Author Topic: Red Phosphorous  (Read 452 times)

Tsathoggua

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Re: Red Phosphorous
« Reply #20 on: May 20, 2011, 12:15:48 AM »
What about say, silicon nitride, or other nitride refractory ceramic? they use some of those for the likes of coatings on fighter jet turbine blades, and missile engine parts, they are about as refractory as one can get.

Even glassy carbon might, I say MIGHT do it, although attack isn't an impossibility. But it is available in the form of crucibles etc, and is extremely resistant to heat, in fact, they use it for the heat-shields of space vehicles to protect from the scorching heat of reentry into the earths atmosphere.

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Sedit

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Re: Red Phosphorous
« Reply #21 on: May 20, 2011, 12:51:49 AM »
The nitrides will more then likely absorb the MW energy simular to how Ammonia does. Microwaves are very close to the atomic resonance frequency of the Nitrogen atom which is the reason why the first laser ever made known as a maser was constructed using Ammonia and exciting it. It produced a coherent beam in the MW spectrum.

Glassy carbon will have the same issue, all the Microwaves will be absorbed and will never reach the reactants meaning the required temperature will rise alot higher. It will be akin to heating it with a conventional burner instead of the molecular penetration that Microwaves will have stimulating each and every bit of carbon in the mixture.
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Tsathoggua

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Re: Red Phosphorous
« Reply #22 on: May 20, 2011, 01:41:18 AM »
Buggrit, I should have realised that former point.
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Shake

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Re: Red Phosphorous
« Reply #23 on: May 20, 2011, 02:48:58 AM »
so a chinese food container wont do? damn.. how about a microwave safe dish? ;)

i think all roads are pointing to ceramics..

what sort of carbon? like any?

dust mask filters they are loaded with it
« Last Edit: June 03, 2011, 07:55:19 AM by Shake »

Tsathoggua

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Re: Red Phosphorous
« Reply #24 on: May 20, 2011, 02:51:22 AM »
Charcoal should do the trick. Activated charcoal as found in a pharmacy (albeit in capsule form usually) for settling stomachs (I think, although its also used for detoxification following ingestion of toxic substances) should be idea, it has a very large surface area.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Sedit

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Re: Red Phosphorous
« Reply #25 on: May 20, 2011, 03:47:01 AM »
Check out the fish store for activated charcoal.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

salat

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Re: Red Phosphorous
« Reply #26 on: May 20, 2011, 11:52:17 AM »
I think the gas is needed - it may be to keep the phosophorus from igniting.

And ya'll got the microwave stuff wrong - it has to do with the polality and dialectric constant of the materials.  Please read at least the basics before you try this. 

Hot flying phosphorus does nasty stuff to your skin.

Salat
« Last Edit: May 20, 2011, 11:56:17 AM by salat »
Salat

Sedit

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Re: Red Phosphorous
« Reply #27 on: May 20, 2011, 01:03:22 PM »
The polarity of the molecule has alot to do with why it resonates at the Microwave frequency Salate but in the end the amount of energy imparted to the molecule has to do with if it resonates in a frequency close to that of the microwave frequency. However the polarity of the material has alot to do with its resonance frequency so if you want to get technical im sure there is formulas written to explain it mathmatically as a derivative between the dielectric constant and its polarity.

Take the Ammonia hydroxide and water experiment as an example. Both solutions are mostly water which is indeed polar yet the one with a small percentage of ammonia in solution will boil in a matter of second where water takes much longer.

Quote
The ammonia molecule readily undergoes nitrogen inversion at room temperature—that is, the nitrogen atom passes through the plane of symmetry of the three hydrogen atoms. A useful analogy is an umbrella turning itself inside out in a strong wind. The energy barrier to this inversion is 24.7 kJ/mol in ammonia, and the resonance frequency is 23.79 GHz, corresponding to microwave radiation of a wavelength of 1.260 cm. The absorption at this frequency was the first microwave spectrum to be observed.[14]
Source: http://www.newworldencyclopedia.org/entry/Ammonia

14.? C. E. Cleeton and N. H. Williams, 1934 - Online version; archive. Electromagnetic Waves of 1.1 cm Wave-Length and the Absorption Spectrum of Ammonia. Received December 21, 1933. URL last accessed May 8, 2006
« Last Edit: May 20, 2011, 01:07:38 PM by Sedit »
There once were some bees and you took all there stuff!
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salat

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Re: Red Phosphorous
« Reply #28 on: May 20, 2011, 02:30:18 PM »
Here are a few points that may have been missed in this reaction:

(a) heating a mixture of phosphoric acid and a particulate carbon reductant with microwave radiation in a nonoxidizing atmosphere;
(b) evolving a phosphorous vapor from the mixture;
(c) condensing the phosphorous vapor to form condensed acid.


The gas flow sweeps the phosphorous vapor along with emitted gases from the reactor into phosphorous recovery system.

The flow of gas is controlled by flow meter
The reactor, a quartz tube 16 mm inside diameter and 610 mm in length, was placed in the

Nitrogen gas at a rate of 500 cm3/min was passed through the reactor during exposure.

Temperature range for this reaction is 600 -1200 C.

So teflon and glass are both out as reaction vessel materials.

My husband said if you can find a heating element in a quartz tube that might work, but you're going to have to figure out  a way to get gas tight fittings on it. And figure out what level of pressure is safe.  The water in the acid will turn to steam first so that will come out right away. 

There was a really cool website that exaplained this stuff in language I underststood - my memory just isn't ver good right now so I have to constantly reteach myself stuff.

Salat
« Last Edit: May 20, 2011, 02:34:44 PM by salat »
Salat

Tsathoggua

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Re: Red Phosphorous
« Reply #29 on: May 20, 2011, 08:12:43 PM »
Yes Salat, just to confirm that, regarding toxicity of WP, it is EXTREMELY toxic, the lethal dosage is quite low...
http://emedicine.medscape.com/article/833585-overview#a0104 to quote 'as little as 15mg has caused death'

Nasty stuff, I had the rather nasty experience of being burnt by willy pete as a kid, a very small exposure, a few mm wide bit of burning WP got itself on my wrist, during distillation of the stuff, hurt, obviously, but that wasn't really much concern compared to what happened later. My arm went weak as a newborn, little coordination in my affected fingers/hand, the effects stayed localised, but damn...I couldn't hold a pen, or write with my affected hand, and it was as if all the physical strength had just drained away. Effects were limited in duration, but lasted long enough to be a real inconvenience, and pretty unnerving to boot. I forget exactly how long now, as I was just a lil'un really at the time, but at least a week, I think, a little longer, but probably not two.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Balkan Bonehead

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Re: Red Phosphorous
« Reply #30 on: May 21, 2011, 02:19:44 AM »
No to phosphoric acid and carbon. Yes to sodium hexametaphosphate, aluminum powder/turnings and SiO2, over a small charcoal fire, preferably one with a fan serving as bellows. Don't fuck with microwaves. Read the thread on science madness for fuck's sake. People have actually done this successfully.

Shake

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Re: Red Phosphorous
« Reply #31 on: May 21, 2011, 06:03:59 AM »
i know what they are doing over there, with the blowtorch or the hot coles, have they tried this? i dont have sodium hexametaphosphate. What if this works?

Sedit

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Re: Red Phosphorous
« Reply #32 on: May 21, 2011, 04:23:19 PM »
Sodium hexametaphosphate can be had easy, matter of fact I can get it much cheeper and simpler then getting H3PO4 concentrated. I have tried this and managed to make a small amount of WP but I have small balls and have not scaled it up yet. Capturing WP on a small scale is a chore in itself.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

Shake

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Re: Red Phosphorous
« Reply #33 on: May 21, 2011, 04:43:11 PM »
H3PO4, hardware, in the section near the tiles chemicals. Like the acid washes are there ect. If you read the labels it says like 80% phosphoric acid.. Ill take another look. the clean ups are on meaning everyone is chucking rubbish out the front, there are microwaves galore on these things.

yesterday i came across a clean up i shit you not, a full photo lab.. microscopes, flasks and funnels, measuring cups and tubular measuring thingos.. tubs.. a few chems, i dug so fuckin hard begging to find a big jar of pdcl2.. the old guy had obviously died.. i was searching his stuff thinking fuck me what are the chances


what you mean u tried this?  with the microwave?? lol
« Last Edit: May 21, 2011, 04:45:41 PM by Shake »

salat

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Re: Red Phosphorous
« Reply #34 on: May 21, 2011, 04:56:24 PM »
I was thinking of going rock collecting before we move out of here - there are phosphate mines down the road - or is that a different chemical??  That patent detailed the normal method for getting phosphorous which I hadn't read before.

Microscopes can be very handy if you're doing plant extractions.

Salat - feeling blonde today.
Salat

Sedit

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Re: Red Phosphorous
« Reply #35 on: May 21, 2011, 05:47:20 PM »
I believe them copper brazing rods contain P in the form of the Copper phosphide. You will achieve nothing dissolving it in acid except poisioning yourself with phosphine.
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Tsathoggua

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Re: Red Phosphorous
« Reply #36 on: May 21, 2011, 06:16:47 PM »
It is possible, now you mention PH3, to thermally decompose it (in an inert atmosphere, bearing in mind diphosphine, P2H4 is pyrophoric, although burns with an incredibly low temperature, so I read, it won't even burn skin) WP being the result.

Although not reccomended unless you have A-a good hood, or large outdoor space, B-a gas mask with a cartridge rated for PH3, and C-bollocks of solid tungsten fucking carbide. Perhaps it could be led through a tube furnace packed with asbestos fiber, ceramic fibers etc, metal of course should be avoided due to reformation of phosphide.

Welding rods/phosphor bronze would be a pricy source though, if the silver/cadmium alloy brazing rods I use are anything to go by, or the welding rods that I have never bought, or had need for, but seen while browsing for inert gas canisters and CO2, etc, not cheap, certainly not for the amount of phosphide that would be in there.

Mole smokes on the other hand, could be better used than for murdering innocent animals, and decomposed (CAREFULLY, taking great care to avoid leaks, doing it in a very good hood, or outside, with a gas mask  or closed-circuit O2 supply in either case) via addition of acid, slowly, in something like a Kipp generator, leading the gas through a hot tube full of asbestos, rockwool, etc as said above, and having a current of argon or nitrogen to sweep the formed phosphorus into ice cold water (exhaust gases should be passed through flame, to pyrolyse any traces of phosphine, that may possibly escape, unlikely as this is)

(edited-realised I mistyped the empirical formula for diphosphine, P2H4 not P2H6, although there are quite a few higher phosphines, including some of them solid in nature)
« Last Edit: May 22, 2011, 12:38:14 AM by Tsathoggua »
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Shake

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Re: Red Phosphorous
« Reply #37 on: May 21, 2011, 07:10:50 PM »
what about the piss method cant we just do that?

Tsathoggua

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Re: Red Phosphorous
« Reply #38 on: May 21, 2011, 11:43:18 PM »
If you want to boil down hundreds of liters of piss, which is going to rather stale, and pretty foul after the time needed to harvest that much, unless you start soliciting donations in the street.

Even then, its the phosphate content, plus organics, which pyrolyse down to carbon, so you are simply reducing phosphate salts with carbon, but doing it by boiling down huge vats of piss.

As far as phosphine goes, just watch it, 50ppm is immediately dangerous to life, 8 hour permissible exposure is about 0.2-0.3 ppm, IIRC, slightly irritating to the airways, but not so much as to provide decent warning properties, pure PH3 doesn't smell much, its the pyrophoric diphosphine gas that pongs of garlic (I imagine smelling similar to willy pete), but its cytotoxic, with a delayed action to the lungs, causes severe hepatic and renal necrosis, CNS dysfunction, changes in blood chemistry and the ion balance of the heart, as well as acting as a specific mitochondrial cardiotoxin.

Put it this way, there are specific CDC guidelines on dealing with phosphine poisoning victims transport to hospital. They specifically advise against the use of bodybags......

And they mention not to induce emesis in the case of ingestion of phosphides, this is not for the patient's sake, but for the sake of those around them, the patient throwing up, or perhaps even starting belching, could well potentially kill somebody nearby. Very, very unpleasant stuff.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Tsathoggua

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Re: Red Phosphorous
« Reply #39 on: May 22, 2011, 12:36:51 AM »
Gah, hex, yes, it does form a phosphide with copper. A-you are going to have to melt the copper to add P, in manufacture, and B-yes, copper phosphide forms when heated. It releases phosphine gas on treatment with acid, and fairly sure it does with base too.

Elemental copper and elemental P=not so elemental Cu3P.

Elemental, my dear hexagon.

So to speak.

RP/I2 afaik has to get fairly hot before it produces PH3 and P2H4 (the latter is what gives the funky smell, although elemental white phos smells like garlic, although not the fishy-garlic smell of diphosphine.

Pure PH3 is apparently odourless. Most production methods (such as reaction of elemental phosphorus with strong acids, or caustic) give a mixture of PH3 and P2H4

For that matter, WP reacts with caustic bases or acids to give off phosphine gas and traces of diphosphine (which if you are lucky will spontaneously ignite, and burn it off leaving clouds of far less noxious phosphorus pentoxide (allbeit the anhydride of phosphoric acid, and the bastard-arse dessicant from hell....its capable of ripping the water from concentrated sulfuric acid!!!)

White phosphorus itself is NOTHING like the red or black allotropes, for those who have never handled it before. It is most decidedly nasty stuff, if you are not very careful. Treat with respect, and you will be fine, fuck about, and it will probably poison you. It really doesn't take much. Skin contact insufficient to burn I would think quite capable of producing toxicity, and even a very small burn, as I found out myself, is capable of causing neurological symptoms. Localised yes in my case, but this was from something perhaps 3mm accross, and rapidly removed.

Need I mention either, phossy jaw......no, best look that up for yourselves.

Just be damn careful with the stuff.

Those phosphorus alloys generally don't have very much of it in there, and are probably quite pricy. Copper phosphide apparently does not give off PH3 on contact with neutral H2O, although digestion in strong acid likely would. My advice? don't do it. Its lethal stuff, and low concentrations deaden the olfactory nerve, just like H2S does, so that in addition to its relatively mild irritant properties make for a real vicious, insidious toxin. Delayed effects by up to 3, maybe even 4 days are not impossible either. By which time, damage has been done.
« Last Edit: May 22, 2011, 12:40:58 AM by Tsathoggua »
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.