Sciencemadness Discussion Board
Not logged in [Login ]
Go To Bottom

Printable Version  
 Pages:  1    3
Author: Subject: First attempt at making WP + clusterfuck
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 13:24
First attempt at making WP + clusterfuck


Today my RP arrived! it is (was) a floury burgundy powder.
When I took it to my lab I tried to make WP. It went extremely well and I had lots of dark yellow blobs of it.
the reason that the WP on the pictures is such a strange shape is because The water was cold. after that I heated it and it melted.
That's where the good news ends.

here's the bad stuff:
I was transferring the RP from the big container (800g!!!) into a smaller one and the bloody thing just caught fire, it almost exploded! I figure it was WP contamination as it smelt of matches. I jumped back, dropping the bottle on the floor and table, that ignited and started making P2O5 smoke. I quickly got my CO2 fire extinguisher and tried putting it out, but it just spread the fire so I collected up my half burnt camera and coat and got out of there. just then my dad arrived. I closed the door hoping for the fire to burn itself out fast. but 20 mins later it was still on fire and the P2O5 smoke had filled the entire area so densely that I couldn't see my hand 1ft. in front of my face. Then I made a mask out of a wet towel, It worked quite well but then my dad wanted to go down and have another go with the fire extinguisher and wouldn't let me come so he took the towel and went down while I waited above the stairs I heard him walking, then I heard a clang, then the fire extinguisher spraying, then coughing and stumbling, then a thud and nothing so I raced down and found him lying unconscious on the stairs so I grabbed him and started pulling and apparently told him ''don't die on me'' but I don't remember, then he seemed to wake up and I half dragged him outside. the fire is out now and we talked a bit. his story was: he went down, fell over the fire extinguisher and lost the wet towel, the sprayed the fire and started coming back, but he was disoriented and ad to follow my shouting, then he says he doesn't remember anything until I shouted at him to not die.

That's the story, now I smell like matches and feel a bit sick, might be from all the adrenalin.
tomorrow I am going to ask for another bottle from the seller as mine is burnt up and it's his fault.

To recap:the synth. of WP went perfectly. the RP spontaneously ignited, there was no flame nearby and the only heat source was a 100* hotplate keeping some water hot The plate was actually 100*) What do you guys think caused it? WP contamination, friction (I had the 800g bottle over the smaller bottle and was geltly turning it to make it fall into the small bottle) or something else?


Endimion17, you must be proud coaching me to make such nice WP first time around! dark yellow, a little lighter than the glob you used in your video: phosphorus chemiluminescence and pyrophoricity. so thank you, hopefully there will be a little RP left over from the fire that I can distill while waiting for the thing from poland
WP.jpg - 181kB WP2.jpg - 162kB

[Edited on 8-4-2013 by Pyro]




all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
elementcollector1
International Hazard
*****




Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline

Mood: Molten

[*] posted on 8-4-2013 at 13:52


Well... that's... interesting. You might want to get you and your dad checked out by a doctor, phosphorus poisoning can be pretty nasty.
As for contaminants, I would imagine WP is not an issue (decays to RP upon exposure to light, if I recall).
Was anything destroyed in the fire?




Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
View user's profile View All Posts By User
Lambda-Eyde
International Hazard
*****




Posts: 856
Registered: 20-11-2008
Location: Norway
Member Is Offline

Mood: Cleaved

[*] posted on 8-4-2013 at 13:55


Holy tits, dude. That could have gone horribly wrong, it's good to hear you're both safe. I don't have anything else to add, really...



This just in: 95,5 % of the world population lives outside the USA
You should really listen to ABBA
Please drop by our IRC channel: #sciencemadness @ irc.efnet.org
View user's profile View All Posts By User
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 14:01


Well, It's not P poisoning, it's P4O10.
It came in a cardboard box wrapped in black plastic. and when I opened the bottle there was a strong WP smell.
I have no idea, last time one of us went even near the table he nearly died! you can't see a thing, I just left it until tomorrow.
Well, you can get phossie jaw from frequent exposure to P4, but i don't know about P4O10. Pulmonary edema might be a problem!

Any theories on the cause of the fire? I really think it's WP contamination




all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
Mailinmypocket
International Hazard
*****




Posts: 1351
Registered: 12-5-2011
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 14:08


I've never really handled much RP so I'm not an expert on its properties in person. Is there a possibility that the container it was in (or box) was of the type of plastic prone to creating static buildup? Again, I didn't think P was that sensitive to static, but perhaps finely divided dry material could be prone to ignition if you were to say, pour enough (800g) of it out and it developed enough charge to make a spark?

Glad to hear you are both okay though, wow.
View user's profile View All Posts By User
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 14:10


It was a HDPE container, and i didn't pour 800g, I poured maybe 50g before it went up in flames. I had half filled a 120ml packing jar



all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
Simbani
Hazard to Self
**




Posts: 50
Registered: 12-12-2012
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 14:22


WP contamination is very likely, due to the production method of RP. Ignition by friction can most likely be excluded, because you need more than a light tap to ignite RP.
I never heard of RP igniting in such a manner by itself, either. I would look for another seller in your case, where you can be sure to get a clean product.

Anyway, I´m glad to hear that you suffered no real damage, low amounts of phosphoric acid won´t kill you :) If you or your dad have to cough the next days there is a
chance of a pulmonary edema, maybe a doc won´t hurt.




View user's profile View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 8-4-2013 at 14:39


I got very uncomfortable reading your story. Burning P way out of control is a scary situation - I have flirted with this myself.

WP will spontaneously catch fire at room temperature in contact with air. I have seen it happen. I have not seen RP do this.

I'm so glad you and your dad are OK. Also, I admire your determination to not let this accident stop you.

I guess with bad actors like P one cannot do too much planning for worst-case scenarios.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 4048
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online

Mood: Semi-victorious.

[*] posted on 8-4-2013 at 14:41


I could have sworn I read a reference somewhere about having to treat red phosphorus carefully, as it has been known to spontaneously convert to white phosphorus, but I'll be damned if I can find it now.

Be careful- or we'll have to rename you "Pyrophosphate".




Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
View user's profile View All Posts By User
Endimion17
International Hazard
*****




Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline

Mood: speeding through time at the rate of 1 second per second

[*] posted on 8-4-2013 at 14:55


Acute poisoning is possible because phosphorus fires quickly bring down the partial pressure of oxygen to low values, so lower oxides are being formed, as well as lingering phosphorus fumes. If there was no light in the room, you could've probably seen a chemiluminescent fog in the room. Luckily for you, you've acted fast.
CO2 extinguisher won't help at all. It's just fanning the fires. Closing the container will help.

You could've easily been killed both, but it would be because of the suffocation and desiccant, acidic efect of the pentoxide upon your alveoli. A gruesome death indeed.
Do not return to the lab yet. Throw a dripping wet towel inside and close the door. Don't come inside for a few days. The towel will absorb the smoke and any lingering P vapors will oxidize. After that, put on a damp cloth on your mouth (very dry air in the room!) and slowly pour water into the container to cover it all up. There's probably more WP inside, and it would ignite if you poked it without water.
After that, ventilate the room and start with the cleanup. There'll be a lot of acidic residue all over the place.

Under different circumstances, I'd recommend you to press charges against the douchebag the seller, but you should keep a low profile. That's a lot of phosphorus, way more than I've ever seen with my eyes in my entire life, so yeah... Keep quiet and be thankful you're alive.

The motherfucker who sold you the vessel obviously got hold of industrial raw material. When RP is being made, it is made from WP and the conversion is never 100% over. There's a balance reaction.
That's why RP is being milled and boiled with lye, to remove nonconverted white allotrope.
I have no idea how the hell he got his hands upon something that's not even for sale. Maybe he bribed someone, or stole it from the chemical plant?

The ignition was a spontaneous combustion of WP. No static electricity. RP is always too damp for that to happen.
It obviously caught fire after being exposed to air for some time. You should've recognized the immediate huge danger you were in when you've opened the bottle and smelled WP, but now you know. Let this be a lesson for you and whoever reads this.

I hope you don't have any burns.

edit: a steel bucket filled with sand is a must in chemical laboratories. It's one of the first things I've obtained. If something is burning, you toss it into the sand. If there's a powder burning on the floor/desk, you cover it with sand.
Inert and very handy.

[Edited on 9-4-2013 by Endimion17]




View user's profile Visit user's homepage View All Posts By User
Endimion17
International Hazard
*****




Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline

Mood: speeding through time at the rate of 1 second per second

[*] posted on 8-4-2013 at 15:00


Quote: Originally posted by DraconicAcid  
I could have sworn I read a reference somewhere about having to treat red phosphorus carefully, as it has been known to spontaneously convert to white phosphorus, but I'll be damned if I can find it now.

Be careful- or we'll have to rename you "Pyrophosphate".


It does convert to WP, but there won't be any buildup of the material. It happens together with moisture, and the result is phosphoric acid and RP mud.
Of course, every sample of RP contains traces of WP, but what happened here was because the seller sold raw industrial material that needed to be processed.

RP is being sold in large drums and if it's processed, nothing happens.

Damn, this makes me so angry. Some people are so reckless, as long there's money involved.




View user's profile Visit user's homepage View All Posts By User
chemcam
National Hazard
****




Posts: 423
Registered: 18-2-2013
Location: Atlantis
Member Is Offline

Mood: I will be gone until mid-september, on a work contract.

[*] posted on 8-4-2013 at 15:09


What on earth do you need that much RP for? Sounds interesting if it is not for drugs. You are very lucky that the damage was not extensive. I too, would think WP was the culprit.



My YouTube Channel: ChemCamTV
IRC Channel: #sciencemadness @ irc.efnet.org
View user's profile Visit user's homepage View All Posts By User
Magpie
lab constructor
*****




Posts: 5939
Registered: 1-11-2003
Location: USA
Member Is Offline

Mood: Chemistry: the subtle science.

[*] posted on 8-4-2013 at 15:12


Quote: Originally posted by Endimion17  

I have no idea how the hell he got his hands upon something that's not even for sale. Maybe he bribed someone, or stole it from the chemical plant?


My brother used to live where phosphorus was being produced on an industrial scale. He said the workers would smuggle RP out of the plant in their lunchboxes. I guess you know what they wanted it for.




The single most important condition for a successful synthesis is good mixing - Nicodem
View user's profile View All Posts By User
Endimion17
International Hazard
*****




Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline

Mood: speeding through time at the rate of 1 second per second

[*] posted on 8-4-2013 at 15:30


Magpie, such occurrences are probably the main source of RP for drug makers and I'm surprised the security is not strict enough to prevent it.

Pyro, when the container bursted into flame, the worst thing you did was to jump back and drop the bottle. You should've been ready. All you had to do is to put it on the table or the floor and close it. I've prevented a similar accident from turning ugly when a dumb student shoved a spoon with bits of burning RP into the bottle. What you need to do is to close it immediately and cool the bottle with wet cloth. The bottles are often plastic so acting quickly is of utmost importance. If the plastic melts, and you don't have anything to cover it with (large steel pot, large glass beaker, bucket of sand), it's evacuation time.
When it cools down, never open the container at once. The rush of air might start a new fire. Just slide the cover and introduce water. Aerosol dispenser works great if you want to save the bottom half of the dry powder, because the upper part will be layers of acid, RP and WP that are difficult to salvage by inexperienced experimenter/technician.




View user's profile Visit user's homepage View All Posts By User
DraconicAcid
International Hazard
*****




Posts: 4048
Registered: 1-2-2013
Location: The tiniest college campus ever....
Member Is Online

Mood: Semi-victorious.

[*] posted on 8-4-2013 at 15:37


Quote: Originally posted by Endimion17  
Pyro, when the container bursted into flame, the worst thing you did was to jump back and drop the bottle. You should've been ready. All you had to do is to put it on the table or the floor and close it.


That's really easy to say, but anyone can be forgiven for panicking or reactive reflexively when the unexpected happens. We can't be expected to expect the unexpected all the time.




Please remember: "Filtrate" is not a verb.
Write up your lab reports the way your instructor wants them, not the way your ex-instructor wants them.
View user's profile View All Posts By User
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 15:39


Well Endi, I dropped the bottle when the thing caught fire in my hands, and then the spilt RP caught fire, it didn't burn in the bottle.
I thought of spraying in water when I saw the sea of white fumes, It was like rising water, rippling and running exactly like it.
I didn't throw in the towel, but it is very damp in there, I'm going back tomorrow to see if I can get in there to open a window.

My dad and I were discussing liability if the fire dpt. got called. I said it would be the polak's fault, he says it would be our fault. what do you think?

But how about the good part? what do you think of the distillation?

I am writing a mad letter to him asking for another bottle because this one caught fire in my hands, if he sends it I will top it up with water as soon as I open it, then dump in a beaker and boil I guess, with some KOH. 32 eur/800g is a super price!

I was incredibly fucking lucky! there was a huge burst of flames and I jumped back, dropping the bottle. my hands and all are burn free, my camera however, is fucked!

Yeah, we are getting sand tomorrow. and a bucket of water.

I am considering recuperating it, but haven't decided yet. I'll see how I feel tomorrow.

When I smellt the WP I had no idea how much dangerous it was. you and Woelen have warned me about it but I had no idea what WP smelt like (''Matches'' is not very accurate, it smells a little plasticky too) and thought that might be the norm.

Chemcam, I couldn't let a deal like that pass up! 800g/32 eur. even WP laced, it's worth it, I'll just boil it with KOH. all I want is to make WP and some P compounds.

Any idea why I feel so sick? adrenalin leftovers? or poisoning?




all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
elementcollector1
International Hazard
*****




Posts: 2684
Registered: 28-12-2011
Location: The Known Universe
Member Is Offline

Mood: Molten

[*] posted on 8-4-2013 at 15:54


Quote: Originally posted by Pyro  
Any idea why I feel so sick? adrenalin leftovers? or poisoning?

Adrenaline doesn't stick around for 2 hours; SEE A DOCTOR!




Elements Collected:52/87
Latest Acquired: Cl
Next in Line: Nd
View user's profile View All Posts By User
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 8-4-2013 at 15:59


too late now, it's 2AM. I'll go tomorrow if i'm sick.
adrenaline might not, i thought it might be an aftereffect




all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
Endimion17
International Hazard
*****




Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline

Mood: speeding through time at the rate of 1 second per second

[*] posted on 8-4-2013 at 16:16


Quote: Originally posted by DraconicAcid  
That's really easy to say, but anyone can be forgiven for panicking or reactive reflexively when the unexpected happens. We can't be expected to expect the unexpected all the time.


Nobody expects the Spanish inquisition, either.

After all, it's 0.8 kg. Enough to make anyone squeamish.


Quote: Originally posted by Pyro  
Well Endi, I dropped the bottle when the thing caught fire in my hands, and then the spilt RP caught fire, it didn't burn in the bottle.
I thought of spraying in water when I saw the sea of white fumes, It was like rising water, rippling and running exactly like it.
I didn't throw in the towel, but it is very damp in there, I'm going back tomorrow to see if I can get in there to open a window.

So the last time you saw the bottle, it was not burning, but - where is it? If it's somewhere in the lab, opened, it's a ticking time bomb. If you find it undamaged, close it and put it in a steel sand bucket.


Quote:

My dad and I were discussing liability if the fire dpt. got called. I said it would be the polak's fault, he says it would be our fault. what do you think?


If you want your father to stand before a judge in a court, accused of negligence of a minor, go for it. That's probably what would happen.


Quote:

But how about the good part? what do you think of the distillation?

Knowing how easy it is to suffocate that fire just by closing the cap, and the fact it won't catch fire immediately, I'd use a spoon and transfer the stuff (without dispersion) in smaller bottles while the original is in a steel bucket, partially buried in sand, where it should remain sitting. But that's me, and I have experience with it.

It can be used for the conversion, but the risk of it spontaneously catching fire is known only to you. I can't really evaluate the risk without knowing exactly how does the thing behave.


Quote:

I am writing a mad letter to him asking for another bottle because this one caught fire in my hands, if he sends it I will top it up with water as soon as I open it, then dump in a beaker and boil I guess, with some KOH. 32 eur/800g is a super price!


Good luck with the purification. Don't do it all at once.


Quote:
I was incredibly fucking lucky! there was a huge burst of flames and I jumped back, dropping the bottle. my hands and all are burn free, my camera however, is fucked!


I still don't understand why would it would make a huge burst. You should've used a spoon. Transfering dusty, flammable material by pouring it through air is not a smart idea. Maybe you're responsible for the ignition. If there was a hotplate near you, and RP aerosol is lingering around... Maybe you've caused some friction, too.
I don't know. I'm not a CSI "genius".


Quote:

When I smellt the WP I had no idea how much dangerous it was. you and Woelen have warned me about it but I had no idea what WP smelt like (''Matches'' is not very accurate, it smells a little plasticky too) and thought that might be the norm.


Realistic RP samples smell. That's fact. If the smell was very intense and there were visible fumes upon opening the container, that would've give me a strong clue that shit is about to hit the fan.


Quote:
Any idea why I feel so sick? adrenalin leftovers? or poisoning?

What does it mean "feeling so sick"? Nausea? Fear? Vertigo?
If your father, being exposed a lot more, lacks the symptoms, it's probably anxiety. Get it? Probably.
Adrenalin rush doesn't last more than a couple of minutes.

How long have you been in the pentoxide atmosphere? Have you been holding your breath?
Did you take a shower? Do you still smell like matches? Does your breath smell?

Again, I can't evaluate this because there isn't enough info. If you feel sick, go to the doctor. "I was playing with Chinese fireworks, big bada boom", standard story.

[Edited on 9-4-2013 by Endimion17]




View user's profile Visit user's homepage View All Posts By User
S.C. Wack
bibliomaster
*****




Posts: 2419
Registered: 7-5-2004
Location: Cornworld, Central USA
Member Is Offline

Mood: Enhanced

[*] posted on 8-4-2013 at 16:32


I imagine there aren't many manufacturers of RP who sell product that ignites in air, in the last hundred years that is.

BTW even RP with no WP but gets wetish can generate PH3. Some RP is treated to slow this down.

[Edited on 9-4-2013 by S.C. Wack]




"You're going to be all right, kid...Everything's under control." Yossarian, to Snowden
View user's profile Visit user's homepage View All Posts By User
plante1999
International Hazard
*****




Posts: 1937
Registered: 27-12-2010
Member Is Offline

Mood: Mad as a hatter

[*] posted on 8-4-2013 at 16:35


I talk with pyro via another mean then the forum, and he told me as dad was having good problems with his lungs...

I do think it is pyro's fault, since like S.C said, nobody want to sell spontaneously flammable material that make toxic fumes... Especially that I never heard of spontaneous RP combustion...




I never asked for this.
View user's profile View All Posts By User
Endimion17
International Hazard
*****




Posts: 1468
Registered: 17-7-2011
Location: shores of a solar sea
Member Is Offline

Mood: speeding through time at the rate of 1 second per second

[*] posted on 8-4-2013 at 16:50


Quote: Originally posted by S.C. Wack  
I imagine there aren't many manufacturers of RP who sell product that ignites in air, in the last hundred years that is.


Unless it has been stolen from a factory. Even then, it wouldn't come as powder. Freshly made RP is a gunky mess that easily cakes up. There's enough WP inside to probably cause weak glowing, fuming and spontaneous combustion.
After it's processed, washed and dried, it's fluffy and dry if kept away from humidity. It doesn't catch fire just by itself. If left exposed to air, it will eventually turn into acidic goo, but it takes a long, long time. Months.

There's something wrong with this story. I do think it's probably his fault, though I can't be sure.


Quote: Originally posted by plante1999  
I talk with pyro via another mean then the forum, and he told me as dad was having good problems with his lungs...


"Good problems" as in "heavy problems"? That might be oedema forming. It's a medical emergency...


Quote:
I do think it is pyro's fault, since like S.C said, nobody want to sell spontaneously flammable material that make toxic fumes... Especially that I never heard of spontaneous RP combustion...


That's simply not true. :)




View user's profile Visit user's homepage View All Posts By User
plante1999
International Hazard
*****




Posts: 1937
Registered: 27-12-2010
Member Is Offline

Mood: Mad as a hatter

[*] posted on 8-4-2013 at 17:10


yes, as heavy problems... Well, for some money I guess, but he would be better to warn that it spontaneously burn making toxic fumes. At least I would warn if I were to sell something like this.



I never asked for this.
View user's profile View All Posts By User
Pyro
International Hazard
*****




Posts: 1305
Registered: 6-4-2012
Location: Gent, Belgium
Member Is Offline

Mood: No Mood

[*] posted on 9-4-2013 at 05:58


Well, I held my breath most of the time or breathed through a damp cloth, but got a few big lungfuls while dragging him up the stairs. now I feel fine, must have been anxiety.

to clear up on the ''pouring'' thing, I held the neck of the RP bottle just above the neck of the empty bottle, and was gently turning it to make the powder fall into the smaller bottle. I have no idea how big the burst came to be, It was right in front of me, so maybe it wasn't that big. the hot plate was maybe 1m away.

The smell might of been intense, but that was the first time I had smelt WP so I had no idea how strongly it smelt. there was no fuming.

I don't see how this might be MY fault Endi.

I feel fine now, he has a little pain breathing. I might go check today to see if the smoke has settled, otherwise i'll check tomorrow.




all above information is intellectual property of Pyro. :D
View user's profile View All Posts By User
Mixell
National Hazard
****




Posts: 449
Registered: 27-12-2010
Member Is Offline

Mood: No Mood

[*] posted on 9-4-2013 at 07:50


Was your RP Polish by any chance?
View user's profile View All Posts By User
 Pages:  1    3

  Go To Top