Sciencemadness Discussion Board - Stupid Mistake - A Warning to All

Stupid Mistake - A Warning to All

Backyard Blaster - 8-10-2003 at 06:02

I've had plenty of experience making acetone peroxide, using HCl. But the other night, I had finally obtained some H2SO4 in the form of drain opener. It had a reddish tint to it, and for some reason I assume it was quite dilute. I couldn't have been more wrong. After mixing the two other ingredients and cooling the solution, I proceeded to what was thankfully a spacious work area to add the acid. Most, but not all, literature on the subject says when using H2SO4 for this purpose, to add it drop by drop. It does not, however, mention what happens if you dump in a bunch (say, 50mL) at once. Assuming that the acid was dilute, and that this was safe to do, I proceeded to pour it into the mixture.
You can probably guess what happened next. If you can remember Mt. Saint Helens, than you've got a pretty accurate picture.
The violent chemical reaction left me with a huge mess on the floor, a jacket that now looks like swiss cheese, and a scare that will last me a lifetime. I was able to wash the acid off my skin before it could cause any burns. I plan to clean up the rest of the mess with a water / sodium bicarbonate mixture, which I will also use on my now-tattered jacket.
I immediately realized my mistake, and I still can't believe I did something so stupid. But I partly blame the literature for failing to point out this dangerous possibility. It's another example, of what danger even a slight lack of knowledge can present. Hopefully by sharing this experience I can spare someone else from perhaps serious injury.

Nevermore - 8-10-2003 at 06:36

not lacking of knowledge, but not reading the bottle, it is clearly written SULFURIC ACID 98%

Duster - 8-10-2003 at 06:56

Lucky that was AP and not NG... Last thing *I* want is HNO3/H2SO4 splattering on me...

Backyard Blaster - 8-10-2003 at 09:44

Actually, I throughly read the labels before I even bought the stuff. It only says "CONTAINS SULPHURIC ACID", and does not specify the concentration. I think it's a safe bet that it's at least 90% pure. I assume the red coloring, is to make spills easier to identify and clean up. Given it's purity, I assume it would be suitable for such uses as HNO3 synthesis. Someday, when I get my wits back, I may give that a try.
I always handle chemicals with the most extreme care, this is the first (and hopefully last) such accident I've ever had. Even the best of us make a mistake at some point, and I'm sure many of you have similar stories to share.

Nevermore - 8-10-2003 at 10:06

go look for HNO3 at agricolture reseller, they use 55% conc for correcting the soil acidity adding NO3 at the same time, kinda cheap, 10 bucks for one gallon...

madscientist - 8-10-2003 at 11:50

It's unfair to blame the literature for the accident for its failing to cite everything that could go wrong assuming one blatantly ignored all its instructuions.

Glad to hear you're okay, though. That incident could've been far more serious than it turned out to be.

[Edited on 8-10-2003 by madscientist]

Backyard Blaster - 9-10-2003 at 06:49

I don't entirely blame the literature; I'm just saying that it ought to point out this dangerous possibility. Most NG data warns of the consequences of adding glycerine too quickly, but no AP data I've seen warns of a mistake like mine.
You're also right, that it could have been much worse. I usually prepare such mixtures on a shelf, but on this night, I had the bottle on the floor because the light was better. Had this been on a shelf, at eye level.... I don't even want to think about it. It's still a miracle I didn't get anything in my eyes, considering some did hit my face and the acid was spewed over a 6-foot+ diameter. You can be certain I'll never make a mistake like this again.
Just out of curiosity, what gasses are produced when cleaning up an H2SO4 spill with NaC2 + water? I had to wonder, as I watched it fizz.....

AngelEyes - 9-10-2003 at 08:04

I did the same damn thing. I added a splash of H2SO4 to about 100ml of acetone/H2O2. The sulphuric reacted with the water in the peroxide giving out a lot of heat. This I assume vapourised the acetone which flash boiled taking most of the rest of the liquid with it in a cloud of vapour out the top of the beaker. I lost some of the carpet, a few clothes (including a jumper I really liked) and a small amount of gas out of my backside. I count myself lucky that it neither caught fire or went in my eye....could have been much worse.

Backyard Blaster - 9-10-2003 at 15:54

When this happened to you, was it a really violent reaction? Mine created a loud WHOOSH!!
While cleaning up the mess today, I even noticed some spatters on the ceiling....
It might be prudent for everyone to keep some baking soda handy, when working with any such acids. Just in case.

AngelEyes - 10-10-2003 at 02:52

Yep. For about half a second after the acid addition it was fine then, just as with yours, whoooosh! I guess the heat also liberated some O2 from the peroxide so I must have had a hot cloud of Acetone and O<sb>2 - damn lucky it didn't ignite.

vulture - 10-10-2003 at 13:38

what gasses are produced when cleaning up an H2SO4 spill with NaC2 + water?

Honestly, this clearly shows why you fucked up. You're merely following recipes, instead of using your brain.

It's Na2CO3 in the first place. If you can't even get the formula right, then how you're supposed to figure out the concentration?

I suggest you take a step back and shape up your theory before doing any other "quickie" experiments.

BromicAcid - 10-10-2003 at 14:33

A similar mistake happened to me, although it wasn't a mistake. Back in my high school days when I didn't know what a haloform reaction was I was trying to figure out why CH3COCH3 + NaOCl went to CHCl3 so I tried to figure out and did some experiments. I tried things like HCl + Acetone and many others, finally I thought that the reaction was not doing good because I needed hypochloric acid to make the reaction work so I decided on using peroxide so HCl + H2O2 ----> 2H2O + 1/2Cl2 then the peroxide would oxidize the chlorine to the hypochloric acid and the reaction would take palce to make the chloroform (now it just seems stupid, you know, haloform reactions, basic enviorments) anyways, I mixed equal volume amounts of 40% H2O2 30% HCl and Acetone for a total volume of a touch over 600 ml. White crystals started to condense on the inside of the flask just above the liquid line. I freaked out and dumped it on the ground when it started seperating into layres and went over 170 C. On the ground crystals started 'pushing' out and the god awful chloroacetone started wreaking havoc with my eyes. I decided getting away would be a good thing so I went into the house for a couple minutes, three minutes later there was a loud explosion, the spot where I poured the mixture out was now a one foot deep crater. It was a very unique experience. Unique as in bad.

Backyard Blaster - 10-10-2003 at 15:39

(In response to the post by vulture:)

Just because I don't have your level of knowledge or experience, is no reason to be so nasty. Personally I think I do pretty well for somebody who never studied chemistry.
Furthermore, I can assure you I DO use my brain and I take plenty of time to ensure such procedures are done correctly. But as humans we are not perfect, and we can only try our best and learn from the mistakes that we do make. I'm sure you yourself have made a mistake or two at some point....
I only posted this story to warn others of a danger - forgive me for trying to spare someone else of possible injury.

vulture - 11-10-2003 at 10:52

There's a big difference between having no knowledge, knowing what you are doing and expertise. I never said one should have chemical expertise to conduct experiments, but the fact that you neutralized your acid with a chemical that you are not familiar with demonstrates my point.

If someone would have told you to use KClO3 to neutralize acid and you didn't know what the reaction products were, what would have happened?

You should atleast have a MINIMAL knowledge of the chemicals you are using!!

[Edited on 11-10-2003 by vulture]

Backyard Blaster - 11-10-2003 at 15:29

I may not have known the chemical formula, but I've known for years (as does anyone with half a brain) that baking soda is used to neutralize acid. I also know that H2SO4 + KClO3 = NO2, so needless to say if someone had suggested this for cleanup, I wouldn't have believed it for second.
I don't know everything, nor do I pretend to. Thanks to you, I at least know the formula for sodium bicarbonate.....
If you must share your knowledge in the future, please do so more graciously.
Just my $.02

Mumbles - 11-10-2003 at 23:51

Quote:

Originally posted by Backyard Blaster
I also know that H2SO4 + KClO3 = NO2

Ok, first of all, that is in no way possible. There is not an atom of Nitrogen on the reactants side. That reaction actually forms a powerful oxidiser. Cl2O7 if I'm not mistaken. Even though it doesn't produce Nitrogen Dioxide, its still not a good idea to, so you at least got that part right.

If you're going to be experimenting, you have to aquire a basic knowledge. Baking Soda is extremely common as well. We're not asking you to remember the chemical formula to Teflon or Cellulose. Learn your elements, polyatomic ions, oxidation state, common compounds, monatomic ions, what to expect from some reactions. Most of that is learned in about a month and a half in basic chemistry.

Backyard Blaster - 12-10-2003 at 06:46

Originally posted by Backyard Blaster
I also know that H2SO4 + KClO3 = NO2

I realized my mistake shortly after submitting. I got KClO3 confused with KNO3. Even with KNO3, I'm not sure if such a mix would produce NO2 without some source of heat.
I think I'd better just keep my mouth shut rather than expose any more of my ignorance.........

vulture - 12-10-2003 at 07:20

I realized my mistake shortly after submitting. I got KClO3 confused with KNO3.

Then why didn't you immediatly edit your reply? There are more than 15 hours between your 2 replies...
Other than that, it can not be explained by a typo, where are the rest of the reaction products?

So, frankly, I don't believe you.

I sincerely hope you realize now that YOU are the one to blame for your experiment gone wrong.

Backyard Blaster - 12-10-2003 at 10:20

I didn't realize the mistake until after I'd gone to bed, and I wasn't about to go online at 1:00 a.m. just to avoid another lambasting from you.

Nevermore - 12-10-2003 at 15:13

Just my two cents about this matter:
first of all buy a periodic table, completed with valence of the elements, then start practice with some simple reactions, you will see that there are elements that easily displace others in some reactions, well those reaction are usually very common and useful: example H2SO4+2NaCl->Na2SO4+2HCl. Then start thinking that cloric, percloric, ipocloric salts are oxidants, manganic, permanganic too..is just common experience, you don't need to graduate in chem to understand those things. The remember most of the reactions give out lotsa of energy, so after you start them, they will proceed by their own, and if you dun take out the heat, the reaction will always get faster and faster.
H2O2 is a strong oxididizer, acetone is a flammable, i wouldn't mix them together before ensured that th heat produced could be absorbed by some ice bath, and i won't add any strong acid to it until it has reached a safe temperature.
You made a mistake with Ap this time, beside i really don't think that the compound exploded after being poured on the floor, since the heat was heavily passed to floor, and the reactants were not in a concentrated form but in a thin layer, anyway, if you made this mistake with something else at now maybe we won't even know.
Before playing with any chemical, open chemfinder, read all about that, open mdms read all about the hazard, then perform the reaction by your own on paper, not following any recipe, work with tiny amount, keep a big becker filled with ice cold water nearby where you can pour the mixture in case something starts to go wrong, and most of everything, add things dropwise unless you have been told not to do so.
Beware of NO2, i would fear it if i was you.

Mr.O-Nitrate - 17-10-2003 at 08:47

Just stay away from Ap....

KABOOOM(pyrojustforfun) - 18-10-2003 at 20:18

<blockquote>quote:<hr>I think I'd better just keep my mouth shut rather than expose any more of my ignorance.........<hr></blockquote>your best sentence under this thread. you're making joke outa yourself please STOP it.
if you knew properties of sulfuric acid you would doubtlessly test your acid and if it was conc you could dilute it with water. before starting the procedure.
you don't seem to know even highschool level chemistry but are doing experiments with unstable explosives ...

Backyard Blaster - 19-10-2003 at 06:44

Thank you so much for your constuctive criticism! As if I hadn't received enough already.
Yes, I admit I didn't know everything about sulfuric acid. But I can assure you I've always handled AP with the utmost caution, and the fact that I still have all my fingers despite having made dozens of batches of this stuff, is pretty good evidence......

wait a sec.....

Mr.O-Nitrate - 19-10-2003 at 10:21

I dont think its possible to dilute H2SO4 with water. It would just hiss and make a cloud of steam. Or can you dilute it with water?

Mumbles - 19-10-2003 at 10:42

Yes, it is possible to dilute with water. It is highly exothermic like you stated though. Its recomended to do it slowly and in an ice bath when starting from 98% Sulfuric. Remember to add acid to the water.

sulphuric acid

mick - 23-10-2003 at 06:24

er, is this a wind up
If you do not know how to dilute sulfuric acid then be careful with everything else you do.
In chemistry adding A to B is completely different from adding B to A, which one is safest in excess.
Try pouring a gallon of petrol on to a fire rather than adding the fire to the petrol.

Pure sulfuric acid boils at 330oC, density 1.84
H2SO4.H2O boils at 290oC, density 1.79
H2SO4.2H2O boils at 167oC, density 1.65
etc
Water boils at 100oC, density 1
Water + the above= lots of heat
So if you end up with a lower layer of conc sulfuric acid with water on top it is stable until you touch it.
Then the water does not just boil it vapourises with pressure, splashing the stuff every where. I have never heard off a successful blind practical chemist (a few fingers missing and scars OK).
When I have diluted conc sulfuric acid, I have added the acid slowly and carefully to stirred ice or ice+water (1 gram ice= 1 ml water) with external cooling, keeping my face well away, even with goggles on and I have only got cigarette burns on my clothes.

vulture - 23-10-2003 at 08:17

Cigarettes & chemistry = bad idea...

Not only hazardous in the lab, but as a chemist you should realize what toxic nasties it produces.

Hell, smoking a cig is worse for your health than being exposed to all sorts of chemicals in a lab using normal safety precautions.

You won't inhale any poisonous chemical fumes on porpuse, now huh? But you are doing it when smoking a cig...

palpy - 23-10-2003 at 08:42

Quote:

Originally posted by mick
I have never heard off a successful blind practical chemist

Well, this reminds me of a well-known case from my country:
Some guy and his friend were dismantling a WW2 hand grenade. It went off, the friend was killed and this guy lost his arm and was blinded. This happened in some late 1950s !!!
But the man has been regularly making AP to recent days. (BLIND! and ONE HANDED

). He damaged his house several times (cos he had been drying the AP on the hetaing!) and was also a few times arrested. And still he refused to stop making explosives...
I heard on the news some year ago, that he had finally lost his other palm, so I suppose he would stop at last.

These people are really dangerous...

dragora - 15-11-2003 at 01:10

i read somewhere that very pure ap i as low as sensitive as petn, it was a paper about analysyng remnants of explosives(forensic analysis)and ap leaves almost no remnants after detonation

AndersHoveland - 2-2-2013 at 16:35

Quote: Originally posted by Backyard Blaster

Actually, I throughly read the labels before I even bought the stuff. It only says "CONTAINS SULPHURIC ACID", and does not specify the concentration. I think it's a safe bet that it's at least 90% pure. I assume the red coloring, is to make spills easier to identify and clean up.

More likely it is of 30% concentration. "Concentrated" means different things depending on the context. In chemistry, "concentrated sulfuric acid" often refers to >97.5%, but for safety labelling it is usually much less. A concentration of 30%, with a red dye, is actually quite common for commercial and industrial purposes. I actually happened to find just such a bottle in a trash bin one time behind a supermarket. I am guessing a pool maintanence worker illegally dumped it there.

Simbani - 2-2-2013 at 16:56

nearly 10 years later..

AndersHoveland - 2-2-2013 at 21:02

Another reason for the exothermic reaction may have some relation to the fact that acetone can actually be slowly oxidized by hydrogen peroxide. This is much more rapid under alkaline conditions (sodium bicarbonate).
"The Journal of biological chemistry", Volume 35, (1918), p90-91

The explosion of acetone peroxide actually proceeds through a radical mechanism, so probably the vigorous decomposition of mixtures of acetone and hydrogen peroxide in solution is somewhat similar.

The decomposition products from acetone peroxide where studied in toluene solution heated to 173 °C. Various different products formed, including radical reactions with the solvent, but 85% of the acetone was recovered unoxidized.
"Thermal Decomposition Reaction of Acetone Triperoxide in Toluene Solution", Gladys N. Eyler, Carmen M. Mateo, Elida E. Alvarez, and Adriana I. Cañizo, (Argentina)
J. Org. Chem., 2000, 65 (8), pp 2319–2321

[Edited on 3-2-2013 by AndersHoveland]

chemrox - 2-2-2013 at 22:59

DO NOT BLAME THE LABEL YOU SNIVELING PANSY!
When you go fucking around with strong mineral acids and primary high explosives expect to get hurt and be appropriately cautious you twit. (I think he should be banned for not taking responsibility.)

Farnsworth - 2-2-2013 at 23:45

Quote:

go look for HNO3 at agricolture reseller, they use 55% conc for correcting the soil acidity adding NO3 at the same time, kinda cheap, 10 bucks for one gallon...

Anyone have more info on this? Google is returning bupkiss.

mayko - 3-2-2013 at 09:33

Glad you are okay, but eesh. I can vouch that the label might not give a concentration (mine doesn't) but a bit on sugar will confirm that it's the Hard Stuff.

It sounds like you might not have been wearing splash-resistant goggles? If not, they are like $1 at a hardware store. Find a place in your lab for them, print this out, and tape it next to that place.

It sounds like you might also have some lighting issues in your lab. Fix that before you do anything dangerous.

I second earlier posts on different rxns to be running at this point in your adventures. First off, is every chemical in your lab labeled? Go through and read the wikipedia page for each one and make your own label with information you think is important. Then, maybe start with some simple reactions. Heating sodium bicarbonate to form sodium carbonate is fun; the outgassing is kinda hilarious, and you get acid neutralizer as a product

Purifying iodine from povidone is pretty fun too. Are you keeping a notebook?

I didn't use H2SO4 at all until relatively recently, so I'd never got in the habit of "add acids to water, not water to acids". I was doing an iodine purification when I relearned that one. Volcanic indeed.

barley81 - 3-2-2013 at 10:12

H2O2 + H2SO4 makes piranha solution which eats up everything including acetone (atomic oxygen might be involved). It should be used very carefully because it's dangerously strong. I found a fritted funnel with a brown ugly stain that wouldn't come off with a night soaking in conc. H2SO4, but piranha solution made the frit fresh & clean in minutes!

This incident reminds me of one I found on the web at http://yarchive.net/chem/piranha_solution.html

Quote:

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.

[Edited on 3-2-2013 by barley81]

Fantasma4500 - 13-2-2013 at 11:29

you should never EVER use H2SO4 for synthesizing this compound as it heats up strongly, and will cause it to form dimeric in any way.. a tiny bit but you dont need much to set off as much as 1 kg..
never ever just proceed to pour in chemicals you dont know concentration of etc. another person was fooled to think a lab glass he bought was heat resistant glass, but it wasnt.. it was cheap chinese look alike pyrex, cost him 2 hands and perhaps even some more of his arm if im not wrong..

Ral123 - 13-2-2013 at 11:53

Safety is a state of mind. Quality glassware, reagents and avoiding organic peroxides is just an addition. H2SO4 for AP is super redneck. Don't do it unless you will triple recrystalise your product after. Only distilled/deionised water, nice reagents and cool to -10 before mixing. After mixing, put in freezer again. I'm pretty sure in April I'll report my 1 year old AP with no signs of decomposition(super dangerous trough).

Adas - 13-2-2013 at 12:18

Quote: Originally posted by Ral123

Safety is a state of mind. Quality glassware, reagents and avoiding organic peroxides is just an addition. H2SO4 for AP is super redneck. Don't do it unless you will triple recrystalise your product after. Only distilled/deionised water, nice reagents and cool to -10 before mixing. After mixing, put in freezer again. I'm pretty sure in April I'll report my 1 year old AP with no signs of decomposition(super dangerous trough).

I also have a few milligrams of pretty old TATP

It is more than a year old, but I don't remember when I set this sample aside. Maybe I will test the sensitivity soon.

Ral123 - 13-2-2013 at 13:56

Yes it's as sensitive as new HMTD. Tell us is it still nice crystals. Does it smell like medicine? If it's that old leave it to see how long will it last. How did you prepare it?

Adas - 14-2-2013 at 08:32

Quote: Originally posted by Ral123

Yes it's as sensitive as new HMTD. Tell us is it still nice crystals. Does it smell like medicine? If it's that old leave it to see how long will it last. How did you prepare it?

No, it still smells like a new sample. I tested the sensitivity right now, it doesn't seem to have changed. It was a standard preparation using tech. grade HCl and washed very well with water (I use old sock as a filter, very little particles pass through and water goes through like nothing).

Variscite - 27-5-2013 at 07:56

Were you even wearing eye protection?

amazingchemistry - 27-5-2013 at 20:21

My two cents with respect to safety:
First of all READ THE MSDS. All chemicals (even drain cleaners) are supposed to have one. Wear Eye protection at the very least, and appropriate gloves and lab coat if possible. Don't blame the literature for this accident. It is not the literature's purpose to advice you about safety.

Finnnicus - 27-5-2013 at 20:35

As we all know here, MSDS are not your ideal source of information, yes, it is a good rough outline to go off, but often wrong. I know from personal experience that particularly concentrations and other percentages are sometimes wrong. H2O2 which is clearly labeled 7% is 3% on the msds...

Moflo drain cleaner is labeled different as well.
Sorry for not pulling up links guys, I'll probably get shit for that.

killswitch - 28-5-2013 at 22:54

More protips:

The blue nitrile gloves you used in Wednesday's KMnO4 titration lab aren't any good against a mixed-acid nitration mixture. Wear LDPE gloves (the crinkly transparent kind that the Sams Club free sample people wear) over the nitrile for real protection.

If you are using a nitrate salt/sulfuric acid mixture to nitrate something, assume it is giving off nitrogen dioxide even if you can't see it. You don't need a reeking reddish-brown cloud of death to destroy your lungs; It's just faster that way. To convince yourself, leave an open container of strong ammonia water next to a container of mixed acid and observe the previously invisible deadly vapor become only slightly less deadly white fog.

If you are using store-bought cold-pack nitrate salts, recrystallize them first to prevent horrible side reactions that will render your product either useless or insanely dangerous. Blame the meth heads for the inconvenience.

Never put a nitrate salt in the microwave.

Even if you think your ammonium nitrate is dry, it probably isn't. Warm it up again until it partially deliquesces, then filter while warm and rinse with cold acetone, then blow-dry until the ketone smell is gone. Bake in the oven at 110 Celsius for another hour to be sure.

ParadoxChem126 - 29-5-2013 at 08:45

Quote: Originally posted by Backyard Blaster

Hopefully by sharing this experience I can spare someone else from perhaps serious injury.

Look at this thread for a serious disaster involving explosives (ETN).
http://www.sciencemadness.org/talk/viewthread.php?tid=22554