Would be interested in reading that ref. Could be a good earner that could.

I KNEW I had a reason for grabbing that brand new microwave I found dumped/left unattended outside tesco ages back...

Its been sitting on my bedside cabinet for ages, serving as nothing better than a gun and med cabinet, and to keep the stuff I use at night to block out sensory input on the top.

I think there might be a couple of coins fallen down the slats in the top though...I do hope it doesn't fry itself extra crispy for that. Although if it starts sparking and kicking off a storm, I guess I could hack the top off with an angle grinder, take the loose change out and braze the top back on with some high-melting silver solder, I have some at hand, as its something I use quite often, although the cadmium content is a little worrying, in terms of what a microwave might do if it starts getting uppity and decides to vaporise bits of whatever gets added on.

no this isnt correct, what sources have i posted before??

No specific supplier is made reference to at all on the page i linked. that would require being signed up, and even then the supplier could be anywhere in the world, it was the "custom made products" page, you can even draw your own

The reason i linked it was because the site has a huge database of chems, whether they are available or not.

Quote from the site
# 1.Our product library, the world's largest with nearly one million CAS numbers.
# 2.Our strong promotion effect, around 500,000 products ranked Google home page.

Have you tried this? It seems like using Phosphates in a similar setup would be better then H3PO4. Using the Sodium Hexametaphosphate is not hard at all. Its capturing the Phosphorus that is problematic which means it should be done on a large scale. This is not exactly something im ready to attempt large scale however.

I know the hexametaphosphate i think.. they use a blowtorch right?

how is capturing the phosphor difficult in the other method?

its fairly simple set up, just a canister in the microwave the inert gas runs in and out of the top of the vessel, catches the P and takes it straight into water.. is that how they are capturing the P doing it over there?

If yeilds are 30 to 50% then it wont take much to make a hundred grams or so.. which would last someone a while, i could imagine with a good little setup you could run upto 700 mills in a vessel



I attached the ref below

you gotta re read the ref

specifically there is chart stating yield goes UP with more heat. the more the wattage, the more yeild. check the chart.

into a 1 liter sized rxn vessel goes 200mL of H3PO4..

Picture this

The reaction vessel might look like a thermos, with 2 tubes coming out of the top. So picture a cylinder about as round as your palm, and 10 inches high with a screw on lid. There are 2 tubes in the lid just facing up ways is ok. - 1 is an inlet, the other is an outlet. the inlet on the vessel goes through a copper pipe, directly up through a small hole in the top of the microwave, to that, a rubber hose is clamped, which leads to the argon tank.


The outlet goes from the lid of the vessel out through the side of the microwave, where a rubber pipe, (which isnt too thick and insulated), runs into a erlenmyer or an rbf, containing 500 - 700mLs water. Into the lid on the catchment, it might be a good idea to stuff the opening, around the ruber tube with some fliter type cloth as the gas will be nasty..


The vessel containing 200mL 86% H3PO4 and the carbon catalyst (not sure if that is necessary) is placed into the microwave- set on high. The gas is set at a steady rate and begins bubbling the water.


The reaction runs for a good few hours, and high heats will only be reached if you use the right material for the vessel. In which case, the liquid in the vessel will begin to boil off slow because good insulators take longer to heat. The initial liquids will be taken with the stream of gas, into the catchment, mixing with the water.

After a couple hundred degrees is reached all of the liquids will be gone, from there, the vessel contents get hotter and hotter (but dont oxidize due to the gas) the inert gas catches the RP vapors as soon as they form, which, with microwave thankfully is low temp.. The P deposits into the catchment and sits on the bottom.

The white, or yellow P wont be miscible with the water.. Everything else will be.


No refluxing.. You are heating a solid once the initial liquids boil away.. Left in the bottom of the container will be crap..

This sounds easy enough i could do it in an afternoon.. But like i have always said.. This stuff is my specialty.. Metal is harder to smash  

ps
I havnt done this, but that is what i got from the Ref.. read it for yourself and correct me if i missed something.. believe me, i have done harder sounding things with equipment setups.. this is one of the easier ones!

thats why i was thinking Mw oven... but your post cleared a few things up for me. makes more sense..

 i like this idea of mw chem.. gear the spinning plate in my microwave so 1 rotation spins a gear several times.. then attach a magnet and use the base as a mag stirrer.

it would be good to be able to vary the temperature accurately aswell..

ok yes thankyou salat..

i did know that microwaves dont really work well on solid materials which is why i was thinking sand wet with silicone or something. I re re read the ref and the quartz is used to allow microwaves to penetrate through like it is not there...

Reaching tempretures this high in a microwave will be difficult unless the vessel can keep in the heat.. it dissapates fast otherwise and we'll be there all day, thats why i put it together that the quartz must have something to do with the keeping in the heat.

Turns out sedit it right . the carbon is used to heat the vessel from with in, not a catalyst..

w/d huh?...  hmm is that public or do i have to sign up?   what ideas did they have for stirring? is stirring necesarry even in m/w distillations?

Microwave it will be able to generate a shitload of heat in a short amount of time by literally shaking every molecule of the reaction mixture at once.

this is what got me thinking mw distillation might not need stirring..

basically, it sounds like if we can control the power in a m/w efficiently, and monitor RXN temps, then we can have a killer way of distilling things right?

Oh and as for the quartz vessels, the fact that there is going to be viciously hot phosphoric acid (think sustained heating would eventually give P2O5? or is it just much too strong of a dessicant, being able to dessicate conc. H2SO4 says something, really...), or close enough, that will eat glass. And at that heat, I imagine it would do so very quickly. And as for what would happen once it got out of your glass vessel, its going to start A-burning its way south, and B-probably doing so in a cloud of blazing willy pete.

So good reason not to use ordinary glass in this case. Concentrated phosphoric acid eats glass. And if possible avoid most metals, iron, copper, aluminium, many will form phosphides, which liberate phosphine on contact with water or moist air. Bad news, as it leaves you with something none too pleasant to dispose of, which you can't rightfully just take and dump on the neighbourhood tip, no, you would have to add H2O and burn it off yourself...lovely job.

Will it attack fused quartz? it may not, soda-lime glass might well behave differently, and of course, borosilicate will in this case, react as soda-lime does.

It behaves in odd ways at times, quite unexpectedly, such as being attacked by hot H3PO4, molten lithium also goes right through it (I am guessing, through replacement of the Na by Li and thus altering the properties, such as MP of the glass.

Sedit, why would people post a knowingly full of shit writeup? it doesn't make sense to me why somebody would actually spend the effort required to type it up, if it was untrue.

Cheapskate shitbags.

I hadn't realised this was from a patent, but assumed it was a writeup by a clandestine chemist/gentleman scientist (the latter term sounds so much more civilized, does it not?)

I take great umbrage at scientists who spout a great torrent of horseshit, tidy it up with a few graphs and then present it to the world at large (or indeed at small, if there happen to be any chemhack dwarves reading, let it be not said that I am dwarf-ist) as a properly done respectable study.

Case in point, the absolute worst of the cunting ratbastard gutterfuck son of a syphilitic whore worst, take one 'doctor' Andrew Wakefield, a gastroenterologist, or rather, used to be, who in 1998, published a study on vaccines and the correlation between MMR vaccination and autism rates, specifically looking at latent measles virus infection and those of my people who have GI problems, such as sensitivity to certain foods (not coeliac, but a number of us for some reason seem to benefit from a gluten or casein or both-free diet, never tried it, don't plan to, as A-I don't like rabbit food, and B-I sure as hell don't want to become less autistic!, if anything, I would prefer to be more so than I am)

What did he do? christ H jesus on a pointy fucking stick, what DIDN'T he do, is more like it.

For one, he was in the pay of certain parties, who wanted certain results, which they duly got, to launch a business scheme intended to profit off a vaccine scare with 'dr' wakefield.

The entire paper was one giant, rather elaborate fraudulent heap of manure.

And for two, he 'recruited' autistic children for tests, involving amongst other things samples taken via endoscopy of the bowel, and spinal taps, even paying a fiver a time for blood samples at a kid's party to the guests (his own son's birthday bash, would you believe it?) (and a fiver? for blood? don't know about you guys, but MY blood is worth more than that, and for that matter, any autie/aspie's blood has to be worth more than that, it comes from one of us, so no shit, of course its going to be...what a sodding cheap ass!)

So thats fraud, child abuse, and child abuse of people who are better than he is at that (I'm not NT-bashing there, so no offense guys, I mean this particular lebensunwertesleben himself), bumming up to paid interests, poisoning the scientific well in general, threatening to sue a news reporter who covered, nay, hounded him as he justly deserved, in an attempt to get him to keep his mouth shut, and actually killing people, indirectly. The vaccine scare he successfully caused lasted a long time, and even now, in the backwaters of human(oid) stupidity there are plenty of the mercury militia out there who refuse to believe not only that autism isn't a disease at all, rather than a different set of neurological wiring, but that it is most certainly not caused by Hg, this leads people not to vaccinate, which leads to disease, which kills people (no shit)

And of course, the amount of bollocks he spewed, that got believed, and he is still at it, having slithered off to the states, after being struck off here in the UK, to become ex playboy suckjob queen, fugly sillicone-titted slapper Jenny McCarthy (actor jim carrey's ex piece of meat) and Autism Squeaks...err..speaks, sorry...my bad...spokesharlot.


Most cases aren't nearly so perdition-accursed awful as he is, but it goes to show, there are some real serpentine little frauds out there who will talk all manner of crap in order to look good in front of others, or make money.

The second, I can understand as a motivation, whilst most certainly wishing it, and them, stomped on with an iron-heeled boot until their kidneys squeak in protest, but in order to gain the admiration of others, that I genuinely do not understand.

If one tells a load of lies, to gain the respect of others, then whilst the respect might be genuine, one would know all along, that it was undeserved. Does that not feel completely hollow, and utterly, totally worthless to most people? to me, doing that would be akin to winning the lottery, and having somebody who to begin with, couldn't give a flying rats arse about you, suddenly start fawning and begging to lick your boots. I.E nothing but contemptible, deserving of being spat upon and nothing more. That, is how such admiration/respect or support would feel, to me.


As for phosphoric acid attacking sillica, how does that OH group behave, under strongly acidic conditions? as a protic acid, or more like an alcohol? think it likely that silicate esters would be forming? I'm going to hazard a guess that SiO2 is amphoteric, although I am not sure, most metals are, I'm not sure how metalloids like Si behave in that context.

Is the formation of a phosphoryl orthosilicate ester likely? although this would of course, judging from the behaviour of other such orthosilicate esters, such as the tetraethyl or methyl esters, hydrolyse to SiO2 either on contact with water, or at elevated temperatures.

Academic of course, when one is dealing with a meter-high plume of incandescent white phosphorus vapor/MW-induced plasma.

But hey, thats me. Although even I would start thinking about it AFTER I took care of the large, microwave oven-shaped hole melted into the ceiling and/or floor/walls

86% may work. You must keep in mind there is a competing reaction here where water and Carbon are converted to hydrogen and carbon monoxide meaning you will have to increase the molar ration of carbon well above that of the 16 molar excess they require. I would just use ALOT of carbon if I where you.

The hydrogen may be dangerous.

The reaction vessle can no be any form of metal keep that in mind. If so then Microwaves will never make it to the reactants inside. Borosilicate can't really take the 600 degrees C. You will need quarts or ceramics.