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Author: Subject: First attempt at making WP + clusterfuck
Endimion17
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[*] posted on 11-4-2013 at 12:05


So now he'll be transfering 400g out of its original bottle. It would be ironic if it bursts into flame. :D

Pyro, when you get your sample, use a spoon and take a detailed macro photo of the sample. Look for any evolving fumes against light.




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Pyro
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[*] posted on 11-4-2013 at 12:18


I hope he'll send me a new one! that would be very ironic!

I was hoping to pour on water as soon as I opened it! I really hope your right and he'll send me a replacement

[Edited on 12-4-2013 by Pyro]




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[*] posted on 11-4-2013 at 12:20


Use a long spoon so you can take out some without picking up the bottle (you can't drop it if it's not being held). Put the lid back on the bottle ASAP.

Or, as you say, dump it into some water as soon as you get it.




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Endimion17
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[*] posted on 11-4-2013 at 12:30


Nah, don't pour water in. What if this batch is ok? You wouldn't want to ruin it.
Take a long glass rod (or a thickwalled tube) and flamework it into an almost vertical spoon, and let that be your way of removing the substance from the container.
When opening the cap, unscrew it and then slide it away, slowly, keeping in mind that you don't want to grind the cap against the neck as it might be dangerous. Don't open it by lifting the cap to avoid mixing the air inside, which is possibly deoxygenated, with outer atmosphere.
Before opening, gently tap the bottle against the ground to ensure compactness of the powder.

Try to recreate your accident using small batches.
I wouldn't pour water inside just because something happened with the last bottle. It's much too valuable.

Inspect the neck and the cap's inside screw for the powder remains. Remove it with a damp cloth if there's any.




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[*] posted on 11-4-2013 at 12:43


Quote: Originally posted by Endimion17  
Nah, don't pour water in. What if this batch is ok? You wouldn't want to ruin it.

I didn't think red phosphorus would react with water. White phosphorus is generally stored underwater, isn't it?




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[*] posted on 11-4-2013 at 13:02


I would pour water into the container ASAP after I opened it and would not pour the contents into water.

The stuff may have a tendency to float on top at first from air bubbles caught between particles.
Then I would close to cap and gently swirl it to dislodge the air particles and let the RP settle to the bottom.

The water will not hurt it at all and can easily be removed under vacuum




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Pyro
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[*] posted on 11-4-2013 at 17:43


I think Endi means it would be wet. I'll take a scoop out for you guys when it arrives!
tomorrow: lime spreading on the floor and salvaging of RP

I only just noticed I have become an international hazard! doesn't seem fitting, it's more like hazard to self and family! Next time it will be inernational! don't worry! :D




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[*] posted on 12-4-2013 at 02:19


This does not sound good at all. I do not agree with Endimion17. Why would this batch be better than the previous one? This seller just could get his hands on a huge pile of red P (tens or maybe even hundreds of kg) and I seriously doubt that the picture he shows on eBay is from his batch he is selling. He simply repackages from bulk into bottles of 800 grams and does this to stay just under 1 kg for shipping. He also sells 400 gram bottles and even 3 kg packages. As pyro writes, he wraps his 800 grams bottles in thick black tape before packaging it. He also sells 900 grams of NaNO2 in exactly the same type of plastic bottles (I have one of these, I ordered NaNO2 from this seller) and these are not wrapped in thick plastic tape, so he can sell 900 grams of NaNO2 in order to just stay under 1 kg total weight.

I would open the bottle in a bucket of water, under the water surface and SLOWLY let some water run in and allow bubbles of air to escape, while the cap is still loosely screwed on the bottle. SLOWLY, because otherwise when all water at once gulps in, it may cause a big bubble of air to escape with a large amount of the contaminated red P as a dust cloud and a possible tremendous flame! BE CAREFUL!!! Keep in mind that all this hassling around with crappy red P is not worth risking your health or even risking your life or your family's life!

This seller does not know very well what he is selling. He sells red P with a high white P content, period! Of course he did not add contamination himself, but he does not know enough of the chemical he sells and that the manufacturing process inherently may introduce a lot of contamination. For such low prices you can't expect good quality, but low quality should not be the same as insanely dangerous. I purchased his NaNO2 (which is less than EUR 4 per 900 grams) and do not expect it to be very pure, but it is not dangerous and is good enough for certain synthesis reactions (e.g. dyes, organic nitrites). Exactly the same I would expect with his red P.

[Edited on 12-4-13 by woelen]




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Endimion17
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[*] posted on 12-4-2013 at 05:02


But Pyro's RP ignited when he poured the powder through the air. The surface available for the reaction was huge.
I'm almost sure nothing would happen even if he took a spoonful of the powder (of course, Pyro, don't transfer a spoonful at a time) and placed it on a flat surface. Even if it ignites, it won't be soon, and it won't be spectacular. RP fires are calm.
The fireworks he was were because of the "powderfall" from the main container which then ignited when fell from his hand.
One of the things that contributed is tilting the container. If it sits upright, and there's no wind, the fresh air doesn't enter by convection.

Before making attempts to make RP wet (it just delays the problem - WP is still inside) and thus subscribing to more tedious work in the future, I'd make few experiments. I'd try to cause an accident in a controlled condition, with small batch (cubic centimetre at most). I'd test for WP by observing fumes and glowing.

In the unlikely event of the upright container catching fire when picking up RP using a vertical spoon, water aerosol dispenser would take care of it. When RP catches fire in a container, it creates an area of pentoxide aerosol and oxygen depleted air which sits above it. Unlike flat surface fires, this one isn't spectacular. I've seen it and dealt with it. Its heat output is poor, so it takes like half a minute or more to seriously weaken the plastic container. It's more like smouldering.
Gentle sprinkle of water and closing the cap extinguishes it for good.

Submerging the container in a bucket of water and opening the cap might send up a fireball, as woelen said. I wouldn't do that.
The only RP available to reaction is the topmost layer. Nothing below will burn. The fire won't spread throughout the material, therefore water aerosol dispenser is enough.

If, after controlled testing, the material proves to be highly contaminated and pyrophoric, I would add enough water to cover it, and then process a small batch using lye to remove the contamination. But that's just me.

Someone mentioned wetting the powder and removing water using vacuum before using it. Baaaaaad idea. I'd say that would make it even more pyrophoric.

[Edited on 12-4-2013 by Endimion17]




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[*] posted on 13-4-2013 at 12:30


Be aware! When you want to purify it with NaOH solution, it produces phosphine which may even kill you! I wouldn't try this for safety's sake..



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[*] posted on 20-4-2013 at 12:11


Cleanup session finished.

I spread slaked lime on the floor to remove acid traces. later I am going to brush it up and whitewash the walls.

The sliding door of my scales was open and H3PO4 got in! but It hasn't visibly corroded anything. I just hope it hasn't gotten in the mechanism. That's the pan, you can see all the H3PO4 on it, it's that thick everywhere.

All the gloves in the top of the box are covered in H3PO4 and smell a little strange, I just tripled them and used them to clean up.

I put water in the brown bottle the I was pouring the P into and it warmed up a bit (P4O10 I guess) and then I smellt REALLY strongly of P4 so I put it on the floor and buried it in slaked lime to make combusion impossible.

My boat that was inthere to keep it fry because all the varnish was striped off now has H3PO4, any idea if this is bad for it? I calculated there ust be a bit more than 2,5kg's H3PO4 there!

quick question:there is no shortage of water vapour in my lab, it's next to the river and the floor is below the water level. how dilute does H3PO4 become before it isn't hygroscopic anymore?

H-80 1.jpg - 152kB




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[*] posted on 21-4-2013 at 06:38


I think your scales have been filled with aerosol. You might want to do something about it.

The bottle got warm because of concentrated phosphoric acid, not because of the pentoxide. Solid pentoxide detonates if you pour water on it.
Now that you've got a shitty, toxic and flammable gunk inside the bottle, you should go to an open field, pour it all out and light it on fire. Step away from it and wait. Occasional poke with a stick is needed to expose every piece of WP. Then cover it with dirt or bury it in a shallow pit. There will still be residual WP/RP, but that will oxidize over the time to form phosphates.
You need to give plants phosphates. Plants love phosphates. (see what I did there? :D)

I don't know what will happen with your boat. Phosphoric acids reacts with cellulose. Higher concentration and temperature increase the rate of this reaction. It's like a phosphorilation inside biological systems, only there's no enzymatic catalysis that makes it spontaneous at physiological temperatures, pH and concentrations.
Wash your boat thoroughly with water. I meant to ask if you've got a drain, but then I've realized the floor is below the river water level.




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[*] posted on 21-4-2013 at 11:43


Buying things from an eBay seller who sells 'empty bottles, nudge nudge, wink wink, know wov I mean?', especially potentially dangerous ones, isn't really smart IMHO...

[Edited on 21-4-2013 by blogfast25]




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[*] posted on 22-4-2013 at 14:17


Well blogfast, it's not about safety, it's about money :)

Endi: My dad went to his local pharmacy and she apparently knew everything about WP and the treatment of it. Since they used WP in both WWI and WWII and there was heavy fighting in Belgium they have included it into medical training!
I am going to open them up and see if i has gotten into the mechanism, If it has I will have to send it back to Mettler Toledo. (Or perhaps a watchmaker could do it)
I was hoping to be able to recover it to convert into WP. how about washing it in CuSO4 to make the present WP a little more inert so I can remove most of the moisture?

soon I need to sweep up the slaked lime from the floor, I think it will stay white for a long time :) hope the owner's ok with it! :D

and thanks for all the help




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[*] posted on 23-4-2013 at 05:16


Money??? You don't think it was a bit of a false economy, to say the least?



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[*] posted on 23-4-2013 at 10:26



Quote:

Someone mentioned wetting the powder and removing water using vacuum before using it. Baaaaaad idea. I'd say that would make it even more pyrophoric.



Don't know why you say that. Only a complete moron would regass with
oxygen. The norm is nitrogen or argon.
Alternatively, you could use KOH or P2O5 to dehydrate, but that'll take a millennium....

In Any case, there is WP in that product. IT NEEDS TO GO UNDERWATER!




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[*] posted on 23-4-2013 at 11:31


Quote:
Quote: Originally posted by Maya  
Someone mentioned wetting the powder and removing water using vacuum before using it. Baaaaaad idea. I'd say that would make it even more pyrophoric.



Don't know why you say that. Only a complete moron would regass with
oxygen. The norm is nitrogen or argon.
Alternatively, you could use KOH or P2O5 to dehydrate, but that'll take a millennium....

In Any case, there is WP in that product. IT NEEDS TO GO UNDERWATER!


It's a bad idea because it would probably leave WP deposited in activated, surface phase. WP is soluble in water, though poorly, but under normal circumstances that's not important because it oxidizes quickly.
Wiki can sometimes be terribly incorrect. It says it insoluble, but its solubility is 2.4 mg/L (Spanggord et al. 1985), or 3 mg/L (Stich 1953). I'll have to correct that.
If it was insoluble, water covering WP wouldn't smell and wouldn't give off fumes at certain conditions.

Who ever mentioned regassing with oxygen? I think you meant to say air? Introducing oxygen could lead to violent reaction. Air would probably cause a spontaneous ignition in the form of smouldering.
Anyway, introducing air to an evacuated vessel with probably weakly pyrophoric material (weakly because it obviously takes some time and air dispersion, unlike some organometallic compounds) is a stupid idea, but it's something most people would do because they either don't know enough chemistry, lack laboratory skills or simply don't have inert gases available.




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[*] posted on 24-4-2013 at 03:58


Ok, I got this as my last message from the tracking of the phosphorus, I'm woried by the translation by google translation.

Wyslanie przesylki z polski

Does anyone can translate to english?

Thanks




I never asked for this.
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[*] posted on 24-4-2013 at 04:05


plante, that's off topic! try google translate.
dispatch charges of polish...

tips on making the P4 less reactive while handling that bottle of crap to make it useful for WP?




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[*] posted on 11-1-2019 at 02:09


Pyro probably does not read your message anymore. This is 6 years ago. I mentioned this thread in the other thread on buying red P in the EU, just as a warning. Not all red P is safe. Stuff, which is highly contaminated with white P is very dangerous. Some bad sellers, however, sell this as 99.9% or so purity of phosphorus. Technically they are right, it indeed is very close to 100% phosphorus, but it is not close to 100% red phosphorus!



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