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Author: Subject: Homemade Phophorus!
dorkwad
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[*] posted on 9-3-2014 at 21:13
Homemade Phophorus!


So I decided to try the cheapo version of making phosphorus in a little borosilicate test tube with some phosphoric acid solution (>25% Krud Kutter) and some lead wire (60/40 lead tin solder wire). This is an even more cheapo version of the cheapo version that's explained in the phosphorus thread and its summation file.

What I came up with was some smoke, maybe this was phosphine? Lol I thought it was just the dilution in the phosphoric acid boiling, I also remember there being a lil flame at the mouth of the tube when it was whisping out, then I didn't look down in it to see the faint glow, but eventually cracked the tube after I saw some green stuff from the outside of it...

Take a look at the pic to see what I'm talking about, also can you tell me what this is, what it means, etc? it is like a crispy crackly cookie that is somehow a little gelatinous and sticky, this green stuff I mean. Please tell me this is actually something cool and not just some Nickelodeon green slime lol.


Lemme quote the phosphorus synthesis thread here at the bottom...

"2 g of lead wire were placed in a borosilicate test tube along with 1 ml of 85% H3PO4. This was heated in a propane torch flame, carefully at first as water was driven off. Heating was increased, and the lead melted under the acid. After a couple minutes a thin stream of whitish smoke started wisping from the test tube. The smoke had the characteristic smell of burning phosphorus. It occurred to me after a bit to turn off the light, and I saw a mysterious and beautiful site: there was a greenish light appearing about halfway down the test tube. The light moved up and down the tube as the heating was increased and decreased in intensity, probably representing the rate of production of flammable vapor vs. its interaction with the atmosphere. After admiring the green glow for a few minutes, I broke off the experiment."



[Edited on 10-3-2014 by dorkwad]

PhosphorusGlass.jpg - 121kB

[Edited on 10-3-2014 by dorkwad]

[Edited on 10-3-2014 by dorkwad]

[Edited on 10-3-2014 by dorkwad]
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dorkwad
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[*] posted on 9-3-2014 at 21:23




[Edited on 10-3-2014 by dorkwad]
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IrC
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[*] posted on 10-3-2014 at 01:56


Sounds like it was an interesting small scale experiment but do others a favor who are not familiar with threads on the site and post links to "phosphorus thread and its summation file". This saves people (especially new people here) from hours of searching and reading. Many people are browsing in spare minutes between school or work and it is very helpful when you mention a reference if you point to it so they can quickly catch up to what you are saying or doing. Don't take this as ragging, just giving a suggestion for what it's worth.




"Science is the belief in the ignorance of the experts" Richard Feynman
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dorkwad
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[*] posted on 10-3-2014 at 02:21


Quote: Originally posted by IrC  
Sounds like it was an interesting small scale experiment but do others a favor who are not familiar with threads on the site and post links to "phosphorus thread and its summation file". This saves people (especially new people here) from hours of searching and reading. Many people are browsing in spare minutes between school or work and it is very helpful when you mention a reference if you point to it so they can quickly catch up to what you are saying or doing. Don't take this as ragging, just giving a suggestion for what it's worth.


Ya that's why I included the synthesis instruction along with my cheapo version of it, but anyways i'll do that for ya'll, here's the phosphorus thread it's actually a sticky on the site btw, http://www.sciencemadness.org/talk/viewthread.php?tid=65
and here's the summation file of the entire 46 page thread
http://www.sciencemadness.org/talk/files.php?pid=247779&...
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[*] posted on 10-3-2014 at 07:21


Why didn't you put this in the phosphorus thread?



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dorkwad
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[*] posted on 10-3-2014 at 14:02


Literally because i dont think much of my experiment and felt the phosphorus thread was to professional for me and what I did lol
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[*] posted on 10-3-2014 at 14:44


Haha, I understand.
;)




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Mailinmypocket
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[*] posted on 10-3-2014 at 16:13


Interesting. I shall try the method you quoted in the OP except with lead granules and 85% phosphoric acid. Will report back and see what the results are. I will try and condense the white vapor somehow and see what we get.
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Antiswat
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[*] posted on 11-3-2014 at 12:35


lead the gas into water
it should coalesce into white phosphorus which can then be heated without air into red phosphorus
i recall this happens just around 200*C




~25 drops = 1mL @dH2O viscocity - STP
Truth is ever growing - but without context theres barely any such.

https://en.wikipedia.org/wiki/Solubility_table
http://www.trimen.pl/witek/calculators/stezenia.html
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Zyklon-A
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[*] posted on 11-3-2014 at 12:54


Isn't it the opposite? I thought: RP + heat → WP.




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[*] posted on 11-3-2014 at 12:57


At 200-250*C, under vacuum and with a catalyst of 0.5 wt % I2, WP does in fact convert to RP.



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[*] posted on 11-3-2014 at 19:14


I don't know why but the stopper just pops out of my tube instead of having the gas go into the water, and my tightly O-ring clamped vial connected to a plastic tube just condenses right when it enters the tube, and either falls back into the vial or on the outside making a mess of droplets that turn into the gas. Any suggestions on getting the gas to go into the damn water? I feel like this shouldn't be hard should it be under vacuum?
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[*] posted on 17-3-2014 at 13:21


I did a very crude experiment here. I used the same amounts as used in the original post, heated the acid until boiling and until steam stopped coming off. At this point I plugged the tube with filter paper to slow any excessive oxygen from entering etc.

The fumes did not make a glow or condense in any way, they were quite thick though and did have the characteristic smell of P.

I might try this again and lead the vapors into water, this was the original plan but I wanted to do a crude run first before glass working some tubing and whatnot. The damage to the glass is substantial though. I didn't get any colored material as mentioned above.
image.jpg - 64kB

The 2g of Pb granules melted into a button under heat, the button now weighs 1.82g.

I'll try this again when I have more time and put more effort into the analysis of the vapor etc. Just wanted to update the thread.
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