Preparation of elemental phosphorus

Quote: Originally posted by blogfast25

Silicates, like glass, tend to have lower melting points than actual silica...

Quote: Originally posted by Rogeryermaw

as usual blogfast, your science is strong! i need your youtube screen name to give access to the videos. [Edited on 25-9-2010 by Rogeryermaw] [Edited on 25-9-2010 by Rogeryermaw]

Quote: Originally posted by Rogeryermaw

this thought just occurred to me. when word gets out that P4 can be produced this way (mostly applicable to u.s. experimenters) NaPO3 may be as hard to get as P4. [Edited on 24-9-2010 by Rogeryermaw]

Quote: Originally posted by blogfast25

As long as we have access to phoshate, we have access to metaphosphate and as long as we have access to good old bones, we have access to phosphate. No worries, really!

Quote: Originally posted by Rogeryermaw

what i have noticed about the use of NaCl as a flux is that it seems to reduce the viscosity of the melt and therefore allows the P4 vapor to escape more easily thus reducing the necessary burn time in the furnace. cut my time in half at least.

Quote: Originally posted by Magpie

We should remember that the key to Charles Hall's breakthrough discovery of how to electrolytically produce aluminum was his use of cryolite (Na3AlF6), a liquid producing flux for the Al2O3 ore. Possibly use of other fluxes in Roger's technology could prove advantageous. Specifically I'm thining of CaF2 and cryolite. CaF2 is readily available from pottery supplies distributors. Cryolite may be available there too. Also there are other fluxes, as any good book on pottery will show. I would experiment with CaF2 in my ceramic tubes if I wasn't concerned that it would eat a hole right through them.

Quote: Originally posted by Magpie

But I was under the impression that many fluxes used for ceramic work are successful because they lower the melting point of both the substrate and the flux, the ultimate being a eutectic composition.

Quote: Originally posted by Magpie

@Roger I wanted to add my twist on air flow regulation: Place a tee in your airline, using the straight section for the airflow to the furnace. On the branch leg place a valve, ideally a globe type for finer regulation, but a ball valve would likely suffice. The airflow then is easily controlled by how much you spill through the valve on the tee. [Edited on 27-9-2010 by Magpie]

Quote: Originally posted by Rogeryermaw

one of the ways they make it [Edited on 27-9-2010 by Rogeryermaw]

One of the ways? It seems to be the ONLY way most of them know. That recipe is over a century old.

I don't mind if drugs are Hofmann's problem child, but I do mind when that child cuts the phone off harvesting the copper. If you hear a can of 9% larger fall from about telephone pole height, that's more likely the lesser spotted, reclusive heroin addict out foraging for berries; addict slang for scrap metal.

With all this furnace talk, have you guys read Dave Gingery's "How to build a gas fired furnace"?

I bought it when I was about 14, along with "How to build your own lathe".

The gas fired furnace one, he tells you all about making your own refractory from firebricks, clay and other things. There's a blue print for a working out the book furnace with a removable lid, and instructions on how to make the formers and ram the refractory. As well as details, drawings and measurements for building a centrifugal blower and some rough information on green sand casting.

The blower, you may as well buy one or scrounge one from the tip (modern combi boilers have a £100+ high heat one in the top, and the boilers end up at the metal scrap yards; ask for 'berries' and remember to say 'berry merry munch' when the deal is done).

The furnace dimensions and details are easily changeable. If you google for anything like DIY / Furnace / Gas / Dave Gingery / Gingery you'll find tons of pages. And there's the hobbicast group on yahoo groups.

I just thought the design could be easily manipulated to make a more permanent retort furnace.

I've read the book tons already and it's just been sat on the shelf for aaaaaaages. As a thank you for making the video and letting me watch it, you can have my copies for free if you like Roger.

I just found my refractory bricks and an empty propane can.

[rquote=188511&tid=65&author=peach
One of the ways? It seems to be the ONLY way most of them know. That recipe is over a century old.

I don't mind if drugs are Hofmann's problem child, but I do mind when that child cuts the phone off harvesting the copper. If you hear a can of 9% larger fall from about telephone pole height, that's more likely the lesser spotted, reclusive heroin addict out foraging for berries; addict slang for scrap metal.

[/rquote]

man that is more real than you know. there was a trolley system in downtown that has been shut down because the wiring has been ripped out twice and on the news(when i was working on the spawar contract building security equpiment for national guard aviation bases) in hawaii about the (i think it was the H3 highway) new highway construction where the ice heads stole the wiring for the new lighting system along the highway...they have no scruples at all!

^^^^^^^^^^^^^^^^^^^^^^

That reminds me of when we made yogurt in Chemistry and someone astutely asked, "Why was he eating the white curd on a cow's tits in the first place?"

[Edited on 30-9-2010 by peach]

Quote: Originally posted by Strepta

@Rogeryermaw: Roger, you stated earlier that the NaCl reduced the "burn time" in your furnace by about half. How did you determine that the reaction was complete? Are you listening for the gas bubbles in the receiver?

Quote: Originally posted by Rogeryermaw

a few things that come to mind are the reactor for one...how much may still be trapped inside? the collection method is losing quite a bit to atmosphere as i stated already since i am counting on vapors condensing in such a short distance and with minimal exposure to the water since we feared the possibility of a steam explosion. there are certainly many factors to be improved. given time and trials the numbers can certainly be improved upon. i should have weighed the product from the last run. it is my belief that my percentage of theoretical would be closer to 19-20%

I agree with bloggerman, and was about to suggest that before reading his reply. If the bubbling stops, it signals the end; theoretically. But there's a good chance some of it is still hiding in the actual melt it's self. Quite a lot from those numbers.

On the next run, I'd look for phosphorus trying to escape the collector; test for it, don't sniff . If any significant amount is found, you could try cooling the collector, like in the metalresearcher sodium thread.

If no real value is escaping, it's got to be in the melt still. Have you tried roasting for any period of time after the bubbling stops? That's a bit of a weak suggestion.

It may need more heat for a higher temperature, or something to push it to the collector, the same way a Dean-Stark needs the water gone to drive it through to the right side of the equation; this may need more heat to drive it out of the melt and to the collector (?it's absorbing in the melt? Hydrogen chloride absorbs nicely in water to hydrochloric, but then comes back out at room temperature for strong acid and all of it is out once the water is gone or the temperature is raised).

From all the gas work I've done, I do know that you have to massively bias the amount of gas you're using over the theoretical for it to absorb properly. They just don't function like liquid / liquid reactions in terms of the theory, unless they're run INCREDIBLY slow and gently, with frits and such. Maybe you could add a frit of metal sponge to the end of the pipe. I know where you can get some aluminium sponge for free. But, as I've learnt with all my gas wash bottles, that's not always a good thing. As they tend to clog. And clogging, mid anhydrous, pressure producing work involving the reactive gases is not good in anyway!

Before even trying the flame method, I'm already wondering about using electrodes and arc welders.

Again, forget worrying about 13%. A total organic synthesis can yield 1% and below after a huge amount of work by genuinely the best chemists around. It doesn't matter when the things going in and process are cheaper than some beer. And when it's only the first few tries.

{EDIT} I just had A THOUGHT! When I'm trying to truly capture a nasty gas from a reaction, like hydrogen chloride, I don't just use water. I use a base in the wash to salt the gas out; as the acidic gas will neutralize with the base. It works so well I can't smell / feel anything, even with my nose against the exhaust. If absorption was a problem at the collector, maybe you could use something similar. Make it faaaar more favourable, energetically, for it to stay in that collector, but in a form that can be easily extracted afterwards. This same trick works for horrendously toxic materials, and it's how they do things industrially where fume hoods don't mean anything. {that EDIT tag seriously annoys me, yeah one, fine. But having to constantly edit an edit tag for missed spaces and spellings....}

To liven things up, here's a funny video for all you welding and fire fans (me included);
<object width="660" height="525"><param name="movie" value="http://www.youtube.com/v/G6Uxh-xtU-g?fs=1&amp;hl=en_GB&amp;color1=0x5d1719&amp;color2=0xcd311b&amp;border=1"></param>& lt;param name="allowFullScreen" value="true"></param><param name="allowscriptaccess" value="always"></param><embed src="http://www.youtube.com/v/G6Uxh-xtU-g?fs=1&amp;hl=en_GB&amp;color1=0x5d1719&amp;color2=0xcd311b&amp;border=1" type="application/x-shockwave-flash" allowscriptaccess="always" allowfullscreen="true" width="660" height="525"></embed></object>

You think that's enough juice? It's enough that they have to talk with the grid before building and starting one of these up. It's a good 1% of what the fission stations can actually output, flickering on and off as the arc makes and breaks. Can't get enough of the sparks, fire and grid hum. I like the way they've got some pop music on in the quiet control room, watching it.
<object width="660" height="525"><param name="movie" value="http://www.youtube.com/v/ijWwfcw0FOo?fs=1&amp;hl=en_GB&amp;color1=0x5d1719&amp;color2=0xcd311b&amp;border=1"></param>& lt;param name="allowFullScreen" value="true"></param><param name="allowscriptaccess" value="always"></param><embed src="http://www.youtube.com/v/ijWwfcw0FOo?fs=1&amp;hl=en_GB&amp;color1=0x5d1719&amp;color2=0xcd311b&amp;border=1" type="application/x-shockwave-flash" allowscriptaccess="always" allowfullscreen="true" width="660" height="525"></embed></object>

[Edited on 30-9-2010 by peach]

Quote: Originally posted by peach

On the next run, I'd look for phosphorus trying to escape the collector. If any significant amount is found, you could try cooling the collector, like in the metalresearcher sodium thread. [Edited on 30-9-2010 by peach]

Quote: Originally posted by Rogeryermaw

it can be cut and peeled off the mass of slag without too much hassle. when a heavier vessel is used it may prove more challenging. i think another run in more controlled circumstances is called for with more stringent data records.

Quote: Originally posted by Rogeryermaw

it also occurs to me that some of the reaction may not be as straightforward as i have been assuming. there may be significant losses to the formation of metal-phosphides as part of the slag. that, to me, would be an acceptable loss since it is the use of a reactive metal that has brought the whole concept of phosphorus production within the reach of home experimenters. i wonder if using the excess aluminum is contributing to this... upon further study this seems very likely since AlP is sold as rodenticide under trade names: Celphos, Fumitoxin, Phostoxin, and Quick Phos which are produced by igniting a mixture of phosphorus and aluminum.

it also depends on how the reaction proceeds too. does all the P evolve then react with excess Al or do these reactions proceed simultaneously. in the first instance a stoich amount or less would be favorable. in the second instance it seems that both P and AlP would be formed regardless of quantity of Al. would be nice to have a way to analyze the slag but i don't think i want to toss it in water and see if it kills me(since metal phosphides release phosphine when wet). any other ideas for analysis? perhaps i could catch a mouse and put it in an aquarium then powder some of the slag, place it in the aquarium and wet it then cover the top(outside of course). homemade pesticide anyone?

you animal rights guys can piss off before posting. i live in the country and mice are a problem as it is.

[Edited on 1-10-2010 by Rogeryermaw]

These are the exact ones I have;

ONE!
TWO!
THREE!

HA, AH, AH, AH!



If you go on eBay and search for "0.01g" / "jewellery" / "jewelery" / "scales" a whole ton of them will turn up. A lot of them are probably from the same factory with the same circuit and weigh bridge in them. Those ones I bought are some of the cheapest on there.

You'll need to get a set to weigh the 10g results and definitely the oxide from a sample of the melt. It's not the RESOLUTION that matters, you don't need to know the 10g numbers to 0.00000001g, but the ACCURACY. Those digital kitchen scales could easily be off by a gram or two at 10g (see the graphs at the end).

Maybe I should buy a whole bunch of these things, produce curves for them on the 0.1mg balance and resell them so people can get cheap, accurate balances with known errors.

You shouldn't need to weigh the water, just the sample from the melt and the resulting oxide. I'm off to watch the UK fireworks championship, day two, so I can't find the numbers right now, but it could really do with working out a safe / measurable sample to use from the melt, assuming it's all hiding as AlP and will go to phosphine. E.g. not the entire melt, but enough that the oxide will show up as a solid number on one of those cheap scales.

I remembering reading, quite randomly whilst wandering around the library in my teens, a book on military warfare. Where they discuss how chemical weapons need their lethal doses multiply up by tens of thousands of times, or more, when dispersed into the air, because they'll dilute down so much before they ever touch someone. The way to test for the AlP safely would be to use a smaller sample and do it outside, downwind, as you're aware.

Graphs I will post up with more explanations at some point; click to get the full version (don't want to make the forum look all spazzed out posting them full size here)

This is my Made In China 0.01g scale (in red) and the digital 1g kitchen scale. The scales on the left and right are not the same. Notice that the;

a.) 'drug dealer' scale is almost always permanently biased to a give a positive result, don't tell them that
b.) error doesn't massively grow or shrink
c.) pattern of error isn't very predictable
d.) 1g kitchen scale is HORRIBLY inaccurate at low numbers
e.) error DOES shrink for the kitchen scales, considerably, and conveniently, as the 0.01g scale cuts off (you can get 100g versions of these 0.01g things, perfect combination according to this graph)
f.) there is quite clearly a periodic swing from positive to negative for the kitchen scales once the mass being weighed goes over 50 - 100g

Scale comparison

Here I'm measuring the mass of all the 20p's, I think, from a big jar of change. I've done it for 1, 2, 10, and 5s as well. Notice that the;

a.) mass of the coins 'on the street' seems biased towards being more than their minted mass. Meaning gunk is building up on their surface quicker than they're wearing down (oxides, salts, greases etc)
b.) it's swinging in a periodic way, up and down, every few years and the coins that are decades old have about the same error as those that are new. So the main error in mass is controlled by the minting accuracy, not handling. The sine wave is the mint tweaking the presses and changing the dies for the coins. Importantly, it's periodic and swinging by roughly the same amplitude, positive and negative.

Errors in coins mass

If I take a stack of ten or twenty coins, randomly out of the jar, the errors begin canceling each other. When I sum up all the errors, this happens...

The % to which I can predict the mass of the stack of coins drops waaaaay down; multiple readings and error canceling.

Some of the cells on here look a bit wonky, hence me not posting it as a final thing yet, I need to finish it off really.

Important numbers

If anyone in the US would like to send me a jar full of low value coins, I can do the same for the US. I'll need 10 - 30 of each value for it to give a good result. I also don't know if they'd vary much from state to state, or if it's all coming from roughly the same mint or at least others controlled to the same standards as each other. I expect it is, or coin operated machines wouldn't work.

What's good about using low value coins is the mint controls the main error, tightly. Everyone has access to it, even tramps. Best of all, the canceling works better the less effort you put into sorting the coins, it works best with an entirely random selection of dirty / shiny, uncleaned coins and from various, random dates.

[Edited on 2-10-2010 by peach]

i will get to the more important numbers and testing soon but here is some preliminary data.




the initial weight of the reactants was about 217g and post reaction almost 200g give or take (scale accuracy)






mass as removed from can (minor losses due to the brittle nature of the slag)



appearance of the inside. note the gas pockets. smelled terribly of phosphorus when broken open(wasn't trying to sniff it but couldn't help catching small whiff as it was very strong.




prepping a small piece to test for formation of PH3.
sorry i did not snap the process as i was nervous enough about TRYING to produce something deadly. was hard to tell for sure but i wet the ground mass in a pickle jar and placed a propane torch over the top. the water appeared to cloud during this but i'm not sure if that indicates absorption of P2O5. i did, however note greenish yellow deposits that fit the physical description of AlP.

based on the weights the reaction mass lost 17(ish) grams leaving 10-12 grams to account for after subtracting the estimated weight of phosphorus collected.

[Edited on 2-10-2010 by Rogeryermaw]

Quote: Originally posted by Rogeryermaw

thinking back to the first successful run i would say the AlP formation is certain. remember how i said that it popped in my hand as i was trying to clean out the reactor? with audible report and a visible flash? i quenched it after the run thus getting the inside of the reactor wet.

Quote: Originally posted by peach

The boria thing may not be a simple case of the dry reagent costs. If it can be run at a much lower temperature, as strepta suggests, that alone may outweigh the extra cost by simplifying what's needed. For instance, it could be heated with nichrome wire perhaps, on a desktop, as opposed to needing a furnace outside. [Edited on 2-10-2010 by peach]

the first things i'm going to try are stoich amounts of reactants and i have a few ideas for improving collector design. i think just by giving the vapor more time to reach the water and allowing it to cool a bit before it gets there will help control loss to air. this could significantly increase yield. my observation after running the experiment at night(the darkness allowed me to see the burning P vapor escaping from the lid) leads me to believe this is one of the areas of the system that can be improved upon the most.

on a positive note i did something for my safety and health today. my wife is bringing me a case of nitrile gloves home from work tonight and i picked up some neoprene gauntlets(almost elbow length). i also picked up a face shield and have a set of z-87.1 goggles.
next i'm going order one of those soviet era gas masks with replaceable cartridges...hopefully i can find cartridges that handle solvent and acid fumes...after that all i need (besides fume cabinet) is a good apron(and a lab coat to look the part)





[Edited on 3-10-2010 by Rogeryermaw]

I should girl it up on the sewing machine and make you an aramid & nomex onepiecey, that'd make a god damn awesome SM picture.

Before going to crystallography and such, it'd probably be worth looking for the phosphane again. Although, in terms of waiting for it to get through the post, the potential complaining that may occur if they manage to break the packet and spill the contents (no matter how well packed) and the time it'd take me to check it, it may be worth having a fiddle with the collector and reactants first, then upgrade to international collaboration if that stumbles as well.

If it has gone to some metal phosphorous compound, I wonder if there'd be an easy method for reoxidizing it to elemental phosphorus, without ending up with oxides or a gigantic bill. It's used as a phosphorus source in semiconductor labs, like Silane is for Silicon. I think they get the silicon back out on it's own with high temperatures under inert gas.

The boria thing, I have zero evidence of blogfast, just that Strepta mentioned it. In my rapid reading, I thought he was saying it starts producing at a lower temperature, but he does say it MELTS at 450C (which of coarse, isn't running and you're likely right about the P2O5 disassociation). What temperature did you have to run it up to Strepta?

If it melts and takes the phosphorus source into solution with it at 450C, I wonder if some form of electrolysis could then be used.

Quote: Originally posted by peach

The boria thing, I have zero evidence of blogfast, just that Strepta mentioned it. In my rapid reading, I thought he was saying it starts producing at a lower temperature, but he does say it MELTS at 450C (which of coarse, isn't running and you're likely right about the P2O5 disassociation). What temperature did you have to run it up to Strepta?

Quote: Originally posted by peach

If it has gone to some metal phosphorous compound, I wonder if there'd be an easy method for reoxidizing it to elemental phosphorus, without ending up with oxides or a gigantic bill. It's used as a phosphorus source in semiconductor labs, like Silane is for Silicon. I think they get the silicon back out on it's own with high temperatures under inert gas.

Quote: Originally posted by Rogeryermaw

the first things i'm going to try are stoich amounts of reactants and i have a few ideas for improving collector design. i think just by giving the vapor more time to reach the water and allowing it to cool a bit before it gets there will help control loss to air. this could significantly increase yield. my observation after running the experiment at night(the darkness allowed me to see the burning P vapor escaping from the lid) leads me to believe this is one of the areas of the system that can be improved upon the most. [Edited on 3-10-2010 by Rogeryermaw]

Quote: Originally posted by Rogeryermaw

no unfortunately i haven't added that bit of equipment to my cache yet. my temps are estimated by the color charts available from metal working sites such as this: http://www.blksmth.com/heat_colors.htm

Stick a bit of copper in there roger and you'll be able to see if it passes the melting point, without having to buy a thermocouple for a rough idea.

You must have a bit of copper lying around.

If not, I know where you can get some...

already done that. i had a copper bottomed pot i set over the furnace to see what color the steel would get to...it's not copper bottomed anymore...

Quote: Originally posted by peach

I should girl it up on the sewing machine and make you an aramid & nomex onepiecey, that'd make a god damn awesome SM picture.

don't you mean S&M picture?

Quote: Originally posted by aax

After a few experiments I have decided that silicon dioxides main purpous in the reaction is to give the mix a thicker consistancy which slows down the reaction.

Quote: Originally posted by blogfast25

Quote: Originally posted by aax   After a few experiments I have decided that silicon dioxides main purpous in the reaction is to give the mix a thicker consistancy which slows down the reaction. Are you possibly a troll, aax? If you've actually carried out any experiments and have drawn some conclusions based on them, then please report. Otherwise, please kindly eff off.

Quote: Originally posted by Rogeryermaw

if delivery of vaporized phosphorus is not submerged you will certainly have to use inert gas or it will all be lost to atmosphere. there is no delay time to the ignition of phosphorus in vapor or even liquid form. if it is warm enough to be in a liquid state it will ignite instantaneously. as far as a spray nozzle i would fear pressurization creating an unsafe condition though i won't discount its possible value without trying it. beware the ignition of liquid phosphorus. you don't want to be close to it. it snaps and pops throwing flaming globs of phosphorus a good distance and the burns it can cause will turn necrotic. they are very slow healing. also cooling your collector may be advantageous but i would refrain from using ice. if your product solidifies in a closed system it will greatly frustrate your attempts to recover it. remember that phosphorus is deadly toxic and the less handling the better. i look forward to your experimentation results.

Quote: Originally posted by Rogeryermaw

minor break but i'm getting low on aluminum. i just ordered a huge cache of chems and gear (though i didnt get aluminum, i'll melt some down and attempt to atomize it myself in the next couple of days).

Quote: Originally posted by Eclectic

Does anyone know if phosphorus is heated by microwaves? If not, a carbon/phosphoric acid reactor and phosphorus condenser totally internal to a microwave oven might be possible...

Quote: Originally posted by Eclectic

Blogfast, havn't you seen the threads on microwave furnaces? The carbon in the reaction mix is a microwave susceptor and will get up to white heat. Of course it would need to be insulated. The question is, would the resulting phosphorus be heated by the microwaves as well.

This guy I was talking about was using domestic microwaves. With them being free from the tip, it's not a problem if you break one in the R&D phases. I can't remember what he was doing to make it work though! What he was using in terms of the absorbent.

Obviously, modifying microwaves at home, almost a kilowatt of invisible radiation emitting death, you better known what you're doing! Or you'll steam your eyes and brains to al dente without even feeling it.

Resonance and diffraction are a good place to start.

I wouldn't be too quick to dismiss domestic microwaves. From what I understand, the main advantage of a laboratory microwave is that they can produce single modes. I'm sure I remember reading published papers that were using domestic microwaves. A fridge pump versus diaphragms style debate.

Anyway, this way beyond where it should be. Something more basic is afoot with the yields than flames versus microwaves. A lot of what I've read about microwaves in the journals hasn't been eye poppingly impressive, as of yet. I've read one paper that is straight out incorrect, and I'm wondering how it even got published. It claims catalytic activity, yet absolutely there is absolutely NOTHING catalytic about it.

Also, if you start using microwaves for the P method, what are you going to use as a crucible? Even if it absorbs the microwaves, what's it going to do around the multiple ingredients, over a thousand C? Then you've got a whole other kettle of nasty fish to think about.

Nah, flames, hot wire elements and arcs until it's producing something over 50%. A simple demonstration is, they use arcs commercially. If it was more efficient to do it with microwaves, the commercial guys would almost certainly be onto it.

[Edited on 12-10-2010 by peach]

before i had any successful experimentation, i had the thought to use the microwave method. like peach said, it is easy to get a very cheap or even free microwave. the thought i had was to use a hole saw(about half inch) since the controls and circuitry are normally on the right, cut a half inch hole through the left side panel and use a file to fit the holes to the neck of a glass retort.



my only concern would be if the heat would destroy the retort or could we find a suitable reducing agent that reacts at lower temp. and, of course, cutting a hole in the microwave might be dangerous... any thoughts?

My thought is, you seem very good in paint.

I particularly enjoy the care put into creating the buttons and display.

The file to fit idea is good, the microwaves shouldn't be able to escape through that, unless the retort is made out of something transparent to microwaves. If it is, you'd need a cage around the collector, made from the screens in the windows of some other tip microwaves.

If you're DIY'ing the screens, you also need a microwave meter to check they're working.

One way around that is to surround the collector with the inside cavity of another microwave, then make sure everyone is a very long way away.

No idea about how it'd work, it'd be easier to try it in the real world. But I still think the flame method should be performing better before going microscopic on the heating.

The flame method is performing too poorly based on your results for it to be a matter of heat. It's the melt or the collector.

I'd try arcs before microwaves. Microwave transformers can be rewound to provide pretty much whatever you like at a few kW. And you can harvest carbon electrodes from old Zinc or Alkaline batteries.

I need to stop talking and get busy trying this myself but, at the moment, I'm covered in expanding foam, after a can of it burst mid a seriously DIY event; I now have a mushroom of urethane foam growing out of the back room floor. Not to worry, the floor sander will sort that.

[Edited on 12-10-2010 by peach]

well it's just tossing ideas around right now. nothing i will try right away. i think i would rather expend energy trying to make the equipment i have now more efficient. does aluminum block microwave energy? i wonder because we have all seen the arcing of an aluminum foil ball in the micro. does that not represent the waves bouncing back and forth on the metallic surface? if so then could not the entire neck and collection equipment be wrapped with multiple layers and sealed with aluminum ducting tape? or use a smaller microwave than the reaction machine, remove its door and place it against the side of the one the reaction is running in then just seal the cracks?

nothing i am wanting to try right away...just tossing off...some ideas

ok now i have a thought about what may be happening in the reaction with NaPO3+Al+SiO2...i believe bloggy to be correct about the formation of Al2O3 taking precedence due to its HoF driving the reaction but what happens to the rest of the aluminum after the O2 has been scavenged from the other reactants? it has nowhere to go but to combine with P until the aluminum charge has been exhausted...need to do some equilibrium work on this but it may just be an issue of being more precise with stoichiometry. i know we talked about this but i think it's time for another test. that may be why there was an unpleasant stench of phosphorus (possibly AlP or PH3) when breaking open the slag but no smoke as of phosphorus residue oxidizing. the smell of P2O5 is not as unpleasant as that mess was...

honestly fellas i'm not trying to get this crap in my lungs! i have been doing all my work outdoors but phosphorus and its compounds obviously have VERY powerful odors.




[Edited on 13-10-2010 by Rogeryermaw]

As Panache says, a folded box would do. Aluminium will reflect it yar. In terms of simplicity, the foil idea is good, but it'd be quite easy to end up with leaks or have them form mid micronuking, so I'd go with getting a second microwave and chopping a hole in the side of it for the collector. As you can weld, and the enclosures are steel, you could weld the two together.

Microwaves from an oven can't escape a metallic enclosure provided the gaps are the same size, or smaller, than the ones on the grill covering the window. They have a long wavelength, so the grill looks like a solid surface to them. That's why phones are shit in terms of signal, they're "line of sight" radios, that really need to be able to see the next station. And the signal is strongly absorbed by all the water in the atmosphere. Hence the phone companies wanting to put masts everywhere, to reboost the signal and resend it to the next one. Saying that, a phone outputs not a lot of energy compared to an actual microwave, so the absorbency thing is not reliable. But the reflection is.

At one point, for reasons unknown, I placed an upside down wine glass in the microwave and then a Smartie sweet on the upside down base. When I returned a minute or two later, the glass had actually melted. I wasn't drunk either.

Since you're dealing with something genuinely toxic, you could pick up a respirator from eBay. You will have to out bid the weapons guys who want another one to hang on the wall and the kinky pReverts buying them for sex games, who'll probably strap a massive dildo to the intake on arrival (I have seen this). There is a fun respirator fact at the end.

I will continue filling cracks, in the walls, and have a think about the experiment and if I can easily check that melt (if you still have some lying around).

{respirator shenanigans}
After the twin towers maga fail, people went nuts buying respirators, thinking they were about to be chemo & bio attacked (places were selling out of them they were going so quickly). But a number of people have actually killed themselves putting respirators on and then forgetting to remove the covers on the cartridges, suffocating themselves but thinking they're being gassed. An operation that is as complex as, put it on, remove covers. The irony is quite outstanding, and fits well with my opinions on safety gear often becoming more of hazard than the original problem.

{edit: wavelengths}
The microwaves thing is kind of related to semiconductors. They produce the billionth of a meter transistors by shining a beam through a stencil onto the silicon. They want the beam to pass through the tiniest gaps possible. Even UV has too long a wavelength now, so they use electron beams. In another strange bit of science, solid objects can be treated as waves as well. By accelerating the electrons to very high velocities, the wavelength fits through the stencil. If they move fast enough, they can teleport through the stencil (seriously). That's how the memory in most digital electronics works now. So, theoretically, if you run fast enough at that wall, you'll teleport to the other side without actually breaking through it. Nice.... I have an evil scheme, suggest this to the next meth user you meet. "Just run REALLY fast! You almost did it last time!"

John, out

[Edited on 13-10-2010 by peach]

Quote: Originally posted by Rogeryermaw

the thought i had was to use a hole saw(about half inch) since the controls and circuitry are normally on the right, cut a half inch hole through the left side panel and use a file to fit the holes to the neck of a glass retort.

Quote: Originally posted by peach

As Panache says, a folded box would do. Aluminium will reflect it yar. [...] Microwaves from an oven can't escape a metallic enclosure provided the gaps are the same size, or smaller, than the ones on the grill covering the window. They have a long wavelength, so the grill looks like a solid surface to them.

Quote: Originally posted by peach

Obviously, modifying microwaves at home, almost a kilowatt of invisible radiation emitting death, you better known what you're doing! Or you'll steam your eyes and brains to al dente without even feeling it.

Quote: Originally posted by Rogeryermaw

ok now i have a thought about what may be happening in the reaction with NaPO3+Al+SiO2...i believe bloggy to be correct about the formation of Al2O3 taking precedence due to its HoF driving the reaction but what happens to the rest of the aluminum after the O2 has been scavenged from the other reactants? it has nowhere to go but to combine with P until the aluminum charge has been exhausted...

This is obviously starting to ask a lot of one guy (he's basically doing all the hard work), so I'm 100% happy to muck in with testing the melt and will commit a fair amount of effort to it if we can devise a solid method for checking it.

Testing it for AlP would be one of the firsts. I have a ton of gas handling stuff, am used to dealing with them and have the super balance and a respirator is in the post with some cartridges (I need one to sand the damn floor for a start normal dust masks leak too much over the 6h it takes).

More ideas for practical tests are needed. We may also need to make a group effort with the chemicals.

[Edited on 13-10-2010 by peach]

Quote: Originally posted by blogfast25

Roger, that just doesn't happen when you're in near stoichiometric conditions

i'll have to look back but we had discussed using an excess of Al and up till this point that's what i have been doing. on the next run i will reduce that to stoich or perhaps 1-2% less. i really don't think there is much elemental P in the slag. if there were it would smoke upon being released through grinding. and since i had been using an excess of Al, that is the main reason i figured it was reacting with the top portion of the P being evolved in the main reaction.

all this talk of microwaves, while intriguing, is only conjecture until i put more work into the methods we are trying now.and i have no fear about escaping radiation. i'll put that bitch in the back corner of the yard and stay a couple hundred feet away while its running. c'mon we've all seen the retarded series "is it a good idead to microwave this?" on you tube. those idiots are still alive!

and microwaving my gonads may just be beneficial...i already have two kids i can barely handle and they won't be out of the house till i'm too old to party properly. definitely don't need more!

[Edited on 13-10-2010 by Rogeryermaw]

Have you seen the episode of Southpark where Stan's dad discovers he can get weed legally, provided he has cancer. So he takes up smoking, sunbathing, drinking and microwaving his balls, then ends up bouncing around town on a space hopper permanently high, with all the women looking at his now bowling ball sized balls?

I was just checking your numbers. Keeping in mind that I've been on my feet for over 12h today painting, wiring plugs and endless other boring, rage inducing shit, and that I'm now getting a bit drunk prior to having a sleep, they seem pretty much okay. There is no huge excess of Al that would explain the lack of P in the result (from what I can see from some very rough calculations; I'll probably try checking them tomorrow depending on how quickly I start working again). The result is off by an order of magnitude, that is a darn big difference. Kitchen scales, after my examination of the anti-fatty Weight Watchers set I have, are not very good at all below 50 - 100g. But I'd be mighty surprised if even they weighed out 0.9g in place of 9g. You could easily see that with your eyes, without even picking it up.

You are in the realms, however, where kitchen scales are probably going to give poor results, 10% inaccuracies. They need about 100g on them before the error drops to a low percentage. 9g, whilst it's not going to weigh out 0.9g, I'd expect it to make about a gram or two of error on that. Anything between 1 - 50g, expect about 10% error from the kitchen scales, and it will decrease as the weight goes up to about 1%-2 or3% at 100g.

I still think there's something more afoot here. The scales aren't great, but they're not THAT far off. And the reactant masses aren't massively off either. Yet the yield is.

Nail the collector if you run it again soon, get that out of the equation. If you reduce the amount of Al and it's still doing it, it has got to be the melt. And I'd vote temperature and it not being driven to completion or fully out of solution. Again, arcs are fearsomely hot. Hot enough to start messing with the special refractories if too close. If it yielded the same amount with flames, they'd probably switch to that, as a gas flame is cheaper than an arc in terms of fuel (the electricity needs the gas / coal to be burnt, then converted and transmitted, then down converted, all involving losses and expensive power plants).

Have your younger Rogers started drawing on the walls yet? Kids are funny. I'd rather they drew on the walls than adults left dirty hand prints all over the place. Adults should know better, and the scribbling on the walls is at least colourful.

Quote: Originally posted by Rogeryermaw

i did some looking back at my records and it seems that i have been doubling the stoich amount of SiO2. presumably the excess O2 is turning the P into P2O5 yes no?