months old so that could have increased sensitivity. As dangerous as it is, I like it. It amazes people when a barely visible soggy speck of it when lit makes an ear ringing bang.

Crysalization during prep can cause it to det? Wow...really surprises me now how much I got away with then when first preparing it years ago in my youth, what I did getting the ethanol and acidic silver nitrate solution to react....

Reverend Necroticus Rex - 30-8-2005 at 17:19

Just this morning, well, yesterday, having not slept for 2 days, I attempted a quick small-scale synthesis of phosphorus iodides, and heated 10g each of red P and I2 together in a boiling tube, started to fume a bit, but all went fairly cleanly.

The cleanup was another matter entirely, in my daftarsed sleep-deprived state, I quenched with water, then added 45% H2O2 to clean the test tube, not thinking that the H2O2 is immediately going to oxidise the formed HI to I2.

I was holding the tube, over the sink in a tiny 2x3 meter bathroom, it started bubbling, so I put it into the sink, only for it to quickly boil, and start spraying out a dirty great bright purple plume of I2, EVERYWHERE along my bathroom, I scraped most of the I2 that sublimed itself on the cold sink and saved it, then went for my gas mask to do a quick cleanup.

Made possibly the worst mistake yet, and tried cleaning it with ammonia

It DID decolorise the ugly orange stains on the tiles, grouting and well, everything else, but I came to my senses half way through it, soaked everything with water, and left.

Luckily enough, no explosions so far, although I did learn that indoor phosphorus halide synths, sleep deprivation and nitrogen triiodide do NOT mix

12AX7 - 30-8-2005 at 19:43

Quote:

Originally posted by Reverend Necroticus Rex
and tried cleaning it with ammonia

Ohh, that's a good one. LOL!

Tim

chromium - 31-8-2005 at 03:43

Quote:

Originally posted by Reverend Necroticus Rex
Made possibly the worst mistake yet, and tried cleaning it with ammonia

Thats why we must to know how to make poisons or explosives. If you did not knew how nitrogen triiodide is made you probably had gone further.

Uncompatiblities data as these are given in MSDS are not very usefull: soda and acids are also incompatible no matter that soda is often best way to cope with acid spills.

My worst mistake was probably boiling solution of potassium dichromate and dilute sulfuric acid on oil bath without boiling stones. Liguid started to bump at some point (as low pH liquids often too) and bit of solution flew into the oil.

Hotplate turned to volcano of smoke and all the room was sprayed with mixture of oil, acid and 6-valent chromium.

[Edited on 31-8-2005 by chromium]

Breath deeply

chloric1 - 31-8-2005 at 09:14

hexavalent chrome mist i9n the air!?! Oh my GOD!

No seriously that is bad news. I need to buy some potassium hydroxide and make some strontium chloride from the pottery supply's carbonate. I have a real treat for you guys when I can do my "homemade dichromate synthesis". I will post more for you when I start my investigations. I will have to be extremely carefull too.

Mishaps, mayhem, and blunders in the lab

prole - 6-9-2005 at 18:51

I'm curious to know from other science-heads about lab activities that went awry, things that maybe inspired heart attacks or strokes (figuritively speaking) to the practicing chemist at the time but are funny to look back on...
I have two that I'm not proud of, but glad I survived to tell the tales, since no one I know personally would or should care at all. Would you like me to recount them? Great! Here they are...
Was attempting anthranilic acid from scratch via n-acetyl-anthranilic acid, which required mechanical stirring. Since I am not equipped with this means, I decided to shake the flask by hand for the duration of the reaction. I had welding gloves, padded clothing, a face shield and goggles on. The flask got so hot, all the water vapour was exiting the neck extremely fast, and scaring the shit out of me. It was bubbling angrily. Of course, this was done outside, one because it smells so bad, and two, I didn't know how it would go. I didn't feel it would explode, so I kept shaking it. (dumbass!). I thought if I set it down, bad things would happen, so I kept at it. Once the water was exhausted, the rxn ceased and failed, and I began to breathe again.
The other idiotic thing I did, was heat VMP Naphtha in an open beaker on an old cheap hotplate indoors, which evidently sparks periodically. It suddenly burst into flame, sending a nice 2 foot column of jet-like flame towards the ceiling. I could see that it wasn't going to spread any time soon, so I watched and waited, trying to figure out what to do. I had a fire extinguisher handy, but didn't want to make a huge mess if I didn't have to. I just put a glass funnel over the beaker and it went out immediatley. Once my nerves calmed, I noticed the pleasant odour of burnt hydrocarbons throughout my house. I told my wife that I was soldering with my blowtorch and burnt some plastic. I got away with it this time...
These are two things that go on my 'don't do that again, asshole' list. What's on yours?

12AX7 - 6-9-2005 at 20:15

http://www.sciencemadness.org/talk/viewthread.php?tid=3698

Hmm.. things that stunk up the house? One day I was grinding some slag, from an aluminum melt (so any impurities are well reduced). Of course it smelled strongly, but I kept grinding it anyway. Afterwards, Mom said the whole house smells like (farts/garlicy/who knows!)... I guess reduced sulfates, phosphates, carbides, and so on are present in that stuff.

I don't know what calcium carbide smells like, but it's probably like that, FWIW.

That's not really the worst I've done, it just smells bad.

Tim

[Edited on 9-7-2005 by 12AX7]

Fleaker - 7-9-2005 at 15:15

Well any calcium carbide present would have reacted with the water to give you some nice acetylene which reeks of garlic :-)

12AX7 - 7-9-2005 at 16:29

Acetylene doesn't smell like garlic, it's odorless... it's the trace elements with the carbide that causes that, remember?

Tim

The_Davster - 7-9-2005 at 16:56

It is phosphide impurities in the CaC2 reacting with water to produce phosphine which is the garlicky smell you refer to.

Fleaker - 8-9-2005 at 13:10

Acetylene doesn't smell like garlic, it's odorless... it's the trace elements with the carbide that causes that, remember?

Actually acetylene/ethyne has quite a pleasing smell when pure Tim.

Impurities give it that odor.

[Edited on 8-9-2005 by Fleaker]

kclo4 - 2-10-2005 at 15:28

well i just did my first "life" threatening "trick".
I had just got done distilling some HNO3 from H2SO4 and NH4NO3. i heard a small part of the distilling flask crack, now i was a little bit hurt from my new still having a small crack in it but i was afraid that it would brake and have all the hot HNO3/H2SO4/NH4HSO4 go all over my stove making NOx and stuff. so i got a bunch of "emergency" water Na2CO3 and NaHCO3 ready for the cato but it never happen. But as i was putting on the lid to my reagant bottle i twisted it just a little tiny bit and the bottle holding at least 150 to 200 mls of red fuming nitric acid broke in half, and making a sharp shard of glass go into my hand cutting a nerve as while the HNO3 got on my pants and all over the floor(only a little bit got on my pants say maybe a 5mls). I ran to my sink and sprayed water all over me then i put some carbonates on the spill and took a shower my hand finally stopped bleeding and i was thanking god that i was warring my face shield!!

Grrr what a waist of HNO3 and blood.

oh ya i was wearing a T-shirt and have over 40 nitric acid droplet burns on my arms!!!

what will happen if i get a little bit of HNO3 in my blood (we are talking almost nothing at all)

has anyone had reagant bottles break really easy?

kbk666 - 2-10-2005 at 18:41

Most ignorant thing I probably did was when I was synthing TNP and wore latex gloves...It eats through latex ya know (I sure didn't).

Magpie - 2-10-2005 at 19:22

klco4 says:

Quote:

But as i was putting on the lid to my reagant bottle i twisted it just a little tiny bit and the bottle holding at least 150 to 200 mls of red fuming nitric acid broke in half,

Was this a regular reagent bottle designed for nitric acid? Do you have any explanation for why the bottle broke?

kclo4 - 2-10-2005 at 20:11

Well, IDK what a nitric acid bottle is.......

It was one of those narrow necked reagent bottles from pelletlab (i figured it would work great nitric acid since it is stained glass)

Some of the other ones I have, have are bubbles in them that are stretched out. But I would not think this be the reason, it must be because the bottles there are crappy or something IDK.

Fun Fact: if i bend my hang just the right way i can see muscle or something way passed the skin.

nocturnal shadow - 5-10-2005 at 10:21

back when i first discovered Ap and was young and stupid i was trying to impress some friends. so first i put a little bit of AP (about the size of a pea) on the ground and hit it with a hammer, pop. so trying to be cool i put a bit of a pile down (a couple of teaspoons) and hit that, it made the a huge ka-boom and me and two of my friends shat ourselves and my ears where still ringing half an hour latter, but the funniest thing was his next door neighbour who was hanging out washing 20 metres away, the look on her face after the boom when all she could see was me lying on my back with a hammer made all the hearing damage worth it.

Douchermann - 11-10-2005 at 11:17

Haha, one of the most ignorant things i've done, was a long long time ago I used to rip apart fireworks and play with the flashpowder, well once I ripped appart a ton of fireworks and filled a little toy car with the flashpowder. Luckily nothing happened (the fuse didn't work right). Another thing was I was generating ammonia gas, and I mixed the NH4NO3 and NaOH together, and it turns out the NaOH had water on it, and the reaction started. I didn't know this at the time so I took a big breath and got tons of ammonia gas. TextGreen

DDTea - 27-12-2005 at 01:34

My whole Chloropicrin experiment was stupid. But the stupidest part was when I was unsure if it was successful, so I took my gas mask off and sniffed the reaction beaker.

It was successful.

The_Davster - 17-3-2006 at 15:55

Today at uni, I was drying glass with a bunsen burner in preparation for a grignard reagent synthesis. A just dried graduated cylinder rolled off my bench....I caught it

I got blisters on my fingers immediatly. Damn these hurt...
How was I so stupid....

[Edited on 17-3-2006 by rogue chemist]

rot - 18-3-2006 at 11:13

A few years ago I was experimenting with dynamite, and decided it would be fun to put some into a large chunk of concrete, I had a very small fuse (from a firecracker

). It detonated when I was only 10 feet away and pieces of concrete went everywhere, the matchbox that I dropped onto the ground after lighting the fuse was ripped to pieces by the flying rocks, if that was my head I could have been dead.

Some time ago I wanted to make calcium chloride for drying my nitroglycerin faster, from chalk (CaCO3) and HCl. I didn't know that this would foam alot, the acid was spilled all over the floor leaving me with a nice mess to clean up.

Recently I was purifying ammonium nitrate from fertilizer, something I did a 100 times. I was making a lot, so when it was boiling down I got impatient and went away to watch some TV. 10 minutes later my neighbour came to my home complaining his garage was filled with smoke. (we share the same garage, seperated by a wall but at the top there is a gap) The AN decomposed because I heated it for too long.

woelen - 18-3-2006 at 13:01

In my younger years, my favorite experiment was electrolysis of a tablesalt solution. I used 9V batteries for that, but the speed of the reaction was soooooo low...... I needed something more powerful.

One evening, I decided to take two electrical wires and made a plug on one side of both wires and the other side was left open with two pieces of copper wire sticking out of the isolated wires. I immersed these wires in a tub with 0.5 liter of water, with some table salt dissolved in it and then put the plug in the 220V wall outlet. A nice vigorous reaction started, gas was produced. I was watching this reaction, it looked nice. I was watching it from above. A green flocculent precipitate was formed slowly as well (I now know from the copper wires, both slowly dissolving, due to use of AC-power).
I did not notice, that the wires slowly moved towards each other. I just was watching the fascinating reaction .... suddenly there was a very bright blue flash, a loud crack and glass shattered all over the place. The salt-water content was splashed into my face (it was luke-warm). Then it was dark.... the fuse was burnt.
What happened, is that an electrical short circuit was formed and a tremendous amount of power was released, causing a small explosion under water. The liquid was blown into my face, but the explosion was so powerful, that the glass jar was shattered. Luckily, I had no painful things. The liquid was only luke warm and it was a dilute salt solution with just a small amount of the green precipitate, it was not particularly toxic or corrosive. The glass jar was broken, but the force of the glass flying around was not large. The only things I had to do was replacing the fuse and cleaning up the mess before my parents arrived (they could arrive every moment).

jack-sparrow - 20-3-2006 at 09:11

Here is my DO NOT DO list :

1) Pt/C in methanol (ignites violently)

2) Vacuuming an acetylene bag with an electric lab water-aspirator (explodes)

3) Synthesize a gas in a 5 steps synthesis and forget to keep filling the cold finger condenser with acetone/dry ice at the distillation step. Lost 10000$ worth of product

4)Forgot to secure stopcocks while distilling a highly valuable solvent. Solvent bumped, stopcock went away, lost 25000$ of products.

5)Manipulate a COLD 5L round-bottom flask filled with 500g of benzaldehyde and 4.5 L ether with nitrile gloves. Condensation AND nitrile gloves is a leading cause of RBF drop on the floor and a nice afternoon of cleaning a smelly mess.

6) More to come ... But not too much I hope

DrP - 21-3-2006 at 08:15

Not me I hasten to add, but my GF was teaching in the undergrad lab last week and was asked by one girl why she wasn't getting a vacuum on her buchner flask....

... she had connected the rubber tube which pulls the vacuum to the clamp rather than the buchner flask which the clamp was holding! Outstanding lack of understanding!!!

Once however, I managed to get the tube twisted in the sink when leaving some polymer to filter. Instead of going down the plug hole, the water sprayed up behind the sink unit. I dind't notice this and left the thing sucking all day.... ....which flooded the labs on the floor below much to the displeasure of the caretaker!

jack-sparrow - 21-3-2006 at 09:23

Here are some other examples (not mines) taken for undergrad labs.

1) Putting glass wool in a separation funnel !?

2) inflating a rubber pipet bulb with compressed air until explosion (impressive AND plain stupid) It can easily contains 50L of air

3) Rinse an erlermeyer flask with water, then filling the erlen with acetone (completely) to remove water traces...

4) Washing an organic phase with sodium bicarbonate, discard the organic phase, evaporate the aqueous phase and get a wonderful and generous amount of white solid which you THINK is your product !

Magpie - 21-3-2006 at 17:24

Sturdur, those are downright funny.

I never saw anything like that in my organic labs. of course the people who do those kinds of things are usually gone after the first 2 weeks or so.

[Edited on 22-3-2006 by Magpie]

The_Davster - 21-3-2006 at 17:41

I laughed pretty hard at the last one myself. But I have seen some stupid stuff in my time in the organic labs as well.
A couple examples:
Someone poured an ether extract into a vaccuum flask with the vaccuum line connected and running(aspirator was supposed to be used, not vaccuuum line), she poured down the side of the flask and everything was sucked down the vacccuum line.

Someone put their hand over the buchner while vaccuum filtering, his hand got stuck and he jerked it upward and the sudden pressure change sent product everywhere.

A girl was drying a testube by blowing compressed air in, and she for whatever reason had the rubber hose with compressed air right down the testtube and she let go, it flew across the room.

The pipette bulbs seriously hold 50L of air!

WOW. (we might not be thinking of the same type of pipette bulb though)

EtherBunny - 30-3-2006 at 18:28

Oh, you won't believe the kind of stuff people do in organic labs. My personal favorite is when people hook up condensers to aspirators and Bunsen burners to water lines.

I do research in organic synthesis, and a while back, when I was just starting out, I did something extremely dumb. I was making methylsuccinic acid, following an ORGSYN protocol. Since it's made from ethyl crotonate, one of the steps is to dump the whole thing into nitric acid to oxidize out any crotonate that may exist after previous step. Anyway, after I did the nitric acid step, I dissolved the whole works in benzene set it up to distill off the benzene to dryness.

The distillation was going at a slow drip, and I decided it would be the perfect time to wash some glassware, when all of a sudden I heard a sound that can best be described as "*BLAM*hissssssss." I looked over into the fumehood to see the entire inside of the setup charred and blackened, with a disgusting grey smoke pouring out of the vacuum port. The temperature was well over 170C, the distillation flask had cracked, and the stopper in the still head holding the thermometer had blown clean out, ejecting thermometer pieces clean out of the fumehood. I was still finding them two weeks later.

Moral of the story: If it contains nitrates and nitrated benzenoids, don't be washing glassware.

One of my colleagues, doing a similar distillation, once managed to decompose some thionyl chloride which blew sulfury gas all over one side of the lab and smelled like the worst fart ever. That was a nasty one to clean.

mick - 3-4-2006 at 10:56

Younger people 30 y ago were a lot more sensible

2) inflating a rubber pipet bulb with compressed air until explosion (impressive AND plain stupid) It can easily contains 50L of air.

The old red rubber pipette filler was well known to inflate with air and water.

From memory

Me and my friend, he was leaving, on a friday afternoon at work decided to see how much water this 25 ml pipette filler would hold. We were on works water pressure of over 60 psi.
After a while the joke got serious.
The rules were
After filling the pipette filler with water you had to pour the water into a glass measuring cylinder and only what was in the cylinder counted.
The results were
After a slow start a 2 l cylinder was require.
I got passed 10 l with spillage. My friend was well past that but the pipette filler went before he could move it.

It was only water under pressure and everthing was wet.

mick

Douchermann - 7-4-2006 at 19:10

Haha, thats awesome mick.

I have a couple stories, all mine are pyro related though, I seem to work a lot safer in a lab environment.

1) My friend and I were up at his farm about a 5 hour drive or so from where we live. We were making smoke mix, and I gave him the KNO3 and sugar and told him to go make about a pound of it. Well he goes back there, and I go back to my duty of making black powder (we made about 4 pounds of granulated blackpowder that night). Now, this is the key part, I brought my gas stove up for him to use. The spoon he is using to stir falls into the flame and catches. He panics and throws it into the pot with all the molten smoke mix. The whole batch catches. All I hear is a "oh shit", I look back and see an 8+Ft flame coming from behind the back of the pickup truck (where he set up the propane stove). When the flame stops, I go back to assess the dammage. The aluminum pot has a hole through it, the spoon is bent from the heat, there is black ash everywhere, and there is a heat scar on the back of the pickup truck.

2) The same friend and I had a bag of KClO4:Al flashpowder laying around. Well his dad recently bought the parts to make a big steel mortar tube, which we assembled. The mortar tube doesn't have a bottom yet, we were going to screw it into a peice of wood. My friend wanted a small fireball to come out of this, so I told him to load up a bit of the flashpowder and I was going to go prepare a delay mechanism. The delay was a peice of a flare core, delicately balanced on top of the tube. After it burned a certain ammount, it was supposed to fall in and ignite the flashpowder. I balance it, and we run about 20 or so ft away. He says "here, take this" and throws me the bag of flashpowder. There is maybe a couple grams of flashpowder left in here, and I remember making about 130 grams of it. All I say is "RUN!" He runs behind the garage, I run behind a different brick wall. After the anticipation builds up as much as it could, I hear the loudest explosion I have ever heard in my life. I run back to where the pipe was and all I see is a white/grey burn mark on the concrete where the pipe once stood. I look around for fragments for a short while, then a couple feet in front of me, the pipe hits the ground. This was about a 20 pound pipe and it was airborn for nearly 10 seconds.

3) This one was completely my fault. I made a batch of negative-x for the day. Then I put it in my coat pocket and forgot about it while I was at my friends house (same friend as the last two times). I fall asleep and drape the coat over my legs. Sometime during the night, the bag must have opened and collected moisture from the air. At around 7am, I wake up to a bright fire. I look down and see a 2 ft flame coming from my legs. I jump out of the bed and by then I realize what happend. My coat was completely ruined, and there is a big burn mark in my friends guest bed (which is in his room also). Him, I, and the other kid that was over just laughed as we tried to hide the evidence from his mom... which we did successfully.

EtherBunny - 8-4-2006 at 18:22

I saw yet another case of complete idiocy the other day, and it's amazing how using the wrong apparatus can really cost you. Yet another colleague, who is a dear friend but seems to be less organically inclined than some of are, was making some sort of acenapthene thing, a crucial intermediate for her synthesis.

This stuff had to be vacuum-distilled (at around 0.2 mm Hg or so) so instead of using something more suited for high vacuum distillation, like a short-path still head with a built-in Vigreux column, she sets up one of those great big multi-piece things with a huge condenser, and attempts to hold her thermometer in the distilling head with a large rubber stopper, which is full of cracks.

When she turned on the vacuum and started heating it up, it took forever to distill because air was being pulled in through the stupid faulty stopper and diminishing the vacuum. In the mean time, the air being pulled in with the distilling flask, combined with the high temperatures, oxidized her product and within a few minutes, everything was burnt, pure carbon. After all was said and done, she ended up with a broken 1-L flask and no acenapthene thing. The next day I threw away all of the rubber-stopper thermometer holders.

However, the most fantastical case of stupidity I have ever seen in my life was committed by none other than the PI. It was the true meaning of a recrystallization gone really, really bad.

He was attempting to recrystallize a metric assload of napthylacetic acid from, I believe, water, where he had it all in a 4-L beaker, boiling on a hot-plate set at full power, because that stuff was not going into solution. In his fumehood, he had another 4-L beaker, a 1-L beaker, a 2-L separatory funnel, and an Allihn-style condenser about three feet long. The sep funnel was right next to the hot-plate, and, unfortunately, it contained ether, which caught on fire.

I was on the other side of the bench doing something, and he yells "Oh shit!" I look over across the lab, and his entire fumehood is a roaring mass of flame. No exaggerations, this was the Bibical burning of Sodom. All he could say was "That's not too good." His vacuum lines started melting, and he charred the back of the hood real nicely, too. He ended up totaling his synthesis and destroying all of the glassware, (about six-hundred bucks worth, we estimate) including the sep funnel, which was his wife's. Oops.

Zinc - 23-5-2006 at 07:26

Today I and my friend were playng with bromine in school. Our chem teacher allow us to work with any chemical we want axcept conc. acids but I don't understand why she doesnt allow us to work with conc. acids if she allows us to work with bromine that is equally dangerous as most conc. acids. Anyway, we poured around 10g to 20g of bromine in a baker, put a spoon ful of Al powder and covered the beaker with a watch glass. This was the first time we were doing this experiment so we didn't know how violent the reaction is. So When the reaction started a huge cloud of a mixture of bromine and aluminum bromide was evolved that filled almost the whole chemistry cabinet. Imediently we walked out of the cabinet. Fourtunatly the cabinet is seperated from the classrom but some bromine and aluminum bromide did come in the classrom so the whole classrom was filled with the smell of bromine. At the same time our classmate were writening a exam and some of them put shirts over their mouths and noses. Suprisingly our chem. teacher was not wery mad at us.

[Edited on 25-5-2006 by Zinc]

S-Bursic - 25-5-2006 at 09:30

Actually, it wasn't 10g to 20g of bromine it was exactly between 12g and 15g.
Yes, I am the friend and we weren't playing with it, we were doing experiments.
We took a 100 ml flask and I poured in enough bromine to cover the bottom of the flask which was about 3 to 4ml of Br2.We put in one spoon (a very small spoon) of Al powder and then we covered it with the watch glass and waited about ten sec. when the bromine started to come out

. My opinion was that it was not properly covered, and that we put in too much bromine for our first time with bromine. It was pure luck that I opened the windows before the experiment started

. We came in about then minutes after and it was still pinching in the throat if you breathed.
Three days after and you can still smell bromine in my hair and my clothes(yes i washed them).
It was a very instructive lesson, although.

Fleaker - 25-5-2006 at 14:51

I know bromine well. Your first mistake was adding aluminum powder. It might take a little while to get off, but use aluminum foil

Much safer than aluminum powder. Another thing to watch out for is not touching a bromine bottle that has bromine on it. First it looks like you cut yourself (the blood red color sans fuming

), then it feels like it!

I did another foolish thing a while back, actually, while synthing bromine from NaBr. I added the sodium bromide to the 32% hydrogen peroxide forgetting that halide ions *catalyze* the decomposition of H2O2. Silly me. Oddly, the 2L of peroxide were just fine carrying it up from the basement. As soon as it reached the sunlight of the backyard...well, needless to say, it flash boiled and sprayed boiling hot peroxide onto my friend and I. Not to mention the liters of oxygen and steam shooting out of the container!

[Edited on 25-5-2006 by Fleaker]

Zinc - 26-5-2006 at 07:32

Originally posted by Fleaker:
Another thing to watch out for is not touching a bromine bottle that has bromine on it. First it looks like you cut yourself (the blood red color sans fuming

), then it feels like it!

Yes I know that. I once got some bromine on my skin.
My finger was brown for 4 days.

S-Bursic - 4-6-2006 at 10:50

I made a mistake, it wasn't a flask it was a beaker. I often mix those two because I don't speak english very often. My apologies.

UniversalSolvent - 4-6-2006 at 11:14

I accidentaly shifted a thistle tube during simple generation of hydrogen using H2SO4 and zinc. A bit of hydrogen shot up the thistle tube and spattered the acid on my shirt and hands, eating large holes in the fabric. I could feel my skin tingling, but the acid was neutralized before any bodily harm was done. I'm just glad that this mistake wasn't made during a reaction using heated sulfuric acid. That could be very nasty indeed.

Someone once told me a story of a large quantity of H2SO4 fountaining out of a piece of glassware into their face during a school experiment. He's not blind though, so it seems nothing overly bad occurred. That would scare the hell out of me, though.

[Edited on 4-6-2006 by UniversalSolvent]

12AX7 - 4-6-2006 at 11:23

I know a precious metal refiner who says he once got a drop of nitric in his eye. After a while the top layer of skin flaked off, doc said the body is more capable of neutralizing acid than base, if it had been NaOH he'd be blind in that eye.

Tim

ethan_c - 12-6-2006 at 00:00

Quote:

Originally posted by uber luminal
1. moved my arm too close to the upper metallic shell, while arc melting a sample. A wingnut was about 3 inches from my wrist when the electricity decided my arm was a greater drop. left a sizable scar on my wrist and scared the piss out of me.

Did I tell you about this- when I was TIG welding the other weekend, I found out that the machine I chose to work on happened to be broken that day (the grounding wire had corroded away at the machine connection). I was also welding thick aluminum plate, so had it set somewhere between 300 and 315 amps- what's interesting is a day or two later, the initial blister sloughed off, and there was another blister underneath! At this point, a couple weeks and about four blisters later, this is proving to be a rather interesting injury in my experience. Rather painful at the time, the only experience I have to compare it to is a cattle prod to the forearm, and they are similar indeed.

ethan_c - 12-6-2006 at 00:06

Quote:

Originally posted by Zinc
Yes I know that. I once got some bromine on my skin.
My finger was brown for 4 days.

My chemistry teacher had some extra bromine, and he sure as hell didn't want it around, so I figured, "Hey, I'll add it to my element collection! Woohoo!" He bottled it up for me and sent me on my way- unfortunately, he put it in a round-bottom bottle, so I just set it sideways on the wooden table where I keep all my in-use chemicals and experiments in the garage. I figured he knew what he was doing- imagine my chagrin when I opened the garage door the next morning to the hearty stench of bromine settling over everything. It had literally melted the cap into a little plasticky puddle, eaten a fair way into the wooden table, and was corroding some nearby transformers at a remarkable rate. So I had the fun of cleaning up bromine everywhere with paper towels, safety glasses, and a home depot respirator. I set up all the fans we had in the garage, and only felt like I had strep throat (strep lung? heh) for not quite a week!
Life is full of nice little surprises, eh?

woelen - 12-6-2006 at 07:07

Ethan, welcome to the world of the halogens

. They are like aggressive animals. Almost impossible to keep in their cage, and while breaking out, they destroy everything on their path. I have had a similar experience some years ago, with a bottle full of chlorine gas, which I prepared and wanted to store in a fridge for future use. A few days later, the inside of the fridge was rusted liked hell. The cap was eaten away and the gas had escaped. Just 1 liter of gas, and it was a real mess. Fortunately, the fridge was a very old thing.

Even iodine is a very nasty little beast, when it has to be stored. It does not eat away caps, but it certainly escapes. I have my iodine stored in a glass bottle with thick plastic cap, wrapped in tissue paper, and then a plastic bag around it. And this plastic bag in another glass bottle with plastic cap. Even with this arrangement, there are brown stains around the glass bottle.

Jdurg - 18-6-2006 at 15:17

I concurr that halogens are a BITCH to store. Thankfully, my iodine that is not sealed in an ampoule is behaving. I have it in an amber-glass bottle with a PTFE cap and NUMEROUS wrappings of Teflon tape around the threads as well as the outside of the cap. The Iodine is then put in a plastic bag and then put into a metal can. No corrosion or noticeable iodine vapor. Bromine is a different beast altogether. ALL of my bromine is permanently sealed in a glass ampoule.

Now for the accidents/stupidity.

1): Junior year of college analytical lab. I was determining the metal composition of a US Nickel. The analysis required the use of concentrated HNO3 and H2SO4 at various parts. So I took the acids and poured them into separate beakers, but forgot to label them. At the end of the lab I was in a rush to leave so I picked up each of the beakers using my one open hand. Thankfully, I held the HNO3 beaker in the hand, but I grabbed the sulfuric acid one by just shoving my thumb into the beaker right into the liquid there. I foolishly thought it was water.

I quickly raced to the disposal area praying to god I didn't drop either of the concentrated acid beakers. Meanwhile, my right thumb was starting to tingle. (Thank god for the presence of dead skin to slow down the "eating" of the flesh). What hurt more was when I finally put the beakers down and washed my thumb in water. Got some nasty thermal burns there, and at the same time wound up moving my forearm over a spilled HNO3 puddle. Skin turned yellow for a few weeks and made a nasty little scar. (Though the scar is mostly healed).

2): Sophomore year of college in my organic lab I did a REALLY stupid thing. At the beginning of lab, I accidentally knocked over an open container of diethyl ether onto my jacket. I went and hung my jacket up near the fume hood so that the ether could evaporate away during the 2 hour long lab. The fumes were making me a bit funky, but I figured the fume hood would take care of everything. After lab, I grabbed my jacket and put it on. I went outside but didn't notice any odors. (Probably because I had gone numb to them after being around them for a few hours). I lit a cigarette and heard a VERY loud "WHOOSH!!!". I then felt very warm and realized that when I scratched my forehead little black flakes fell down. Then I smelled the odor of rotted eggs. I guess there was enough ether vapor coming off of my jacket to ignite and instantly burn the hair off of my face. I looked like an idiot for quite a long time, and my eyebrows still haven't fully returned. Heh. I guess smoking really is bad for you.

3): A few years ago I wanted to make some chlorine for my element collection. Up to that point, I had heard that chlorine was a green-yellow gas but never had a chance to see it in person. At that point in time, the only colored gas I had personally seen was NO2 which is pretty darkly colored, so I figured the yellow-green color of chlorine gas would be just as intense. WRONG!!!! Cl2 is pretty faintly colored and unless you are looking through a very large amount of it, or a very high pressure of it, it's not instantly visible. So I had a small glass jar and had some calcium hypochlorite powder and some acidic drain cleaner I had bought which had HCl in it. I knew that if I mixed them some Cl2 should be generated. I added a slurry of the hypochlorite and the HCl drain cleaner. It bubbled up a bit, but not too intensely. I didn't notice any green color in the jar so I put it up to my nose and inhaled deeply to determine what was going on. A few things I can tell you is that yes, it did produce chlorine gas, and yes, my lungs and nasal passages hurt for weeks. It also showed how brain farts and chemical reactions are not a very good combination

The_Davster - 24-6-2006 at 19:42

Let me just say, kimax is not invincible, I was boiling a KClO3 solution after running a cell, the bottom of the 2L beaker broke, and the hot chlorate solution containing what would theoretically be almost a pound of potassium chlorate went everywhere. As my hotplate needs some fixing, I was doing this on the kitchen stove, which only magnified the mess as having several hundred grams of KClO3 precipitate in the space between the stove and the counter was a bitch to clean up. :mad:

It even got inside the oven somehow.

And I needed that chlorate, the first is coming up :mad:

I will also be taking a brief international flight soon, I am hoping chlorate isent one of the things swabs for explosives pick up...

...not that Im bringing it with me, just crosscontamination I am worried about.

[Edited on 25-6-2006 by rogue chemist]

dejitaru - 2-7-2006 at 23:54

I was making nitroglycerin.

And I added the glycerin too quickly. I felt the beaker get warm so I rushed it to the deep freezer and thought nothing of it. Seconds later, a thick orange fog comes billowing from the chest and rapidly fills the room. I open the front door, put on my shoes, and get the hell out of there. The novelty subsides. Holding my breath, I step in and drag the freezer (still containing the nitroglycerin) inch by inch out the door. Mild nausea sets in.
It took an hour or so to ventilate the house and clean the freezer.

I set it on a towel to dampen the shock. The stuff boiled over and disintegrated everything.

[Edited on 2006.07.03 by dejitaru]

hinz - 5-9-2006 at 14:54

Last weekend, the same shit with chloracetone as Reverend Necroticus Rex happened to, happened to me.
I learned on the painful way that it isn't possible to scale up a well working test-tube reaction to an amount that reacts in a 1000ml RBF.
The acetone trichlorisocyanuric acid mixture in the test-tube only boiled after adding some sulfuric acid as acid catalyst. (acid catalysed enol-aldol reaction).
So I thought if it's only boilling a bit in the test-tube, it works also under reflux. I put 120 g C3O3N3Cl3 (0.5 mol) in the flask, connected the joint, put the cooling water on and begann to add 600ml (appr 10 mol) of acified (10ml H2SO4)acetone from the top of the condensor. I expected the mixture to boil and the evaporation heat to take away the excess heat, for this purpose I used the large excess of acetone (1,5 mol of 10 mol gets (mono) chlorinated).
But I thought wrong. First nothing happened but then the temp. rised, it begann to boil and the bubbles climbed in the condensor. After this I went instinctifly backwards and a few seconds later the flask exploded to quite small pieces of glass.

Afterwards taken for your amusement:
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...
http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...

Later (after cleaning my lab) I tried it aggain, this time I preheated the acified acetone to boiling and added the TCCA in portions of a few gram a time. This time it worked perfect, on each addition of TCCA, the mixture boiled of it's own, so it was not necessary to heat it.

http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...

http://pic20.picturetrail.com/VOL1206/4241286/12555424/18477...

BTW. Does anyone know if this reaction is possible:

CH3COCH2Cl + CHCl2-CONH2 + NH2-CH3 =triethylamine=>
CH3-CO-CH2-N(CH3)-CHCl-CONH2

If I condense the product later in alkaline solution, does it give a useful yield as a heterocyclic ring by condensation of CH3 from acetone with the CONH2 from acetamid or give it just a polymer?

Nicodem - 6-9-2006 at 06:42

I can't believe you added 10ml H2SO4 when a couple of drops is enough! Neither can I believe you used no ice bath! And you actually dripped the highly acidified acetone onto the full batch of solid TCCA! You just called for a disaster. You are lucky there was only little chloroacetone formed before the flask blowing up or else you would be in dip shit.
I’m glad you are OK, but let this stupidity be a lesson to you.

To all that are about prepare chloroacetone:
STICK TO THE ORIGINAL PATENT PROCEDURE AND DO NOT FUCK UP WITH STUPID AND IRRATIONAL MODIFICATIONS!

How many times must this be said? Chloroacetone is something you really don’t want to mess with. The TCCA chlorination is very exothermic and MUST BE COOLED with an ice bath or else it will runaway. No more than the needed amount of H2SO4 must be used. Don’t add more if the reaction seams slow, rather have patience and wait. It can take one hour for all the cyanuric acid to precipitate but at least you will avoid such disasters.
Remember that here you have a very concentrated solution of a powerful oxidant with a fuel, which is technically speaking an explosive mixture!

Besides if one wants a pure product the reaction must be conducted in an ice bath anyway, and the amount of acid catalyst minimum. Otherwise you get more overchlorination products.

garage chemist - 6-9-2006 at 10:50

Adding acidified acetone to solid TCCA will produce no chloroacetone and only polychlorinated derivatives, since you have a large excess of chlorinating agent at the beginning.
If the flask wouldn't have exploded, you'd have been left with a solution of polychlorinated acetone in excess acetone, i.e. no yield.

Zinc - 30-4-2007 at 01:25

Yesterday I was making a mixture of KBrO3, S, Fe powder and paraffin oil. I started adding the paraffin oil with a dropper that I used before for H2SO4 and I didn’t wash it. The mixture ignited in the mortar. It burned fast and the mortar survived unharmed.

Grignard rxn

dedalus - 30-4-2007 at 13:28

The second worst thing in chemistry is when the reaction doesn't go.

The worst thing is when it goes just a little too well.

I was attempting to make a Grignard reagent from a lacrymatory halide that shall remain unnamed. The reaction wouldn't start. Add Iodine Crystal. Nothing. Scratch scratch scratch with a glass rod. Nothing. Heat it a little. Nothing.

Finally...a little bubbling. A little more. Now, a lot of bubbling....cut to: boiling reaction mixture spurting out of the top of the reflux condensor like something outta a John Holmes movie.

OhMan. Thought I was going to die, with my eyes tearing.

nitro-genes - 3-5-2007 at 06:40

When in highschool I found an old dusty chemistry book in the attic that belonged to my father, it mentioned the industrial nitration of glycerine with 1 part nitric acid and 2 parts sulfuric acid at a temperarure of 0 degrees to produce nitroglycerin. The information about nitroglycerin itself was pretty limited, but said that it would explode from the least amount of heat or shock.
So I "borrowed" some nitric acid from school and made about 15 ml's of nitroglycerin. After scooping of the oily layer with a spoon I found that it didn't explode when lit with a match. Well, surely this couldn't be nitroglycerin then. Angry as I was I splashed it all into the sinc of my mother to flush it down the drain...

I used to make dark aluminium powder from aluminium foil in the ballmill. This took about 5 days to complete, but after several 200 gram batches, I started to wonder how it would be after 14 days. To eliminate excess oxide formation I decided to make the drum as airtight as possible. After two weeks I was eager to see the result, so without thinking I opened the drum directly which imidiately burst into flames. This scared me so much that I dropped the drum, creating a sort of jetengine like white flame that sounded like a freightrain. The neighbours living 200 meters abroad later asked if we had seen a very bright light as well.

[Edited on by nitro-genes]

vulture - 3-5-2007 at 14:15

I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway, these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.

They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap, they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt.

dedalus - 4-5-2007 at 10:10

Quote:

Originally posted by vulture
I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway, these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.

They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap, they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt.

Merck Index #1851 - Caro's Acid.

H2SO5....the active ingedient. Also called peroxymonosulfuric acid. The Merck entry references two explosions, one at Brown U in 1955, one at Sun Oil in 1960.

Nerro - 4-5-2007 at 10:32

Quote:

Originally posted by dedalus
The second worst thing in chemistry is when the reaction doesn't go.

The worst thing is when it goes just a little too well.

I was attempting to make a Grignard reagent from a lacrymatory halide that shall remain unnamed. The reaction wouldn't start. Add Iodine Crystal. Nothing. Scratch scratch scratch with a glass rod. Nothing. Heat it a little. Nothing.

Finally...a little bubbling. A little more. Now, a lot of bubbling....cut to: boiling reaction mixture spurting out of the top of the reflux condensor like something outta a John Holmes movie.

OhMan. Thought I was going to die, with my eyes tearing.

"Out of a John Holmes movie" LOL!

Was it benzyl bromide? I hated working with that.

Quote:

originally posted by Vulture
I've heard a nice story this week. There is a physical chemistry department at my uni which is located in a different building (fortunately!). Anyway, these guys use alot of wafers and they clean them using SPM, which is basically 30% H2O2 with conc H2SO4, aka piranha fluid.

They use quite alot of the stuff, about 25-50L per week. After they were done with it, thus when it was nicely contaminated with all kinds of crap, they had the brilliant idea of storing it in 25L jerrycans to be disposed of later. Unfortunately they screwed the caps on TIGHT and put it in a room with windows which faces the south. With the extremely nice weather here (30C) it was ofcourse an accident waiting to happen. One of the jerrycans blew up during the weekend and the other one whilst they were cleaning up the mess. It's a bloody miracle nobody got hurt.

PhysChem... It takes all kinds I guess

Who was responsible for the disposal of the Piraña? Was he punished in any way?

dedalus - 4-5-2007 at 11:30

It was benzyl chloride.

Nerro - 4-5-2007 at 14:18

Come to think of it, I once did an oxidation with pyridinium chlorochromate which suddenly went berserk in similar way. Nothing happened for an hour so I decided to heat the reaction mixture a little. Once the temperature came above 35 degrees I stopped heating to see what would happen. The mixture kept on heating up and after a while the temperature was as high as 120°C... (the manual stated that a maximum of 60°C was to be observed!) The reaction didn't splatter all over the place or anything nasty like that but the products consisted solely of a black smelly tar-like substance...

Still, it beats the hell out of that little LiAlH4 accident...

[Edited on 4-5-2007 by Nerro]

Zinc - 16-5-2007 at 03:16

I was once making chlorate whistle mix. I know that the chemicals shouldn't be ground together but I did it. The mixture exploded in the mortar and slightly injured my hand but the mortar survived unharmed. Before that I was grinding the chemicals together in a glased mortar so it didn't explode. This one was not glased.

Also I was once making a mixture of NH4Cl, NH4NO3 and Zn. The mixture ignites when it comes in contact with water. The film can in wich I was mixing the chemicals by shaking them together wasn't dry so the mixture ignited but I dropped the film can imidiently so I was not injured but the carpet on wich it fell was burned. Before that I made the same mixture and it didn't ignite when I put a drop of water on it.

[Edited on 16-5-2007 by Zinc]

phangue - 13-6-2007 at 14:03

I was trying to dissolve fragmented tire leads in about ½ quart of HCl. I decided to hasten the process by cooking it on a hotplate. Trouble was, the container was not heat resistant. Then, I had to clean up the hotplate, work bench, me, the floor—the whole room with a water hose. GO FIGURE!

The second most ignorant thing was when I got interested in home-brew munitions years ago. So I nitrated some cotton, put it in a bottle (about ¾” in the bottom) and forgot about it. Several years latter, a friend and I was discussing munitions, and he said, “Phangue, you realllly should get rid of that gun cotton—someday it will torch your house.” Several weeks later I took the bottle to the back yard, uncorked it, lit a match and touched it off--inside the bottle. The resulting fireball took my moustache, eye lashes, and brows. Funny thing was that the mild mannered, elderly lady over the fence replied, “I don’t know what the shit he’s doing!”

hashashan - 13-6-2007 at 23:57

I think i beat all of you guys with stupidity

Did anyone was stupid enough to dry TACP over H2SO4? well i think i was stupid enough some time ago.
i accidentaly bumped the beaker and the plate with about 20 grams of TACP just fell into the H2SO4, it detonated instantly opening my hand, tore it open quite nicely, if thats not enough i was all sprayed with quite hot H2SO4. got about 10% body burns some of them 3rd degree and really deep. it took me about 2 months to heal from the burns (still have some really severe scars) 2 operations were made to reapir the hand(which i have to say is almost ok now, almost full movement however the torn nerves are still not healed and the sensation on one finger is dull).

Oh yeah the place was also quite a mess, the beaker blown a hole in my table(i got really lucky that the gasses were blown towards the wall and only a tiny amount went into my hand, otherwise my hand would be shred into little pieces). Half of my clothes had holes in them, my bed is still holed like hell(i do have to buy a new one), traces of acid could be found even after cleaning all my room with sodium bicarbonate solution even after 2 months.

So do i get an award?

Phosphor-ing - 14-6-2007 at 06:03

You very nearly got The Darwin Award!

Pages: 1 2