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Author: Subject: Had an acciedent.......
blip
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[*] posted on 7-8-2003 at 18:31


I once attempted distillation of MEK from nail polish remover in my microwave. :o After about 10 minutes on and off the glass bowl I used to condense the gas exploded and was heard a room away. Apparently it got superheated and shot out of the "boiler" cup so fast that it split the thing in half and splattered it all over my microwave. It's a turned out to be good cleaner and I knew the risks, but I'm so f'ing lucky it didn't combust. :o I'm not gonna take risks like that anymore!

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My hope too, is that there will be some chemistry student here I can interest in picking up a study I started a long time ago. It had great potential... the prof thought I had found a new type of chemical bond (and I've never seen any research in this area since), but due to circumstances beyond my control, I couldn't finish the research. Ah well. Cheers


Interesting, please explain. :)




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[*] posted on 7-8-2003 at 23:02


I usually pride myself on my clean glassware, but after trying to boil a few solutions that superheated... well, let us just say that there is such a thing as a healthy ammount of grime.

[edit - spelink]

[Edited on 8-8-2003 by Ramiel]




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JustMe
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[*] posted on 8-8-2003 at 08:36


Well, its off topic, of course, Blip... and I'm going on vacation tomorrow... so I'll just give an overview of the class of compounds I was studying.

My study involved Saccharin (yes, the sweetener), which is actually an interesting compound structurally. I was synthesizing transition element saccharin salts with the premise that saccharin could act as a chelating agent (i.e. form coordination compounds) with same elements. This would mean a new class of coordinating compounds not seen before.

So I prepared Saccharin salts of Copper (II and I), Cobalt (II), Iron (II), Manganese (II), Zinc, Nickel, Silver and even Palladium (interesting yellow cubic crystals on the last one). One piece of evidence in favor of my hypothesis was that Copper Saccharin dissolved in Acetone to form a deep green solution from which green crystals slowly separate, resembling Cupric Acetate. If you look up the structure for this acetate, two copper ions are bound by acetate bridges and I believe that Saccharin was doing something similar.

I found all sorts of neat chemistry going on, and I was able to grow large crystals of these salts.

Anyway, hope that answers your question. I may start another thread on this project only to see if I can interest somebody in picking up where I left off (in an academic venue)... or even just for fun if you can get the chemicals. Then I'll reveal some more of what I found out.

Cheers.
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[*] posted on 8-8-2003 at 09:34
First experience with superheating


One balmy day I was recrystallizing an amine salt in IPA. I wanted to reduce the volume of solvent after the first flush of crystals so I decided to boil it off on a hotplate. I turned the hotplate on and left for a few minutes. I returned much later than I should have and was surprised to see that much solvent still remaining. I dropped in a stirbar and was taken aghast by a supersonic whoosh sound and the flooding of the area by IPA. Definitely preferable to a sulfuric acid spill though.


DCM will shrink common soda bottle plastic too. Although I don't know the chemistry behind it (does anyone?), DCM in a soda bottle for a few hours makes for an interesting souvenier.
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Al Koholic
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[*] posted on 29-9-2003 at 18:35


Thick walled wine bottle + too much HCl + too much Al foil + plastic tubing of too small a diameter leading into a wash bottle = BOOM in your hand.
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thumbdown.gif posted on 23-10-2003 at 18:21
Had an acciedent.......


hi guys, i just thought i better tell you this to warn some of the less experienced about this. About a month ago i made about 80g of AP, the standard way with sulfuric. I have made it many times b4 with only one accident that could have been more serious (left AP in sun, detonated, blew concrete throught neigbours window...) So here i was with 80g, and decided to make some small detonaters. I used 1 inch copper tubes. I seperated probably about 1g AP and put it on a piece if paper, wich i was going to use to pour the shit into the tube. As i poured the stuff in, the friction in between the crystals and the paper caused by the ap running down into the tube, detonated. Luckily i was wearing a full face mask, thick clothing and industraial goves. I got 7 stiches on the side of my hip, from which they reomved a tiny but of copper, and 2nd degree burn to most of my palm and front if fingers. I am so lucky i did not lose any finger or have more serious burns. Ater this i quit dealing with AP after experiencing first hand, just how sensitive this shit can be.
BE CAREFUL, it may just save your life.....
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[*] posted on 23-10-2003 at 19:02
drat


It appears that malicious raccoons wrote part of the board software, because when I tried to merge this message with the thread "A cautionary tale" in Miscellaneous, XMB managed to totally screw up the old thread.

Anyway trichomegrower, if you're posting on a subject that already has a thread - like accidents we've had - please post in that thread.

[Edited on 10-24-2003 by Polverone]
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[*] posted on 23-10-2003 at 20:42


Well, I won't berate you as you obviously learned your lesson. Sorry you got hurt. Just remember people, hundreds of chemists smarter than you or I have been killed screwing around. So, if you don't want to die then don't make large amounts of these sensitive compounds. I know we all believe we are safe, but as you can see this field often leaves no room for error. Hell, most of the guys who died making these compounds died after years of experience. Sometimes we just need to be satisfied by only testing a little of the product. If you are in this game just for the thrills then sooner or later you are going to take a spill.



-A little bit of HNO3 is what I need; a little bit of KNO3 is what I see... Maybe I should just find a girlfriend to date instead?
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[*] posted on 24-10-2003 at 03:21


yes, very well said. I could have easily died as i was very much considering just loading all of it into a bottle and blowing it to hell, but "luckily" changed my mind. Who else has ever made AP that is that sensitive? what does it usually take for it to detonate? such as, pouring into a container, touch it, putting in sun, slightly heating etc.
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[*] posted on 24-10-2003 at 05:56
Incidents with HMTD


Did anyone ever have similar incidents with HMTD, i.e. unpredictable detonation etc? Or does anyone know someone who had?
In my experience, it always was very stable, and would not detonate by flame, it'd just deflagrate. Else it needs a hard, well-aimed hammer blow. Friction never seemed a problem, I tested it with very small amounts. THe only way I managed to set it off reliably, without confinement, was with a small amount of thermite...
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[*] posted on 24-10-2003 at 06:01


Yowtch! Good thing you were wearing safety gear, or else you might be lacking a couple of senses.....
Makes me a bit more nervous about AP, for sure. I've made tons of it over the years, even using it for detonators, and haven't had any such accidents.
Drying in the sun doesn't sound like a good idea. I've always dried mine in a cool, shady area, and I never use any kind of heat source to accelerate the process. I often test for impact and friction sensitivity, and it always seems to pass. The only reason I can think of, for your accident, is perhaps there was a high level of acid remaining in the product. Also, you didn't specify which acid you used; most literature I've read suggests that HCl yields a slightly less sensitive form of AP (dimeric).
Definately some food for thought there, and like many other posters/readers, I too would dump this stuff without a second thought, if I had access to a safer primary explosive.
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[*] posted on 24-10-2003 at 08:25


Dimeric or trimeric depends on the temperature. Dimeric is LESS stable than trimeric!

If you are stupid and smash some conc H2SO4 into your reaction mix you'll get mostly dimeric because of the hydration heat.




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[*] posted on 24-10-2003 at 10:37


Heh, I had not even thought about the dangers of Acid + AP when I came up with the crazy idea of making Chloroacetone by AP + Hydrochloric Acid. Fortunately, that was just a post- not an actual experiment. I have had my eyes on AP for a while, but not with much longing to make. To me, I see it more as 4th of July fun...and as a detonator for ANNM :) .

But you see, this is why I am afraid of explosives... They are too unpredictable for. The comparison has been made between them an a pet boa constrictor (I don't remember who made it, but it was very good): the boa constrictor has a one-track mind... He may love you all along, but then thinks, "gee, I like you so much I could just EAT you," and in line with the one-track mind, he does. The next day he thinks, "I sure miss that guy."

Explosives are the same way. Do not ever let yourself become complacent around something so unpredictable, and especially not as unstable as AP! As for me, I play the Violin and I use my hands a lot...I don't like the risk of losing fingers.


So, I will stick to my toxic materials- at least they are mildly predictable and won't explode on me :).
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[*] posted on 24-10-2003 at 13:34


A guy in my class is now in the mater hospital in dublin (A Children's hospital for seriously ill children) after an incedent with HMTD. He has lost sight in one eye and is fighting for his life in intensive care. Please, think about the risks before making organic peroxides.
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[*] posted on 25-10-2003 at 19:07
argh I really feel sorry for him


we all know how powerful HMTD is please tell how the accident happend. HMTD is not even comparable with AP. it doesn't sublime thus doesn't grow its crystal size. at room T decomposition is negligible but accelerates with T rise.
<table border=1><tr>weight loss %</tr><tr><td>temperature<br>hour</td><td>60°C</td><td>75°C</td><td>100°C</td>< ;/tr><tr><td>2</td><td>0.10</td><td>0.25</td><td>3.25</td></tr><tr><td>8< ;/td><td>0.35</td><td>0.60</td><td>29.6</td></tr><tr><td>24</td><td>0.5</td> ;<td>7.3</td><td>68.0</td></tr><tr><td>48</td><td>0.5</td><td>2.25</td><td& gt;decomp smell</td></tr></table>
deflegration point is 200°C !! (for AP it's about 100°C). impact sensitivity is 30% lower than mercury fulminate. I think with the following notes dialing with HMTD becomes reasonably safe.
1. use atleast 30% H2O2 or higher concentrations (but not very high)
2. for acid catalyzer use citric acid
3. at the stage when you want to let the soln T rich to room T stir vigorously for some hours (till most crystalls form)
4. instead of neutralizing with bicarb soln just wash several times with tap water and a last time with distilled water then 2 times with ethanol
5. make sure it's "completely" dry before use
6. keep in dry, cool and dark places
7. use immediately (it stores well though)
8. NEVER mix HMTD with anything
9. the most reliable method I have seen is the one on megalomania's site. needless to say the proportion of chemicals, durations, temperature... are very important
note: 1, 2 & 3 have effect on crystall size of the batch and as a resut on impact sensitivity




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[*] posted on 25-10-2003 at 19:54


Hmm, I just wondered how you judge reliability... for myself, I tend to take the data out of a book, or journal papers (simply because they wouldn't publish unless it was 100% reproducible). Always made HMTD according to COPAE, and never ever had a problem with it, and HMTD's properties were always reproducible :) --> a scientist's dream!

[Edited on 26-10-2003 by chemoleo]
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[*] posted on 6-11-2003 at 15:45
HMTD vs AP


In my dreams I have stored HMTD for over 12 mnths. Also dream about making it by the kilo and I always end up with a 90-95% yield I have never had an accident yet and would never even dream about making AP as HMTD has always safely fitted the bill with no differences in batch and it can be plasticised with a little patience. Large crystals forming in AP differences in one batch from another, forget that:)



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[*] posted on 4-12-2003 at 20:45


I'm trying to finish up my list of accident's that I've had during the course of my chemistry adventures and I've added it to my web site. It's good for a laugh

http://members.aol.com/bromicacid/mistakes.htm




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[*] posted on 4-12-2003 at 20:57


That was truly an epic tale of phosphorus production gone wrong, at the end. Did you ever make it go right?
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biggrin.gif posted on 5-12-2003 at 07:58


"Welcome to hell"... Indeed!
Anyway, have you used aluminium powder in excess and calcium phosphate?
Sodium phosphate would require much less heating to initiate, and bulk aluminium would be much more safer, the stochiometric amount wouldn't give aluminium phosphide (or so I think).
A tale of my own stupidity. It wasn't an accident, but it was stupid.
I made some thermite by wrapping anhydrous CuCl2 (the hydrated version said to decompose on heating, so dehydration is said to have be accomplished by heating in a stream of HCl gas... ...I heated it in a Pyrex flask over a candle :D , dehydrated nicely to a brown powder, which is the colour of anhydrous CuCl2 , this gives us all a lesson - don't trust the textbooks!) in aluminium foil. Then I heated it over a candle :D, IT IGNITED! it then burned with a brilliant white flame, and the stupid bit was that I was doing it INDOORS! The air filled with smoke, which I believe consisted of AlCl3 and Al2O3 - not healthy. I was holding it with tweezers - not even at arms length! Thank god the thing burned out before the flame reached the other end - the consequences for the tweezers would have been vile. I didn't think nothing of it at the time, though. :D:D:D
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[*] posted on 5-12-2003 at 11:23


Quote:

Anyway, have you used aluminium powder in excess and calcium phosphate?
Sodium phosphate would require much less heating to initiate, and bulk aluminium would be much more safer, the stochiometric amount wouldn't give aluminium phosphide (or so I think)


I used stoichimetric amounts according to the following reaction:

(NaPO3)6 + 10Al + 3SiO2 -----> 3Na2SiO3 + 5Al2O3 + 6P

Sodium hexametaphosphate was superior to other phosphates I have tried. Revisions of the reaction used straight aluminum powder where as the reaction I used in my mishap involved aluminum turnings with aluminum powder. Also, in further experimentation I used really fine sand (that I bought from chem supply company, fumed silica, 100 g was about .5 L in volume) and I improved my reaction vessel, put a screen over the end to diffuse bubbles and trap phosphorus from reaching the top. I plan to do more experimentation in the summer months, I will post detailed results when I get my yeild over 7%. I believe the aluminum phosphide was just because the reaction was nowhere near complete, if it went to completion it would have all been reacted away like you reconed.




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[*] posted on 22-9-2004 at 02:47
Sulphuric acid


Iv discovered that using Sulphuric acid to make AP makes it more sensative. despite they tempature.

Stick to Hydrochloric, I dont know why but it makes a difference!




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[*] posted on 22-9-2004 at 14:22


HCl evaporates off of the CTAP while sulfuric does not. So therefore when using sulfuric acid it stays on the crystalls which leads to increased sensitivity.

But a simple search could have solved your question on this.
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[*] posted on 25-9-2004 at 11:21
AP


TomThumb, H2SO4 also tends to increase the heat of the reaction. Higher heat
favors the less stable dimeric form of AP. So you're right - stick to HCl.




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[*] posted on 9-11-2004 at 07:02


Since you ask, I will relate to you my incident with HMTD, back when I was less interested in the "theoretical" and more in the "practical."

Was loading HTMD into empty .22 magnum casings using the TM-31-210 method (though not using the recommended safety equipment)

The contaminated casings, me being a little overzealous with packing pressure...possibly a few other factors contributed to the next few minutes of high drama, involving me with a dumfounded look on my face staring at a hole in the desk, wondering why my ears were buzzing and just where was all that blood coming from?

6 hours and 37 stitches later I was pretty much back to normal... except for the piece of metal that nearly took out my right eye. It's amazing what modern surgery is capable of - this was over 10 years ago though, so I'm sure the techniques have even improved since then.

I was lucky in that I survived and still have 10 fingers and 2 eyes, though the intraocular lens implant I needed to restore my vision kept me out of the military...the FBI... and a few other positions I aspired to later.

Ironically, I spend most of my day now reminding people to wear their eye-protection as an Industrial Safety Professional.

Life's a joker, no?
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