Purification of phosphorus -- treatment of WP burns

I made my sample by dry distillation of mixture of RP and pure quartz sand to avoid bumping and to make a porous bed in the retort. If one's careful and patient, mildly orange samples can be obtained, devoid of sand particles. The traces of residue in the retort are black and I can't identify it.
However, due to the nature of the apparatus (distilling could be done with a candle; it's very dangerous and requires an experienced experimentator, but this is not the topic of this thread) some RP will be carried over into the receiving water.

The first thing I did was to put it in a syringe full of water and to push it through a piece of cotton at the bottom of a beaker filled with hot water. Some of the spheres that come out are orange, some are yellow. They're all quite opaque. My conclusion is that, theoretically, proper filtering could be enough to get very pure yellow samples, but it's simply too hard to do, so this is for removing the worst impurities. This is the filtered product.

It glows, but not furiously as cleaner samples.
I've made it in the shape of a ring and, at ~ 25 °C, it behaves like a piece of plastic. It can be bent in one direction, but snaps without warning if you try to bend it in the original position.

Next thing I did was to divide the sample into two batches. One for nitric, and one for chromic acid bath. I'll describe what I've did, and write a recommendation.


- procedure -

I took 50 ml of distilled water, added to it 1 ml of concentrated sulphuric acid and about two tiny spatulas of potassium dichromate. I dunked the WP inside, melted it and swirled it a couple of times. I left it at current room temperature (~28 °C), covered with a box to protect it from the light. It remained molten.
At first some kind of yellowish, opaque precipitate formed on the surface of the sample, which was being slowly eaten as the hours progressed.
This is what it looked like after almost two days of soaking.


After removing the chromic acid, and short rinse with dilute sulphuric acid, this is what I've got.


Upon solidifying, it turned opaque and strongly yellow with a lemon tint. The orange tint was almost gone.

I've thought this was it, the best that chromic acid can do (I was wrong), so I've put it in a nitric acid bath for several hours, in a molten state, swirling. The procedure did not appear to have altered its color significantly. It was still yellow, and the transparency was still low.


So that's what happened with the larger batch. I've cut it with a knife, melted it into ingots and stored under distilled water.



The smaller batch first went through a nitric acid bath which removed much of its orange color.


Then I tried to wash it with chromic acid. I was out for about six hours and the small batch was sitting molten, without any precipitate (obviously because of the initial nitric acid bath), in the corrosive orange mixture.
Oh boy was I surprised when I got home and rinsed the chromic acid.



This is the purest WP I've personally seen in my entire life. It's not colorless, it still has a hint of yellow, but it's almost colorless. The opacity is negligible and due to the surface roughness. Upon cutting with a knife, it's like a piece of glass. The only purer sample I saw was Theodore Gray's, but that was over the Web.

It glows better than the earlier impure samples.

In a couple of days, when I get a hold of professional DSLR camera, I'll make nice macro photos. This is just a prelude.

Later I've melted all together, both lemon and colorless form (photo with the bottle).


- conclusion -

I don't know if chromic+nitric acid methods could replace the initial cotton filtering. I haven't tried it yet.

After cotton filtering, several hours of swirling in warm nitric acid is capable of destroying all of the opaque, sandy precipitate, and remove most of the orange color. It can't remove all of the opaque impurities, indicating they aren't made of one compound.

Sitting under chromic acid is capable of removing both the color and precipitate, but should be used together with the nitric acid method, preferably after it, because the nitric acid method allows the oxidation and fuming, therefore building up of phosphoric acid in the mixture.

The most important thing is to have lots of chromium(VI) above the sample and not to cover the entire bottom of the vessel. The sample should be small (not larger than a thumbnail) to form a blob surrounded by the acid.
My first attempt failed because the amount of chromium(VI) was too low and the sample covered the entire bottom. There wasn't any speedy cleanup. The lack of chromium(VI) was obvious by the dark brown color of the partially spent solution.
In the case of the smaller, already rather pure (HNO3) sample, the orange color of the chromic acid was almost untouched after the cleaning, indicating there was an excess of chromium(VI).

I'll run the chromic acid bath with the combined batch once more, this time for more than few hours, because I want colorless ingots. Later, I'll expose a piece of colorless sample to the sunlight during the day, to see the color change.


I must say it was quite entertaining to build up adrenaline while taking the large batch and cutting it with a knife, using a gloved hand in a dimly lit room. The stuff really looks like some weird alchemical shit, like a true philosopher's stone. It glows, the vapor close to it glows and flows like liquid, cool fire. You just want to stare at it because it's so enchanting, but you know there'll be trouble if you do it. It really looks poisonous, like those glowing skull-shaped vapors above opened poison bottles in cartoons (perhaps there's a connection). I had the ventilation system on maximum setting the whole time to suck the fumes away.

The feeling of cutting pure sample at room temperature is similar of cutting cold, not so old piece of resin. It is waxy, and sort of like a hard clay, but it can burst into shards.
The colder it is, the more brittle it becomes and can snap, sending dangerous shards around the table, which is obviously very dangerous because you've got few minutes at most before they catch fire. They melt under their own heat so you have to cool them with ice before catching them with tweezers, or just pick the drop with paper tissue. If it's larger than 1 mm in diameter, expect it to burst into flames in a matter of seconds. Throw it immediately in a copper(II) solution or on a safe surface to allow burning. It's advisable to do it during the night, because you can turn off the light to see where they are.
While cutting, it's best to tilt the knife left-right, being careful before the final snap, which I did using wet gloved hands. Of course, you have to do it in a rush. Occasional dunking in the ice cold water is preferred because it builds up heat.

[Edited on 2-8-12 by woelen]

Quote: Originally posted by Endimion17

I made my sample by dry distillation of mixture of RP and pure quartz sand to avoid bumping and to make a porous bed in the retort. If one's careful and patient, mildly orange samples can be obtained, devoid of sand particles. The traces of residue in the retort are black and I can't identify it. However, due to the nature of the apparatus (distilling could be done with a candle; it's very dangerous and requires an experienced experimentator, but this is not the topic of this thread) some RP will be carried over into the receiving water.

Quote: Originally posted by BromicAcid

plante1999, preparation was described in the original post: Quote: Originally posted by Endimion17   I made my sample by dry distillation of mixture of RP and pure quartz sand to avoid bumping and to make a porous bed in the retort. If one's careful and patient, mildly orange samples can be obtained, devoid of sand particles. The traces of residue in the retort are black and I can't identify it. However, due to the nature of the apparatus (distilling could be done with a candle; it's very dangerous and requires an experienced experimentator, but this is not the topic of this thread) some RP will be carried over into the receiving water.

Thanks, guys.
BromicAcid, that's a very cool quote. I know the feeling and I live for it.

No advices, huh?

The burn looks ok, only surface layer is missing, the next layer is pretty much intact. There are no "holes" or any other deeper pits which are common in these cases, probably because I didn't let the stuff burn, but was furiously shaking it off.
Other wounds are fine, no surface layer detachments, only occasional boil.
I'm feeling fine. Absolutely no symptoms of poisoning and at least intestinal cramps should've started. I didn't go to the ER.

Before heading off to bed, I've put the WP on stirring in chromic acid again. I've secured the stirrer so that if it fails again, all it can do is to embed itself into the melt.
It was stirring in the dark the whole night, and this is what I've found this morning around 11:00.


Obviously, the green stuff is chromium(III). WP has solidified in the form of sand.

Upon removal of the spent chromic acid, the product looks like this.


Absolutely no traces of yellow color. Pure white, cleaner than the last purest sample, this time the whole batch. Again, I've put it on a chromic acid stirring bath (less than an hour, to see if the orange color changes again) and then I'm gonna melt it into ingots and take a photo.

I have reasons to believe this is beyond analytical grade stuff. Usually when you buy WP, it's yellow.

The only thing I'm puzzled about is whether the chromium(VI) was spent on impurities or was it oxidizing the phosphorus, too.

[Edited on 30-7-2012 by Endimion17]

It seems chromic acid is being reduced by WP alone. It went green after like 30 minutes of swirling, so I replaced it with distilled water.

I can't seem to determine the color of the purified sample anymore. It became so pure its color is vague, and my lab lights are both incadescent and fluorescent, so the stuff seems to have a very weak greenish or yelowish tint. Maybe it's because of my inability to distinguish such tints? I don't know.

The melt seems to be a bit more opaque than earlier melts. I hope chromium(III) isn't responsible. Maybe I'm just wrong, because I'm now comparing a small blob and a large batch. Maybe it's just turbidity because of the all night stirring. After all, there were problems with coalescing of the droplets.

As you can see in these images , it's practically colorless, and the subtle white balance differences make it hard to determine the true color, no matter how good you edit it afterwards.
As expected, pure WP strongly refracts light, and you can see the rainbow in the blob from the first post, and that's why the sandy WP looked completely white.
I've took similar photos so you can compare the colors.
It would be the best to take a photo in the sunlight, but it would turn yellow, and I don't want that after all this trouble.

The glow, as usual, isn't appreciable at 0 °C, but soon after it warms up, it's easily visible even with the lights on. The purer the sample is, the stronger the glowing.

Any ideas what to do next? Any photography wishes? Reaction videos?



BTW I've started to treat my wound with silver sulfadiazine. I guess that any traces of WP were oxidized during the night (the smell was gone before I went to bed), and the only danger right now are bacteria. I feel fine and have no symptoms of poisoning.

Thanks for the feedback, I appreciate it.
The wound seems to be reacting to the sulfadiazine silver as predicted - the exposed layer is covered with goo. It's probably partially composed of white blood cells that rushed to the scene, then killed by the silver. You can see some hemolysis at the top, that's probably where copper has lodged in the burned top layer. There's no inflamation, and no puss, the wound doesn't smell at all. I think I'll post photos of the wound each day for the next week for you to see the progress. AFAIK, there are no such sets of photos on the Web and I believe that would be quite useful for anyone out there who will get burned some day.
There are more burns, but as they're just boils (also 2nd degree but boring) or first degree and some superficial reduced copper marks, I'll skip that.
As for the scars, I doubt there'll be any after few months. I've had a boiling water accident in the lab like two years ago and it involved a sensitive area of the arm, today it's not even visible. I had quite a lot of burns in my life, even chemical ones, and I don't have visible scars. Nevertheless, I'll ask my pharmacist if he has any advice.

This is the shirt. As you can see, my left teet was almost burned, and one piece almost landed on my thigh.


I made another batch of raw WP few hours ago, and skipped the cotton and the nitric acid method. Straight to the chromic acid, but hot and swirling. I want to simplify this as much as I can to provide a decent and less dangerous method for obtaining extremely pure samples.

This time, I'm carefully measuring the masses and durations, and will inform you of the yields. So far, they seem to be extremely high. My 0.1 g scale didn't register any loss of the initial 3.5 g of RP, and the time for cleaning seems to be less than 15 minutes. I turned off the stirrer and now waiting for the spheres to merge together.
Also, the amount of dichromate needed for batches of few grams is really ridiculous.

Here are 40 seconds of mesmerizing stirring action. I cranked up the voltage near the end, so the blob disappears.
<iframe sandbox width="420" height="315" src="http://www.youtube.com/embed/Z7ibNhABRX8" frameborder="0" allowfullscreen></iframe>
Sorry about the video quality, that's about the best I can do with my equipment at the moment.

[Edited on 31-7-2012 by Endimion17]

Thanks. Retort was made out of regular borosilicate test tube.
I used a quiet, small, half oxidizing flame of a gas torch, but it could've been a Bunsen burner, too. The temperature doesn't have to be high. I've mentioned candles because of the temperature. Of course, more RP, more heat. Better use propane-butane.
The bumping is not bad per se, but it can lead to a water surge, cracking of the retort and then you're screwed. I think Leidenfrost effect happens, because RP, while gassing out P vapor, can slide towards the neck and cause mayhem.
You can use regular sand, just treat it with HCl first, then roasting, to decrease the amount of impurities.

Vacuum only lowers the boiling point... It doesn't affect the temperature of RP breakup. I'm not sure of the benefits. Your pump will be in a serious trouble.

Don't use quickfit glassware like flasks etc, unless you have the means for purging out air. Larger glassware, more air, more initial RP fire, lower yield. Also, working with larger amounts of RP... I'd be quite nervous. 3-4 g is my maximum. This is not something you can leave alone. You simply have to be there, holding the burner, tapping the setup occasionally to avoid sudden caving of the material which leads to rapid release of the gas and pyrophoric burps.

Packing of RP+sand should be like this.

There has to be a slope, to avoid a buildup of P vapor in the bottom. Receiving water should be around the melting point of WP, to avoid clogging.

I finished my quantitative experiment, so here are the results and the photo.

m(SiO2) = 0.6 g
m(RP) = 3.5 g

distilling time <20 min

m(raw WP) = 3.5 g

cleaning time (hot, swirling chromic acid) ~10 min

m(pure WP) = 3.3 g


The last mass would've been >3.4 g, if there wasn't WP mud on the top, that I couldn't join with the sample.
I recommend slow automatic stirring, without dispersion. It seems that very pure samples have trouble coalescing. That's OK if you want WP powder.



I think the color is partially due to chromic acid hydrosol. If the chromium goes from (VI) to (III), then it's a greenish tint. Dispersion is really something that should be avoided while cleaning.

An interesting thing happens when you try to melt it. It goes completely transparent and soon it gets cloudy.


I have no idea what is happening here. WP melt should be transparent and highly refractive. No opacity.



All in all, my yield after the initial fire, the distillation and purification is a bit over 97%, and is consistent with other experiments. I don't think I could go higher.
Don't disperse it or you'll have troubles with the mud and chromic acid hydrosol. Use slower stirring in warm water and do it overnight to save on time and to use the lack of sunlight. It would be the best to allow few blobs swirling around, joining and breaking up like in a highspeed lava lamp.


Regarding the wound, there was a bit more hemolysis (maybe I hurt it during sleep), but no redness, so no inflamation. However, the gauze has stuck on it, meaning it started drying and now proper epithelization should kick in. That's good, though posting daily photos of a piece of gauze looses its purpose. I'll continue with small amount of Ag-sulfadiazine, and start daily disinfection of the surrounding area with ethanol. I have no symptoms of poisoning except some small bad digestion and general feeling like shit, but that's common when you try my family's cuisine and don't have enough sleep.
I'm starting with multivitamins, extra vitamin C and plenty of milk. Death can occur within a week or so, so I better deal with it.

Quote: Originally posted by Rogeryermaw

firstly let me say that if you are in fear for your health don't let anyone tell you not to seek medical care. that said, the resource of first hand knowledge available here about phosphorus burns is rather low (personally i feel that is a good thing) so the experience base to draw on is limited. my experiences with phosphorus burns are minor but the wounds were deep and very painful. i tried making PCl3 on a test tube scale and there was a point where my chlorine generator pushed too much gas and the result was liquified P4 sloshing out of the tube. the resulting fire melted the test tube and glass tubing from the gas generator. when it dropped, it got on my hand and my pants. instinctively i patted the fire but that only spread it so i dropped my pants, rolled them into a ball to extinguish the fire and wrapped a wet towel around my hand. i did not have a method of neutralization handy so i had to get the area cold and peel the phosphorus off the wound. this was around a year ago and i have suffered no ill effect to this day. my wife (nurse) says your wound looks healthy and said she would treat it as a normal wound. use a good triple antibiotic, and loose gauze so it can breathe. re-dress the area every day or two. after 3-4 days let it breath so it can crust over an heal. otherwise, just keep it clean. you have done a great job of caring for it thus far. the use of a good triple antibiotic will help to minimize the appearance of scar tissue. again let me re-stress that if you are in fear for your health, do not let anyone tell you not to seek medical attention. i can only relate my own experiences with this beast which do not cover all bases in any way. speedy recovery, man. as far as the welding excuse, due to the size and area of the burn, it may be wise to say you accidentally laid the area down on a hot surface after welding.

Good grief, you peeled WP from your wound?
Then you were in a much greater danger than I ever was. I haven't found any on my burned tissue. It either burned off (I don't recall much pain, maybe because of the adrenaline), or fell on the floor.
I have found a tiny glowing speck few cm away from the wound, resting on the hairs. I could barely see it, like when you look sideways, searching for a faint star. And that's it.
I'm grateful for your wife's input. Yes, the gauze is loosen, it's like 6-7 layers, it's not encased with surgical tape, there's plenty of room beneath it. I don't think letting it breathe without the dressing is appropriate at this time because it's quite deep. I'll continue this until day five, at least.
I have triple antibiotic in a powder form, but I don't see the neccessity as I'm using Ag-sulfadiazine.

If things get worse, I'm heading to ER. No worries about that.

Quote: Originally posted by Pyro

endiminion, you should say you had an accident using a flare, flares often contain WP, chances are they will not ask too many questions. say you used a road flare, or that you were on a boat,... The flares I have on the boat contain WP, and at one point the company recalled them as they were not safe for use, something about them exploding. I knew english wasn't your first language, by what I can make out on your P container, it says Fosfor, which means you can live in either:Belgium, Holland, germany, and a few others. which one is it? EDIT:if you are going to say its a welding accident i personally think that you should say that flux dripped onto your hand, even though if you are welding you should be wearing welding gloves lol. Just go to ER, even if you tell them you got it purifying WP, what can they do? chances are WP is not illegal, and the cops will have a heck of a time getting a warrant [Edited on 1-8-2012 by Pyro]

Quote: Originally posted by Pok

Tell the doctor that you found a piece of amber when you were in holidays at the baltic sea...you stored in under water and took it out at home when it spontaneously took fire in your hand: http://www.ncbi.nlm.nih.gov/pubmed/18926385 This is a credible argumentation! Go to the doctor! [Edited on 1-8-2012 by Pok]

That would take me to the cover of the magazines, and sooner or later, this thread would become famous, as my lie about baltic holidays.
I could make up that a friend of mine was playing with it. That would be credible.

Quote: Originally posted by gutter_ca

http://www.utsandiego.com/news/2012/may/17/phosphorous-may-h... Supposedly happened here in San Diego.

Quote: Originally posted by Pyro

All white marine flares contain WP, if the corruption is staggering you should not worry too much lol. bribe the doc not to tell anyone. maybe you burnt yourself with hot jam? or soldering? or molten sugar while making caramel? the choices are endless, how about not going o the ER but to your local doctor who you know and tell him it was a burn caused by unspecified substances, or tell the ER that. they have no right to force you to tell them, and if they try, go away and try a different ER

If I had the money to bribe the doc, I wouldn't be saving money to buy lab equipment.

Pok is right, you can't lie because this is not a thermal burn. It's a chemical burn, and it's a WP chemical burn.
There's only one ER.

Quote: Originally posted by freakinto

I know I'm just an anonymous but listen to me please. My friend is a nurse and she says you should have gone to ER immediately when that happened. Your wound doesn't look very good. That thing absorbs constantly and can damage your kidneys and liver. Please go before it's too late. If things get worse, it can be already late, she also said that even now can be late. I'm not trying to scare you or something like that but please go to the doctor. Life is the most important. [Edited on 2-8-2012 by freakinto]

Absorbs what? If there was any WP in the wound, it would smell of matches. It stopped smelling like that less than 3 hours after the accident.
Thanks for being so concerned, but I really feel the same as before. I know there's the one week window for going six feet under, but you have to have symptoms for that to happen. This is not acute cyanide poisoning that throws people on the ground. If liver starts failing, I'd be having a bad time already.

I'll do a private blood test of my liver markers, that shouldn't be awfully expensive.

Day 4. I've noticed this morning that my gauze dressing is gray, meaning the silver creme is not being sucked into the wound greatly as before, and is being reduced to elemental silver after migrating to the surface.
Few minutes ago, I've removed the gauze. The wound is healing. There's scar tissue being formed, and the open, gooey area is reduced by some 75%. This is the inner side of the dressing. You can see the reduced silver around it. There's a lot less aseptic goo.

This is going to be fine. I've washed it with tap water, let it dry while swabing the surrounding area with iodine tincture, put a thinner layer of silver and another gauze.

Maybe it would be nice if the admins would add something like "burn treatment" in the title, I'd hate to see all this effort being forgotten. One day this info could save someone's ass.


Back to WP. I've put two samples out in the sun. They literally turn yellow in a matter of few seconds.

Even the first photo isn't showing the initial lack of color because it was faster than my response. You'd literally have to snap the photo as soon as you take them out of a light tight box. It takes like ten seconds to go vegetable oil yellow. The lower photo is one hour later. The samples have melted in the scorching sun. There's the yellowish crust, and you can see by the cracks in it they've gone orange. It essentially turns into the color of the raw sample before the cleaning process.
That's why I've put my clean WP in a closed coffee can with some sand on the bottom, to go by the book.

[Edited on 2-8-2012 by Endimion17]

Quote: Originally posted by Endimion17

Absorbs what? If there was any WP in the wound, it would smell of matches. It stopped smelling like that less than 3 hours after the accident. Thanks for being so concerned, but I really feel the same as before. I know there's the one week window for going six feet under, but you have to have symptoms for that to happen. This is not acute cyanide poisoning that throws people on the ground. If liver starts failing, I'd be having a bad time already.

Well, you sounded scared despite that knowledge so I tried to help you. However, I am glad you are OK now. Good luck and take care.

@Endimion17
I wanted to let you now, that this a great thread and that I really enjoyed reading it!

As far as experiments with white phosphorus are concerned here are a few more ideas:
Burning a piece of white phosphorus in an atmosphere of oxygen is very beautiful. It looks like sort of a sun en miniature. (there are videos on youtube). I had a teacher who used to throw a little peace of WP in hot, fuming nitric acid - very intense, dangerous reaction - the onset can be slow. If you dissolve a bit of WP in castor oil in a large flask and shake the flask you can observe very well the fluorescence. A demonstation of the Mitscherlich test is also something interesting to do, but take care not to inhale the vapours...

Here some links to videos about WP:
Mitscherlich test
burning WP can´t be extinguished by water
Se youtube for "phosphorus sun" videos.

Quote: Originally posted by gutter_ca

http://www.utsandiego.com/news/2012/may/17/phosphorous-may-h... Supposedly happened here in San Diego.

"There is phosphorous that naturally occurs on the sand at the beach, but no one has ever heard of pants catching fire," Stone told the Register.

“Laboratory testing confirmed elevated levels of phosphate on the rocks,” said a brief statement issued by the Orange County Health Care Agency.
The statement said the agency’s role in the matter is done.
http://www.utsandiego.com/news/2012/jun/02/tp-hot-rocks-phos...

At San Diego County’s Department of Environmental Health, hazardous materials chief Mike Vizzier said Friday he had no plans to go looking for suspicious stones at the site. “We talked with Orange County, and they said they looked and they could not find any more,” Vizzier said.

He’s still wary about elements of the story. “We are not even convinced it was phosphorus yet,” he said.

Abbott said he has no doubt that the fire and the burns are real, but he’s baffled by the source of the flames. “It must be something that ignites at low temperature, so I am assuming the orange stuff is human made … and probably something that was designed to burn,” Abbott said.
http://www.utsandiego.com/news/2012/may/19/tp-fire-starting-...

Nothing about the burns there. Matches from 1800's sunken cargo are raised on occasion, causing surprises and sending divers to the hospital.

Quote: Originally posted by a_bab

Freak accidents do occur and they may not be even freak; let's say the power goes off and your magnet breaks the beaker full of finely divided phosphorus. Were you prepared for this event?

Quote: Originally posted by Heuteufel

@Endimion17 I wanted to let you now, that this a great thread and that I really enjoyed reading it! As far as experiments with white phosphorus are concerned here are a few more ideas: Burning a piece of white phosphorus in an atmosphere of oxygen is very beautiful. It looks like sort of a sun en miniature. (there are videos on youtube). I had a teacher who used to throw a little peace of WP in hot, fuming nitric acid - very intense, dangerous reaction - the onset can be slow. If you dissolve a bit of WP in castor oil in a large flask and shake the flask you can observe very well the fluorescence. A demonstation of the Mitscherlich test is also something interesting to do, but take care not to inhale the vapours... Here some links to videos about WP: Mitscherlich test burning WP can´t be extinguished by water Se youtube for "phosphorus sun" videos.

Quote: Originally posted by Rogeryermaw

@e17 i am sure most of us here are curious as to the progress of your convalescence. any news? pain reduced? healing well? you should be out of the woods as far as systemic damage from absorption. how are you?

Quote: Originally posted by Pyro

wow, that looks so much better, does it still hurt? the WP looks awesome, i can't wait untill i am ready to try

Quote: Originally posted by Rogeryermaw

both the healing and the P4 look great. my own scars are barely noticeable a year later and only if i'm looking for them. your phosphorus looks phenomenal! truly bright glow! that is a sight most will never see in their lifetime. makes me want to procure some chromic acid.

It would be kind of cool to have a "special mark", wouldn't it?
If you have a rich pinchful of K-dichromate, you can clean probably more than all the samples I've made so far, so go for it. Let's stuff the Web with these photos.

Quote: Originally posted by a_bab

Rogeryermaw, the phosphorus doesn't glow that much at all. It's a very pale and delicate color, much like any ZnS based glow in the dark item, but very delicate. The fumes is what makes it so nice - you can see them glowing above the phosphorus piece, up to a few cm of height. Actually it's simple: you saw a fuming piece of WP being filmed - now thing about these fumes as being phosphorescent aswell. What's nice about phosphorus is the fumes - they look "supernatural". That photo only shows the color, which indeed I find almost corect. I now remember my first attempt at getting some phosphorus and the first obvious source was matchbox strikers. Having collected about 100 of them, I dry distilled them in a testube under a CO2 flow. Once I set up the "aparatus" I turned off the light (my lab was in a basement). The sight was something wonderfull: the phosphorus vapors expelled by the CO2 flow looked like a green flame, fairly bright, but cold (you could pass the hand over it with no harm). That was a special magical moment, and I then understood what Brand must have felt like. BTW, I guess it takes some serious years of playing with WP like this in order to get the phossy jaw - I'm convinced that people who made matches must have felt the smell all the time. [Edited on 7-8-2012 by a_bab]

a_bab, if only it would look that nice.

Here are the wound updates. I've increased the delay between every next image by one day (so day9 and day10 are two days apart), because the changes aren't that speedy anymore.
So here it is: 8, 9, 10, 11, 12

I think there'll be hardly any visible scars by the time winter starts. If there wasn't for that silver creme, this would've been a different story...
My other burns are fine. I'm still missing tip of one finger where one large boil was, but it's getting fine.


OK, now for the fun part. I had a few ml of bromine left so why not trying reacting it with very pure WP? Anyone reading about it knows it's extremely violent, but has anyone ever seen it online? Here it is, a video taken a little over one hour ago.

<iframe sandbox width="420" height="315" src="http://www.youtube.com/embed/HXuKgTTfSdY" frameborder="0" allowfullscreen></iframe>

I know, this wasn't exactly a safe experiment because it's obvious the stuff was ejected out, but I had this intricate dropping mechanism and I was not close, wearing protective equipment. Also, water hose was on standby, and there was dirt, too.

The amount of WP was half of a typical pea and even that is pretty massive. The amount of bromine spent was very small. As soon as they touched each other, most of the WP was ejected. It was like deadly fireworks.

Honestly, it's a lot more loud than it seems. My camera's microphone is designed for recording mainly typical voice registers, not bangs.
I don't recommend doing this. It is VERY dangerous. It seems to be more violent than cesium and water. The danger is even greater knowing that most of the WP comes out molten and on fire. You can easily get severely hurt. If you increase the mass, this becomes a deadly weapon, so please don't do it or you will get hurt. This is far more dangerous than typical amateur explosive mixtures because it can melt your face off, and kill you during the next week. Treat it with utmost respect.

the most interesting screenshot...


[Edited on 13-8-2012 by Endimion17]

[Edited on 13-8-2012 by Endimion17]

Wow this is great

I don't think I would ever attempt this kind of thing

I am a mad scientist after all so I can't say for sure .

I would just be afraid of getting phossy jaw.

Great post , thanks for sharing.

Quote: Originally posted by BromicAcid

When I went to the hospital several years ago for a thermite burn here were the main issues: 1) No one knew what thermite was 1a) No one cared what thermite was 1c) No one believed I knew what I was talking about

Quote: Originally posted by Rogeryermaw

on the other hand, doctors and medical staff are supposed to follow the hippocratic oath which guarantees absolute privacy concerning your medical status unless it involves a gunshot or child abuse which require reporting (at least in the u.s.). not sure how burns from listed chemicals would be handled.....

actually in hindsight, visiting a military doctor would be best, atleast in the US and europe. don't know about [DELETED]
but I love the bar of WP!! awesome!
I will definitely try it on a small scale first, after i get a damn torch hot enough! (might take a little while, will ask for one for christmas )

[Edited on 18-8-2012 by Pyro]

Yes, if you leave such pearls in chromic acid for at least a month, all of the Cr(VI) turns to blue Cr(II), and the obviously exponential drop in reaction rate means that WP's surface will be etched more and more slowly, etching its surface in a fractal manner, I guess. They indeed show some opalescence, but more than opalescence, they show chatoyancy. It's incredible. I should take a photo of it.

BTW I was wrong here. The scar is still there.
It's possible I'll be left with a permanent one. It's been a few months and it basically looks the same as it did in photo #12, with the exception that now my skin regained its surface texture. But the discoloration is still there and, funny enough, changes with my overall condition. If I'm cold, tired or scared, it gets this ugly cyanotic tinge, like a bruise.
When I'm warm, rested and happy, it's pink. So it's like a mood ring, only it works more reliably.

Phosphorus burns

here are the promised pics:






these two are from when I squirted a pipette full of WP into a beaker of cold water, I have never seen this before!
it looks a little yellow but was actually more white, the water is yellow because it contains a tiny bit of chromic acid that got pipetted over with the WP



these are the three beakers needed, on the left a soln. of K2Cr2O7+H2SO4, on the right a more concentrated soln. to put the crap into and in the back distilled water to put the pure WP into




this is the main blob of WP under chromic acid




this is a blob of burning WP on water, as you see it floats! I was pipetting it and accidentally squeezed the bulb ever so slightly and a molten drop came out of the pipette and caught fire before it hit the water



this is the finished product on my desk!



[Edited on 15-8-2013 by Pyro]

Very nice!!

Beautiful work Pyro! Not to sound like a broken record but, be careful, as I'm sure you are

Very cool!
I'm puzzled, are those needles in that photo with the cold water?

Just be careful, and keep those beakers secured by clamps or small bricks. You don't want to flip that. I know the chances for that to happen are small, but the consequences are grave, so procedures that might sound like an overkill are in fact perfectly normal.
Oh, and remember not to heat it too much. I know it speeds up the cleaning process, but together with high concentration of chromic acid, you actually lose the phosphorus itself. The original procedure takes like a week or so, at room temperature, in the liquid state, just to minimize the loses. You have lots of RP so you don't have to care too much about that, but remember that it can start boiling, and you saw what a tiny liquid blob does outside water. Now imagine a lava lamp like behaviour >100 °C. Pretty sight, if conducted in a desert.

[Edited on 15-8-2013 by Endimion17]

Certainly, go ahead. I don't hold any patents.

That thing with the needles is interesting. The only time I've seen phosphorus crystals is when I left an extremely clean sample etching in the chromic acid for a long, long time. It kind of reminded me of surfaces of Europa and Enceladus, but more ordered.

Nice work Pyro. The last picture looks like two sleeping baby Draculas