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megalomania
June 14th, 2003, 08:19 PM
nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 03-16-2001 01:30 PM
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To Obtain Phosphorus: Ground bone-ash, 12 parts; water, 24 parts; mix to a pap in a large tub, and add in a slender stream (still stirring) sulfuric acid, 8 parts; work well together, adding more water if required; in 24 hours thin with water, agitate well , and, if convenient, heat the mixture in a leaden pan, and as soon as the paste has lost its gramular charracter, transfer it into a series of tall casks; largely dilute with water; and, after settling, decant the clear portion; wash the residue well with water, mix the clear liquids, and evaporate in a copper or lead pan, till the calcarious deposit (gypsum) becomes considerable, then cool, decant the clear, and drain the sediment on a filter; evaporate the clear liquid to the consistence of honey (say to 4 parts), add 1 part of powdered charcoal, and evaporate to dryness in an iron pan or till the bottom of the latter becomes red hot; the dry mixture, when cold, is put into earthen retorts well covered with luting and property dried, and heat is applied sideways rather than at the bottom, by means of an air furnace. The beak of the retort is connected with a copper tube, the other end of which is made to dip about 1/4 inch beneath the surface of lukewarm water placed in a trough or wide-mouthed bottle. The distilled product is purified by squeezing it through chamois leather under warm water, and is then moulded for sale by melting it under water heated to about 145 F, plunging the wider end of a slightly tapering but straight glass tube. into the water, sucking this up to the top of the glass, so as to warm and wet it, next immersing the end into the liquid phosphorus, and sucking it up to any desired height. The bottom of the tube is now closed with the finger, it is withdrawn, and transferred to a pan of cold water to congeal the phosphorus, which will then commonly fall out, or may be easily be expelled by pressure with a piece of wire. Keep it in places where neither light nor heat has access, in phials filled with cold water which has been boiled to expel all air, and enclose the phials in opaque cases.
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Agent Blak
Frequent Poster
Posts: 766
From: Sk. Canada
Registered: SEP 2000
posted 03-17-2001 11:26 AM
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Exactly what are the uses of white/yellow Phosphorus(P)?

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A wise man once said:
"...I Am Not Much of a Dancer But,
Just Wait Till The Fucking Begins"

Agent Blak-------OUT!!



Bandit
Frequent Poster
Posts: 82
From: U.K.
Registered: SEP 2000
posted 03-17-2001 12:29 PM
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I dont know about yellow, but white is used in grenades. It lights with contact with air. Tracer round use this as well.
Bandit



c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 03-17-2001 01:54 PM
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Just be very careful making/handling this stuff - in addition to its obvious dangers it's highly toxic. Despite strict regulation of white phosphorous production in 1906, munitions workers in both wars suffered the effects of chronic exposure such as phosphonecrosis (phossy jaw), and acute exposure effects that included liver and kidney damage from inhalation and skin absorption. The fatal dose for humans is ridiculously small - on the order of 15 to 100 mg.
http://www.epa.gov/ttn/uatw/hlthef/whitepho.html



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 03-21-2001 01:47 PM
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I Don't have earthen retorts, but say i did want to make this what is luting?


nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 03-21-2001 09:19 PM
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Luting is a fireproof material used to seal the gaps between the retort and the condenser. The material used to seal fireplace cracks would work well.
Steel pipes would be suitable replacements for earthen retorts.

WP would be excellent for breaking contact with LEOs. Since the army WP grenade has a radius of more than 20 yards, and WP burns down into the flesh, is highly toxic, and provides excellent screening smoke, a WP grenade would be an ideal urban criminal weapon.

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SATANIC
Frequent Poster
Posts: 237
From: australia
Registered: SEP 2000
posted 03-21-2001 11:38 PM
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is bone ash just ash from burning bone?
what would the WP be mixed with in a grenade? does it really explode in contact with air?

A WP grenade would really kick ass. from pics i have seen, it would really kill. even ruin night vision from a distance away. really a good screening / getaway weapon.



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 03-21-2001 11:44 PM
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Bone ash is 'calcined bone' and the way i understand it is basically destructive distillation in the open. Roasting it like a mineral kinda. I read WP ingites @ 10-15 degrees above room temp. There still the chance that it would ignite below that though.



c0deblue
Frequent Poster
Posts: 229
From:
Registered: JAN 2001
posted 03-22-2001 12:22 AM
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A useful reference on White Phosphorous properties: http://chppm-www.apgea.army.mil/dts/docs/detwp.pdf
According to this, WP ignites spontaneously with air *or* at 30 degrees C.



nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 03-22-2001 06:21 PM
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Here's a picture showing the results of "phossy jaw".


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"The knowledge that they fear is a weapon to be used against them"

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[This message has been edited by nbk2000 (edited March 22, 2001).]



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 03-22-2001 10:06 PM
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ouch.. yuck..i mean fuck..that sucks


Donutty
Frequent Poster
Posts: 228
From: UK
Registered: SEP 2000
posted 03-23-2001 01:32 PM
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This is probably of no use, but:
Today I found a bottle of 30% Phosphoric Acid... any use??



FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 03-23-2001 06:33 PM
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Well, don't quote me on this but you might be able to react it w/ a base and get a phosphate, and then use the phosphate *somewhere* in the process above.


Agent Blak
Frequent Poster
Posts: 766
From: Sk. Canada
Registered: SEP 2000
posted 03-24-2001 12:38 PM
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May in an acid Cat. rx


FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 03-24-2001 10:05 PM
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Agent Blak: what does that mean?


CragHack
Frequent Poster
Posts: 618
From:
Registered: DEC 2000
posted 03-24-2001 10:23 PM
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i.e. acid catalyzed reaction. like when you make AP
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...Æ



SofaKing
Frequent Poster
Posts: 399
From: YEAH RIGHT !!
Registered: SEP 2000
posted 03-25-2001 01:07 AM
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There are other self-igniting compounds around. One I have heard mentioned is diethyl-zinc does anyone have info on that ?


Rhadon
Frequent Poster
Posts: 95
From: Germany
Registered: OCT 2000
posted 03-26-2001 08:06 AM
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I found sth. on diethyl zinc:
Prepd by the interaction of zinc and ethyl iodide
from zinc and ethyl bromide / ethyl iodide;
Properties: Mobile liquid. Stable in sealed tube and carbon dioxide. Ignites in air, burns with a blue flame, giving off a peculiar, garlic-like odor. Miscible with ether, petroleum ether, benzene, other hydrocarbons.
Use: In organic synthesis; in preservation on archival pape.



SMAG 12B/E5
Frequent Poster
Posts: 61
From:
Registered: FEB 2001
posted 03-26-2001 11:39 PM
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White phosphorus and yellow phosphorus are the same. It is not mixed with anything in most rounds. It is sometimes submerged in a petroleum liquid. The hermatically-sealed rounds are exploded by a burster charge, usually centrally located in the device. Don't allow air to contact this material. WP can "mess up your whole day".
WP can be converted to red phosphorus, for igniters, by sustained heating in a closed vessel for (?) hours at (?) degrees.


FadeToBlackened
Frequent Poster
Posts: 201
From: Hell
Registered: MAR 2001
posted 04-30-2001 09:22 PM
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I have seen another method for making WP that involves heating tricalcium phosphate (main in gredient of bone ash) with carbon and silica. Is the sulfuric acid part just used to purify the phosphate? What purpose does silica serve? Is it a sort of flux or something to reduce the temperature needed?


nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 05-02-2001 10:10 AM
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The sulfuric acid is used to remove all the organic and acid soluble material from the bones. If you're using bone ash than you don't need to use the acid step.
The silica is used to bind the calcium into a non-volatile silicate, freeing the phosphorus. I believe it also lowers the reaction temperature too.

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Alchemist
Frequent Poster
Posts: 211
From: Woodland hills,Ca.,L.A.
Registered: NOV 2000
posted 05-11-2001 11:08 AM
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Hello NBK2000,
Have you made WP using the method you posted? If so what was the yield. Has anyone else tried it. Also I have seen many types of Phosphate fertilizers (example; Calcium Phosphate).Will any of these work if they are rich in Phosphate?

P.S.,White phosphorus is metastable and slowly changes to a stable form, red phosporus,in the presence of light or upon heating. Red phosphorus is far more stable than the white form. It does not catch fire in air at temperatures below 240°C whereas white phosphorus ignites at about 40°C. Red phosphorus cannot be converted into white
phosphorus except by vaporizing it.

Thanks.......................................

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nbk2000
Moderator
Posts: 1096
From: Guess
Registered: SEP 2000
posted 05-11-2001 01:25 PM
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No I haven't. I found this process in an old book about how to do just about everything yourself from the 1800s.
Calcium or ammonium phosphate will work in the process quite well. The ammonium salt is prefered because of the lower temperatures needed to break it up into phosphorus.

Marvin
June 15th, 2003, 07:49 AM
The sulphuric acid steps arnt purifying the calcium phosphate, they are converting it into phosphoric acid. Strongly heating phosphoric acid drives off water, and leaves a polymeric metaphosphoric acid, doing this while mixed with carbon is a very cunning idea. The metaphosphoric/carbon mixture will produce phosphorous at a lower temperature than the calcium phosphate/carbon/silica process that requires an arc furnace.

Phosphoric acid can be used in the add carbon and bake step directly, so can ammonium phosphate, as this loses ammonia and water to produce metaphosphate under the same conditions. 'Distill' is a bit of an understatement in moden terms, some of the references I have on this process speak of the rhetort being heated to 'whiteness' to get the reaction to run the reaction.

Myrol
October 9th, 2004, 12:09 PM
Well, some minutes ago I made some white Phosphorous...with nearly zero yield :( I put some red P into a 180x18mm Test tube around 2g and plugged the End of the tube with a paperplug (he was 4cm far from the P away.)

So I started to heat that stuff......it worked well the red P vaporized into a yellow smoke and condensed inside the tube to give yellow waxy like P. The Heat was hold on till I got a bad surprise......I remind a disturbing odor like garlic and saw some fumes coming out of the tube and three secs later...WOOOMM....

a dull WHOOFF beside my right Ear. The vaporized white P ignited spontaneusly to make a fucking FAE beside me!! I felt a pressure in my Ear it was not to loud but loud enough to scare the Neighbour running on his Balcony :D well, my ear is now ok but again....this is to strange for me :o

Making white P this way DONT works with satisfactory results.....The risk of a sudden fire or like me a FAE is VERY strong. Also white P is extremly Toxic, its very hazardous to handle it but I LOVE it due to its fantastic shining and the low flashpoint. So, has someone a good Idea how to make white P out of the Red one without vaporizing it out of the Apparatus and being poisoned trough the toxic fumes.

How Poisonus is white P really? Orally very but via inhalation? I dont know, but its everytime a great risk to make him, better be blown into Fishfood as to decay slowly within and die as a human wreck. (IMO)

nbk2000
October 9th, 2004, 02:24 PM
You used a PAPER PLUG?!

And then you wonder why you failed. :rolleyes:

I did it once using a flame-sealed length of pyrex tubing. One end was heated, the other not.

I would use water to keep teh WP end well chilled, so there'd be little pressure buildup from the heating of the RP end.

Myrol
October 24th, 2004, 09:36 AM
Well, Paper can be wasted, it's cheap. An expensive sublimation apparatus should be good cleaned out after use. No one would trash him. WP is a whore in cleaning glassware. Its toxic volatile and stinks like garlic. I prefer to dump the contaminated Test Tube after making him because due to the toxicity it's not worth the risk of cleaning out.....Paper is just a cheap choice to keep the Tube *a little* Airtight. Due this stupid failure, I never make WP ever again.

FUTI
October 25th, 2004, 04:19 PM
Use copper-sufate solution to neutalize its toxicity to clean labware!
Rest of the written here is true.

SmoLL
June 18th, 2006, 01:54 PM
Hello all, i found some to the process make some white Phosphorous.

Red phosphorus is slight hycroscopic, red to dark red crumbs, sensitive againt friction, much more stable than the white form, pulverization in airtight ball-mills. Red phosphorus can be converted into white phosphorus in a sublimation apparatus.

White phosphorus is unstable on the open air, most reactive with oxygen, similar like white wax scales, very toxic, stabel in airtight glas bottles at low temperatures. White phosphorus can be converted into red phosphorus by a burning process.

Process making white phosphorus:
Put some powdered red phosphorus into a 500 ml distilling flask, connect the beaker to a simple condenser. Connect the condenser to a 500 ml receiving flask, set the distilling flask to a hotplate and put the receiving flask to a salt ice bad. The red phosphorus is careful vaporized and a little icy air is pumped into the receiving flask. This should form some crude white phosphorus on the bottom of the flask.

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A perfect example of n00b copy/paste

What happens when vaporized white phosphorous is exposed to a stream of oxygen in the confines of a flask?

:rolleyes:

NBK

a_bab
June 19th, 2006, 06:18 PM
icy air... now that's something [stupid].

Normaly CO2 it's used, and it works even if not being "icy".