Sciencemadness Discussion Board - Preparation of elemental phosphorus

from everything i have read i shouldn't have to flush the reactor. it will be producing carbon monoxide which should burn the oxygen away at an early stage with these temps.

[Edited on 19-8-2010 by Rogeryermaw]

That would indicate you're running Ca3(PO4)2 + C, right? Why not consider Al as a reducing agent? My own test with Na metaphosphate + Al + SiO2 (open crucible) was very successful.

Rogeryermaw - 19-8-2010 at 23:02

the steel parts of the apparatus were only in the $20 range most of which if not all i'm sure will be reusable so i'm willing to try different mixtures to obtain results that will benefit the private chemist community...rotten dope heads ruined it for all of us.

blogfast25 - 20-8-2010 at 04:25

the steel parts of the apparatus were only in the $20 range most of which if not all i'm sure will be reusable so i'm willing to try different mixtures to obtain results that will benefit the private chemist community...rotten dope heads ruined it for all of us.

I think you'll find that removing post-reaction gunge (the 'slag') from your apparatus will be fairly easy with a power tool.

My own test with someone else's formula, here:

http://www.sciencemadness.org/talk/viewthread.php?tid=65&...

... was quite successful, albeit without capturing the formed P4. Na metaphosphate/Al/SiO2 lights up easily with some strong external heating and seems to burn right through (it generates a lot of heat once started).

Ca3(PO4)2 based mixes, whether reduced with C or Al and based on what I've seen and read, need higher heat and sustained heating to keep going.

Regards fluxing the reactor with Ar before use, I seem to have forgotten one of my own arguments I made against it! Assuming you generate a reasonable amount of P4, it will quickly scavenge any O2. The volume of your reactor is about 290 cm3, or 0.29 L, so even empty and at RT it would contain about 0.2 x (0.29 /22.4) = 2 mmol (millimol), the equivalent of 0.2 mmol of P4 (P4 + 10 O2 --> 2 P2O5) or about 0.03 g of P4!

Undoubtedly Hennig Brand on that famed day in 1669 didn't flush his retort either ;-) !

Rogeryermaw - 20-8-2010 at 05:32

That's what i'm counting on...once the residual oxygen is used up in the process, as long as the collector is inert and cool enough P vapors should solidify...i wonder if using an ice slurry in the collector would eliminate the need to have the spout submerged...that would solve the safety issue about water being drawn into the reaction vessel

blogfast25 - 20-8-2010 at 08:27

That's what i'm counting on...once the residual oxygen is used up in the process, as long as the collector is inert and cool enough P vapors should solidify...i wonder if using an ice slurry in the collector would eliminate the need to have the spout submerged...that would solve the safety issue about water being drawn into the reaction vessel

I think you'll find it will solidify faster than you might wish: clogging of the spout may even be an unexpected problem. It might help to heat the spout to above the melting point of P4 at least...

Alternatively, get a thermocouple right after the reaction zone for better control. Always useful!

[Edited on 20-8-2010 by blogfast25]

Rogeryermaw - 20-8-2010 at 14:28

clogging of the output spout has concerned me too... i don't want the whole thing to become a big bomb full of deadly scorching hot reactants and phosphorus... how about a slightly longer pipe running into the collector with the end of the pipe only 1/2" or so into hot water to keep the condensate in liquid phase? also the temps around the furnace should keep the material in the delivery tube liquid since steel conducts heat fairly well.

Taoiseach - 21-8-2010 at 00:54

This looks like a dangerous setup. A slight drop in temperature might cause underpressure in the reaction chamber. If water gets sucked back into the red-hot chamber it will cause an explosion. Once the reaction subsides OR you run out of charcoal the chamber will begin to cool down and then it has to be disconnected from the collector or disaster will ensue! You could make the spout somewhat longer and carefully insulate it with mineral wool to keep the P4 fluid. You could also try to attach a stainless steel funnel to the spout. Invert the funnel and put it into the collector so that its mouth is just barely under water - this will effectively avoid suckback.

un0me2 - 21-8-2010 at 02:47

I am currently looking at the synthesis of free, elemental phosphorus from phosphine (PH3), there is the thermal dissociation of phosphine (garage_chemists favorite

- BTW I really would like a look at whatever anyone has on a thermite-type reaction giving a phosphine precursor).

There is also the reported reaction of phosphine with dimethylchloramine, which "reportedly" gives free, elemental phosphorus and dimethylammonium chloride (as reported here: http://pubs.acs.org/doi/abs/10.1021/ic50067a009). That would be an EXTREMELY interesting solution to producing elemental Phosphorus, as it would be feasible to produce elemental phosphorus using an RT hydrolysis of MxPx' salts to give PH3 (logically, there should be no need to dry it), pass the gas generated into a solution of dimethylchloramine (obviously an inert atmosphere would be vital). But at least there is not the need for the high-temperature on one end and then removal of the massive amount of excess heat.

Converting the elemental, presumably white, Phosphorus into the much more easily worked with Red Alletrope would probably be the next problem (pressure vessel, etc. I have several journal articles on the same).

There is also the reported combustion of phosphine (drying would be required) in an atmosphere of chlorine to give PCl5. I am trying to find some more details on that specific reaction, but if it is in fact the case (Buckholtz, et al's Patent would be proved).

In any event, a more amateur friendly synthesis of a phosphine precursor (I've attached one synthesis of Zinc Phosphide from Zinc Orthophosphate - hydrolysis of which in H3PO4 would give phosphine and zinc orthophosphate (ie. the precursor is regenerated by the hydrolysis reaction).

Attachment: Fluck.The.Chemistry.of.Phosphine.pdf (857kB)
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Attachment: Murali.Gopalam.Preparation.of.Zinc.Phosphide.pdf (393kB)
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blogfast25 - 21-8-2010 at 04:50

@ rogeryermaw:

What do you plan for heating? Will the entire reactor bit be heated, in a furnace for instance? Or will you use bunsen burners?

As long as the spout isn't submerged, at least the risk of suckback is nil. You could perhaps used a thermos flask half-filled with iced water as collector?

Magpie - 21-8-2010 at 08:09

His P4 is going to hopefully drop into a vented paint can purged continuously with inert gas (CO2). I presume Roger will have water in the bottom of the paint can, yet provide a sufficient "air gap" so the spout end is not submerged. So suckback is not an issue.

As someone else pointed out keeping the retort spout at a high enough temperature to keep the P4 from solidifying is not going to be a problem if he has the other end red hot.

blogfast25 - 21-8-2010 at 08:57

As someone else pointed out keeping the retort spout at a high enough temperature to keep the P4 from solidifying is not going to be a problem if he has the other end red hot.

Well, that all depends on the difference between the red hot zone and the spout itself... In continuous operation the spout would inevitably heat up. But at start up there will be some formation of P4 deposit.

Magpie - 21-8-2010 at 10:07

I'd be more concerned with slag plugging the outlet than P4. P4 melts quite easily. Therefore I recommend being careful to not overcharge the reactants.

Also, if the P comes out as a gas what's to keep some of it from leaving with the vent gas into the environment? Doing this outside, as already stated, and being aware of that possibility is recommended. Stay upwind.

Rogeryermaw - 21-8-2010 at 10:28

As someone else pointed out keeping the retort spout at a high enough temperature to keep the P4 from solidifying is not going to be a problem if he has the other end red hot.

so i'm thinking a good preheat below the reaction temp will reduce the chance of cold deposits, and the funnel with slight submersion is a good idea since it would increase the volume of water having to be drawn in causing it to surface and break the vacuum. i will be carrying this out in a force fed coal furnace, outdoors with gloves and protective clothing.

Rogeryermaw - 21-8-2010 at 10:30

I'd be more concerned with slag plugging the outlet than P4. P4 melts quite easily. Therefore I recommend being careful to not overcharge the reactants.

Also, if the P comes out as a gas what's to keep some of it from leaving with the vent gas into the environment? Doing this outside, as already stated, and being aware of that possibility is recommended. Stay upwind.

THOSE are very good and scary points though i have considered the slag issue...i have entertained the ideas of some sort of fine steel screen near the last adapter but it may just burn away or cause other issue and have also thought of laying the pipe at a slight angle and making sure to leave an airspace at the top of the reactant mixture. as blogfast pointed out, i will likely try a small charge for the first run. depending on how it performs i have other pipe and fittings if the output needs to be longer.

[Edited on 21-8-2010 by Rogeryermaw]

blogfast25 - 21-8-2010 at 12:17

Good point by Magpie about the slag. The force fed charcoal furnace is all good, IMHO. If you load the reactor into the furnace at a small angle, spout at the higher end, blockage by slag shouldn't become an issue, IMHO. That and not over-charging.

I think the whole thing is a lot less dangerous than we might imagine but it needs to be done properly to succeed...

Magpie - 21-8-2010 at 12:48

Good point by Magpie about the slag. The force fed charcoal furnace is all good, IMHO. If you load the reactor into the furnace at a small angle, spout at the higher end, blockage by slag shouldn't become an issue, IMHO. That and not over-charging.

I think the whole thing is a lot less dangerous than we might imagine but it needs to be done properly to succeed...

I had my ceramic retort angled slightly downward to allow the liquid P4 to drain better. The slag from the Al/NaPO3/SiO2 run was foam-like, and I'm not sure that tilting the retort had much affect on it.

Try to get all your reactants dry so you don't generate any more phosphine than necessary.

In regard to potential danger, I felt that my handling of the retort following the run was really too dangerous. I want to make some more P4 someday but one of the reasons I stopped was the feeling that I really didn't have the situation under proper control.

blogfast25 - 21-8-2010 at 12:54

Yes, my own Al/NaPO3/SiO2 mix in open crucible conditions also foamed, as the P4 escapes. It was also quite viscous. And continued to react after I'd switched the propane flame off. I wouldn't be surprised this mix could be initiated with the usual suspects, then allowed to propagate. Or ignited with Nichrome wire/current.

[Edited on 21-8-2010 by blogfast25]

Rogeryermaw - 21-8-2010 at 13:24

yay! it's finally raining! maybe they will drop the burn ban so i can run this experiment.

un0me2 - 21-8-2010 at 14:19

Here is the paper I was waiting for on the reaction of dimethylchloramine and phosphine to give elemental Phosphorus. They start from Aluminium Phosphide & go via the production of phosphine therefrom.

Attachment: Highsmith.Sisler.A.New.Reaction.of.Chloramines.with.Phosphines.pdf (771kB)
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I just threw the synthesis of Zinc Phosphide up, starting from Zinc Phosphate(s). With strong phosphoric acid it should give Zinc Phosphate and dry Phosphine

Attachment: Murali.Gopalam.Preparation.of.Zinc.Phosphide.pdf (393kB)
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Now, I'm looking at that synthesis of Zinc Phosphide by thermal reduction with carbon and wondering why that couldn't be achieved in a MW. Carbon is a MW Susceptor and the hot carbon should reduce the Zinc Phosphate to the Phosphide by essentially the same mechanism as is done in the paper purely thermally.

All we need now is a decent route to dimethylamine - I do have the sneakiest suspicion that I have seen various agricultural products as methylamine salts.

EDIT

Whoops, apparently the Red Phosphorus is the allotrope that is formed. Really should have taken the time to read it better before I posted it - then again, kinda hard not to be excited

Here is a paper on the preparation of the relevant methyldichloramine and dimethylchloramine by treating the relevant methylamine.HCl with calcium hypochlorite...

Attachment: Stevenson.Schomaker.The.Molecular.Structure.of.Dimethyl.Chloramine.and.Methyl.Dichloramine.pdf (693kB)
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[Edited on 22-8-2010 by un0me2]

Rogeryermaw - 21-8-2010 at 19:22

i found something that people in this thread may find very interesting. http://blog.modernmechanix.com/2007/08/02/arc-furnace-incase... this may very well be adaptable for phosphorus recovery. very cheap to build too.

stygian - 21-8-2010 at 19:37

that man is not protecting his skin as he should be!

un0me2 - 22-8-2010 at 03:13

I think that given that paper, if the residue is non-reactive at ordinary temperatures (and neither is pure phosphine), it may even be possible to get Red Phosphorus from a fairly simple procedure at STP.

blogfast25 - 22-8-2010 at 10:32

That has been posted here before. Mind you, there isn't much that hasn't been posted here before!

Rogeryermaw - 22-8-2010 at 11:49

sorry bout that...you have to admit it's pretty cool though. 2 flowerpots, sand, fire clay, and a couple of coal or graphite art pencils. the weekends are getting hard to sit through. knowing my reactants are sitting on a truck somewhere and UPS doesn't move on the weekend...patience though...i can't rush through the experiment...

i have seen in various places that you cannot gas red phosphorus to get PCl3. but i ran across this article a while back about the production of phosphorus oxychloride from phosphorus thichloride derived from red phosphorus. am i misinformed?

"charge your rxn flask with dry RP powder. lead the Cl2/helium line through one stopper (use cork POCl3 attacks rubber stoppers) the center one is equiped with a glass stir bar that reaches the bottom with atleast 5cm to spare, the end in the flask has had a short section of glass rod melted to it crossways. The last neck has a hose leading out a window or to a hood if you have one. The flask is now charged with helium, not helium for balloons, that stuff is only about 35% helium and the rest air. get a small cylinder from a welding store, nitrogen will work in a pinch but you want a light gas. If you were to use argon it would blanket the RP and prevent the Cl2 from getting to it. Now that your flask is inerted, slowly (REALLY SLOWWWW...) turn on the supply of Cl2. The trick here is to let the chlorine 'trickle' in in small amounts (PPH amounts). If you put too much in the RXN goes exothermic and will produce flame, possibly an explosion if you have a large enough amount of RP or melt through your flask creating a dangerous chemical fire. If you do it right you can feel the flask by the RP and it will be warm possibly hot but not flaming. Gradually the RP will start to look 'wet' as the phosphorus trichloride starts to form you may have to break up and stir the RP from time to time to get it all to react. Eventually you will have a puddle of PCl3 with some RP that did not react. Now you can turn up the chlorine a little bit and start stirring to react the rest. Once the liquid is as clear as it is gonna get flush the flask with helium again and insert a section of glass tube into the liquid. You now have to pass pure O2 through it for several hours.

sorry i can't provide a source. i copied this text and saved it in my notes some time ago. also sorry if this is the wrong place for this but i saw mention of PCl3 earlier in this thread and that is a compound i am interested in but if it can't be done with red phosphorus that would be good to know...i'm hesitant to try it with white phosphorus because of how reactive it is.

[Edited on 22-8-2010 by Rogeryermaw]

blogfast25 - 22-8-2010 at 12:44

P is amazingly reactive with most non-metals.

aliced25 - 22-8-2010 at 21:08

That has been posted here before. Mind you, there isn't much that hasn't been posted here before!

What has been posted here before? The reaction of Phosphine with Dimethylchloramine? If so, was it tried? I'd prefer to know if it doesn't work before anyone tries it...

@Rogeryermaw

If you have a look, the preparation of POCl3 from P4O10 & NaCl (per Tarbutton, et al) in a tube very like the one I saw on the previous page (starting at about 250'C IIRC) is also "reported" (from a VERY RELIABLE source, ie. not me

) to work "just as the paper says".

I'll throw up two of the papers cited by the paper in question, as they are rather instructive.

[Edited on 23-8-2010 by aliced25]

Attachment: Lucas.Ewing.New.Method.of.Preparing.PF5.pdf (306kB)
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Attachment: Thorpe.Hambly.On.POF3.pdf (83kB)
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Attachment: Tarbutton.POCl3.from.P2O5.NaCl.pdf (802kB)
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Rogeryermaw - 23-8-2010 at 08:27

@ Alice that was an interesting read...seems simpler than the method i was looking at. it's a bit difficult to obtain P2O5 though...and that was a synth i wanted to try too. could you reduce P2O5 with carbon to obtain elemental P?

Panache - 23-8-2010 at 22:19

metal phosphides are sold commercially as rat bait, the phosphine being released in the gut after the metal phosphide is hydrolysed. Nice. Initially they were released/sold without any coating but many a sheep were killed when the rain soaked the bait in the shed during a heavy storm, i believe they are now only fatal if ingested not just wetted, that said i wonder if carrion eating animals fare poorly on the dead rats?
They are not sold at supermarkets and the like as they are generally used for heavy infestations, so rural product suppliers etc carry them in larger quantities.
its a shame so much effort has be be gone through for such a ubiquitous element.

Rogeryermaw - 24-8-2010 at 19:09

according to UPS i should be receiving a package tomorrow so i will spend the day preparing the furnace and, if all goes well and weather allowing, i will have some pics and a rundown of my process. upon reading an excerpt from an alchemical text, i have decided to somewhat prolong the process and allow the necessary temp to be reached VERY gradually. a good preheat such as this should ensure dryness of the reactants and proper warming of the delivery tube so as to avoid solidification of the distillate in the tube.

then again...arc furnaces don't pre-heat do they? i mean when you strike an arc with welding gear it is instantly HOT!

[Edited on 25-8-2010 by Rogeryermaw]

blogfast25 - 25-8-2010 at 05:49

, i will have some pics and a rundown of my process. upon reading an excerpt from an alchemical text, i have decided to somewhat prolong the process and allow the necessary temp to be reached VERY gradually. a good preheat such as this should ensure dryness of the reactants and proper warming of the delivery tube so as to avoid solidification of the distillate in the tube.

then again...arc furnaces don't pre-heat do they? i mean when you strike an arc with welding gear it is instantly HOT!

[Edited on 25-8-2010 by Rogeryermaw]

Very well, can't wait! During the run itself, put that camera aside: you want to keep your wits about and your legs in 'go, go, go!' mode in the unlikely event things get hairy!

That Hennig Brand guy thought he was making gold from piss, I guess he got lucky not to get burned!

Rogeryermaw - 25-8-2010 at 13:49

oh ya! its my birthday!! not really but every time i receive a chemical order i get giddy. i also picked up some refractory cement today so i could make a furnace specifically for the preparation of phosphorus. i also purchased 2 lbs. of phosphate so i could run the synth multiple times if the first run goes well. the time is close so wish me luck. and thanks for the advice blogfast. i have it in mind and i will be sure to take great care during this process (limbering up for the hundred yard dash)

Avoid suckback with an outlet shield

watson.fawkes - 25-8-2010 at 16:53

You can avoid suckback by putting a passive shield around the outlet pipe. The inert gas shield will exit out the top of the shield. A wier pipe with integral trap keeps the water level low enough to avoid the outlet.

[Drawing rendered in Inkscape; original attached.]

P4 collector pipe.png - 6kB

Attachment: P4 collector pipe.svg (8kB)
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Rogeryermaw - 27-8-2010 at 10:57

sorry folks that its been so long. the week has been out of control! daughter started school this week. soon. promise.

Rogeryermaw - 29-8-2010 at 19:42

ok. i finished a preliminary run. i have come to the conclusion that i will have to switch to propane fuel to get the temp i need. the reactor wouldn't get any hotter than a dull orange. according to info available from forge and foundry sources that's only 900-1000 celsius. also i may change the reactor from rigid to emt. emt is steel but has a much thinner wall. the furnace is dug out in sand and the top is an old bbq lid coated with refractory cement. it gets freakin hot but i think the emt will transfer more heat to the reactants. also propane will allow me to run it without having to add fuel and lose heat. i will give it a go with the new ideas in place wednesday or thursday. thanks for being patient.

DSCN0010.JPG - 116kB

also wanting to give Al a try. the lower temp needed for reaction with aluminum is enticing.

[Edited on 30-8-2010 by Rogeryermaw]

blogfast25 - 30-8-2010 at 07:36

Getting a higher temperature with propane will not be easy: provided you have plenty of air, lump BBQ charcoal burns like the clappers: very, very hot! Your furnace looks very adequate to me. Is that incoming pipe for air?

What reagent mix were you using?

For Al, you can also use Al foil shredded in a food blender: sieve off the fines, that'll do in a good mix, preferably with metaphosphate (most Calgon tablets - consult the labels). Fine Al shreddings, Na metaphosphate and SiO2 in the right ratio will work in your conditions, or I'll EAT MY HAT!

But please tell me that that isn't your condenser... you need at least something that's bottle shaped, IMHO...

[Edited on 30-8-2010 by blogfast25]

Rogeryermaw - 30-8-2010 at 11:16

if you can show me a drawing or diagram of what you feel the condenser should entail please do. if i can see it i can build it. but the reason i opted for propane is that during this first run i used charcoal and it burns away so fast that i have to keep opening the furnace to add fuel and it causes me to lose a lot of heat. looking at some of the home foundry designs on youtube i see several designs running propane that actually melt steel to a pourable temp. yes i know it is not the ideal mix but my reactants are calcium diphosphate, carbon, and silicon dioxide in stoichiometric ratios.

3CaH(PO4)+6C+3SiO2 -> 3Ca2SiO4+6CO+PH3+2P

is the balanced equation. using molar mass its roughly: CaH(PO4)=22.5g, C =4g, SiO2 =10g. and according to the eq. there IS some phosphine developed so i will be staying well away when the reaction starts.

coming wednesday i will have a bit of cash to work on lab equip so i will get some Al powder and Na meta and have a go with it. it seems sodium hexametaphosphate is readily available and relatively cheap here as photo chemical at about $14/lb
ya the pipe on the right is bringing air in from a blower motor. it is from a bounce house and moves A LOT of air.

seems an awful lot of trouble to get POCl3 which isn't even regulated. one of these days i'm going to start meeting meth cooks in dark alleys and beat the hell out of them for ruining the future of research in america. i know its not entirely their fault but they are the scapegoat that gives the govt and pharmaceutical companies fuel to take chemistry away from the rest of us... sorry for the rant but i know all of you feel the sting at one time or another.

[Edited on 30-8-2010 by Rogeryermaw]

[Edited on 30-8-2010 by Rogeryermaw]

blogfast25 - 30-8-2010 at 12:12

if you can show me a drawing or diagram of what you feel the condenser should entail please do. if i can see it i can build it. but the reason i opted for propane is that during this first run i used charcoal and it burns away so fast that i have to keep opening the furnace to add fuel and it causes me to lose a lot of heat. looking at some of the home foundry designs on youtube i see several designs running propane that actually melt steel to a pourable temp. yes i know it is not the ideal mix but my reactants are calcium diphosphate, carbon, and silicon dioxide in stoichiometric ratios.

3CaH(PO4)+6C+3SiO2 -> 3Ca2SiO4+6CO+PH3+2P

is the balanced equation. using molar mass its roughly: CaH(PO4)=22.5g, C =4g, SiO2 =10g. and according to the eq. there IS some phosphine developed so i will be staying well away when the reaction starts.

coming wednesday i will have a bit of cash to work on lab equip so i will get some Al powder and Na meta and have a go with it. it seems sodium hexametaphosphate is readily available and relatively cheap here as photo chemical at about $14/lb
ya the pipe on the right is bringing air in from a blower motor. it is from a bounce house and moves A LOT of air.

I've no design for a condenser but I was thinking of something like a vase with a more narrow top opening, half filled with iced water...

Actually, the famous painting of Hennig Brandt discovering phosphorus (instead of gold- hehehe) is an inspiration for a condenser...

http://2.bp.blogspot.com/_Bo_1OwpTPWg/Rxz-xOdD7fI/AAAAAAAAAB...
(Howzat for a diagram, eh!)

Charcoal fuelled furnaces do need regular refueling, that's true. It's the main drawback of mine too...

The chemistry however doesn't make an enormous amount of sense: why are you using the calcium diphosphate CaHPO4 and not the ternary tricalcium ortho phosphate Ca3(PO4)2? Now you're planning to make PH3... ooops!

Your equation isn't balanced:

3 CaH(PO4) + 6C + 3 SiO2 -> 3 Ca2SiO4 + 6 CO + PH3 + 2P

... because it has 3 Ca on the left and 3 x 2 Ca = 6 Ca on the right. Correctly balanced it is:

2 CaHPO4 + 6 C + SiO2 --> Ca2SiO4 + 4/3 P + 2/3 PH3 + 6 CO

Note that the P/PH3 ration remains 2.

With Ca3(PO4)2 it becomes:

Ca3(PO4)2 + 5 C + 3/2 SiO2 --> 3/2 Ca2SiO4 + 2 P + 5 CO

... and no phosphine! For Ca3(PO4)2 you can basically use bone ash, or react your calcium diphosphate with slaked lime:

Ca(OH)2 + 2 CaHPO4 ---> Ca3(PO4)2 + 2 H2O

... then filter and dry on high heat.

Alternatively, go the sodium hexametaphosphate way... I believe you can even convert your calcium diphosphate into Ca metaphosphate and I think it's explained in a post above.

Ooops.. it appears only Ca(H2PO4)2 can be easily converted to metaphosphate, not CaHPO4...

And after rereading much of this long thread, the more I read, the more I'm convinced the sodium hexametaphosphate/Al/SiO2 route is the way to go because of the seemingly much lower temperature requirements:

2 NaPO3 + 4/3 Al + SiO2 ---> Na2SiO3 + 2 P + 2/3 Al2O3

(2 NaPO3 = 1/3 (NaPO3)6)

[Edited on 30-8-2010 by blogfast25]

[Edited on 30-8-2010 by blogfast25]

Rogeryermaw - 30-8-2010 at 13:46

oh believe me i didn't want to be using the dibasic. i ordered bone ash and was sent bone ash synthetic. it's ok though. i like the metaphosphate idea and will be using it. if i can find a decent smallish metal funnel i will weld it to the bottom of the delivery pipe. that should reduce the chances of a vacuum induced catastrophy. you are correct about my equation. it should have looked like:

6 CaH(PO4) + 18 C + 3 SiO2 = 3 Ca2SiO4 + 18 CO + 2 PH3 + 4 P.

i hate to waste chemicals so i will play with these but i do very much like the idea of the aluminum reduction of the metaphosphate so i will run it next. i also like the idea of eliminating PH3 since it's deadly and a waste of phosphorus.your helpfulness is much appreciated. particularly the lack of venom. far too much anger and biting sarcasm find there way here and you conduct yourself like a professional. thank you.

BTW i do so love this picture!

[Edited on 30-8-2010 by Rogeryermaw]

[Edited on 30-8-2010 by Rogeryermaw]

aliced25 - 31-8-2010 at 02:20

The type(s) of condensers are enormous, but when working with such temperatures you'll need a working fluid (and fins for heat transfer) inside an outer pipe, with the working fluid being pumped in at the bottom and out at the top. One of the glycols should be up to the task. I'd suggest cutting some fins into the inner pipe ABOVE where the outer pipe joins it, so it works as an air-condenser, precooling the distillate before it gets to the condenser.

blogfast25 - 31-8-2010 at 06:15

Quote: Originally posted by aliced25

The type(s) of condensers are enormous, but when working with such temperatures you'll need a working fluid (and fins for heat transfer) inside an outer pipe, with the working fluid being pumped in at the bottom and out at the top. One of the glycols should be up to the task. I'd suggest cutting some fins into the inner pipe ABOVE where the outer pipe joins it, so it works as an air-condenser, precooling the distillate before it gets to the condenser.

I don't think anything like that is necessary. While the painting isn't necessarily technically very accurate, Brandt achieved reduction of phosphate in primitive conditions, without sophisticated condensers. Brandt was eventually reduced to selling the method to various buyers (see p. 312, of the excellent 'Nature's Building Blocks' by John Emsley).

Others like me have actually pointed out to the risk of the P cooling and solidifying TOO QUICKLY! We have some evidence of that happening in experimental conditions, higher up in the thread...

blogfast25 - 31-8-2010 at 06:20

@ Roger:

It is a wonderful painting. He (they?) must have been flabbergasted, having made the first glow-in-the-dark, instead of gold...

Rogeryermaw - 31-8-2010 at 10:01

going by info i collected from my last attempt, after about 25-30 minutes in the fire, the vessel heated the output to a fairly warm temp. well within the liquid range for phosphorus. an idea i have come up with is to weld a stainless funnel such as this to the end of the delivery tube. the increase in area at the opening should make it difficult for the reactor to pull in enough water to do damage in that if it pulls water in to a certain volume the end of the funnel would no longer be submerged thus breaking vacuum. any thoughts?

funnel.jpg - 4kB

blogfast25 - 31-8-2010 at 11:38

Getting to within the liquid range of P isn't near good enough, of course: you need to get the reaction going which in the case of orthophosphates going by he literature may well be above 1000 C.

Your funnel idea seems good to me. Not sure it's really necessary; you'll have to see...

I think I might have another open crucible test with NaPO3/Al/SiO2 for some better observations...

Rogeryermaw - 31-8-2010 at 13:05

i'm sorry i may have been unclear. the reaction vessel was quite hot. the section i was referring to was the part outside of the furnace. it was uncomfortably hot to the touch so no worry about P4 solidifying in the tube. also i boiled the water in the catch pan before placing it under the tube.

[Edited on 31-8-2010 by Rogeryermaw]

blogfast25 - 31-8-2010 at 13:07

Yes, I misunderstood you. I think you're right.

Rogeryermaw - 31-8-2010 at 13:19

tomorrow or thursday i will run it again with the lp gas. i will also order the sodium metaphosophate. i may use the furnace to melt my own Al. i want to try the idea i found about stirring molten Al to produce coarse powdered Al. be nice if it was suitable for this reaction.

mr.crow - 31-8-2010 at 14:37

The inverted funnel is a good technique to stop suckback. The phosphorus vapor inside would burn when it hits the air if this were to occur. Still way better than a steam explosion.

Aluminum would be molten at the operating temperature but I would still go with powdered Al so it makes contact. Molten metals have a high surface tension.

Being exothermic the reaction would really take off. Maybe it would be too fast at large scale?

Well enough armchair chemistry from me. This sounds like its going to be legendary

Rogeryermaw - 1-9-2010 at 22:08

ok i built a new reactor with emt since it has thinner walls. blogfast you were on the right track about the propane. it can work but not with a BBQ tank. the volume of gas is just too low. anyhoo i ordered a lb. each of aluminum and sodium meta. we gonna get some phosphorus before its all over!

6(NaPO3) + 10Al + 3SiO2 = 3Na2SiO3 + 5Al2O3 + 6P

per mole (approx)
(NaPO3)=102
Al = 27
SiO2 = 60

prep
34g Sodium Hexametaphosphate
9g Aluminum
20g Silicon Dioxide
i will mix these reactants and use maybe half the mixture for a charge. does this math look correct? your input is valued. i have one curiosity. aluminum always has a surface layer of oxide. does that play into the reaction or is the amount negligible?

blogfast25 - 2-9-2010 at 07:40

The eyes of the world are on you! ;-)

ScienceSquirrel - 2-9-2010 at 08:04

Your reactant masses look a bit off to me.
If your reaction is stoichiometric and I doubt that it is with all sorts of crap being formed you would have a ratio of 6:10:3.

Hence;

34g 0.33M Sodium Hexametaphosphate
15g 0.55M Aluminum
10g 0.165M Silicon Dioxide

In practice the best yield will probably be achieved by using one or two of the reactants in excess.
The aluminium oxide coating on the aluminium powder will be negligble and can be ignored.

blogfast25 - 2-9-2010 at 11:26

Quote: Originally posted by ScienceSquirrel

Your reactant masses look a bit off to me.
If your reaction is stoichiometric and I doubt that it is with all sorts of crap being formed you would have a ratio of 6:10:3.

Hence;

34g 0.33M Sodium Hexametaphosphate
15g 0.55M Aluminum
10g 0.165M Silicon Dioxide

In practice the best yield will probably be achieved by using one or two of the reactants in excess.
The aluminium oxide coating on the aluminium powder will be negligble and can be ignored.

Correct. I'd use a 10 - 20 % excess of Al.

Rogeryermaw - 2-9-2010 at 20:02

thank you. a bit excess Al would be a good idea if it won't react with the P4. it will burn up any extra O2 from the atm in the reactor.

Rogeryermaw - 3-9-2010 at 13:11

well...that was fast. the new reactants are here so tonight is the night. i will post results asap.

Rogeryermaw - 3-9-2010 at 16:48

i have done it!!!!!!!! i will post pics soon as i clean and solidify it all. they will be up tonight!!!

[Edited on 4-9-2010 by Rogeryermaw]

phos 1.JPG - 65kB

the phosphorus came over easily. the reaction was stable and controlled and i could easily have scaled it up much further and will tomorrow. i didn't take pics of the process because it's essentially the same as last time with minor changes to the furnace that wouldn't show on film anyway and of course the reactor which is designed the same but with thinner metal and instead of 1.5 inch rigid i used 1 inch emt for better heat transfer. the P4 is fairly pure. the pics don't do it justice. it's yellow but transparent and smokes freely in air. also you see the bright yellow flame and voluminous smoke. sorry...i would be more clear and detailed but i'm more giddy now than my first joint, sex, or roller coaster!!! ready to go again tomorrow.

[Edited on 4-9-2010 by Rogeryermaw]

Sedit - 3-9-2010 at 18:53

Let me be the first to say congrates, I have always thought this to be a fairly easy reaction(while sitting in my armchair) that people tend to over think putting P4 on some sort of unreachable height that they will never achieve but have always dreamed of. Thank you for showing that with a little dedication and creativity is not the shit storm people make it out to be while they also sit there in there armchair.

Rogeryermaw - 3-9-2010 at 19:08

thank you and all too true. however i think it IS a little more difficult to achieve on a lab scale to obtain useful amounts and i did cheat on that a bit by having space for an outdoor furnace. but those of you who suggested the lower temp reaction of sodium meta and aluminum were the ones who made it possible. now to scale it up and send out free samples to some of the more dedicated among the chemist community...

i will say this though...i will have to develop a more convenient process to collect and filter the product...it smokes instantly and when the collector is hot, if it is sloshed at all and P4 surfaces, it will ignite and float on the gasses produced, burning away costing you product. tonight i will work on design for an apparatus to help with this.

[Edited on 4-9-2010 by Rogeryermaw]

Sedit - 3-9-2010 at 19:59

I have a kiln that up till recently cost me to much to operated however I envisioned a simular setup as yours just a better heat source ect... ect...

My main question is what is your plans for conversion to the red variety? For storage it would be the best way to go since its less toxic and performs many of the same functions as long as time isn't a factor.

Rogeryermaw - 3-9-2010 at 20:10

that is an excellent question that keeps me up at night. there are many proposed methods such as under water with iodine in sunlight or heating under inert atmosphere... i'm not sure what method i will use yet...it's so much easier to turn red into white.

ehow has a neat article on this:

http://www.ehow.com/how_6063919_convert-white-red-phosphorus...

IMPORTANT!!!

Rogeryermaw - 3-9-2010 at 21:14

for anyone wanting to try this synthesis: your results may vary but i was outside attempting to knock the slag out of the reactor i used and the most unusual thing happened. emt or electrical metal tubing is, i believe, galvanized. that may or may not play into this experience. after about 4 or 5 inches of slag was removed and as i kept working at it, along the side of the pipe there was an audible (and fairly loud) pop and a visible flash. in all, with the down pipe removed, the reactor pipe is about 14 inches long. i was holding it about 3-4 inches from the sealed end and the flash was close to my hand...outside of the pipe. no idea how it happened. it was P4 related as the smell is unmistakable but how it was generated and how it occurred i could not tell you but phosphorus usually burns. this was either a rapid decomposition or a small explosion. thinking it may be a fluke i continued but after a second time i decided it was safer to build a new one. i am sure some P4 must have been trapped in the slag but how this happened outside of the reactor i cannot guess. can anyone shed light on this? i see no loss of integrity to the wall of the pipe so it has me at a loss. i have worked metal for years and anyone who has knows that when you heat steel to glowing it will form a layer of slag that will chip away but i have never seen it ignite so i can only guess it has something to do with the reaction materials in combo with P4 trapped in the pipe...melon scratcher

Eclectic - 4-9-2010 at 01:04

Spontaneously flammable phosphine formed from reaction of metal phosphides and moisture in the air? Your slags may be more toxic and dangerous to work with than the phosphorus.

blogfast25 - 4-9-2010 at 05:10

Congratulations, Rogeryermaw!

Can you post some details on formulation used and quantity? Any idea of yield?

Awww... a phosphine 'explosion' seems indeed by far the most likely cause and worrisome too! Could moisture in the ingredients be the source of hydrogen? Without a source of hydrogen, no phosphine. Or did moisture seep in after the main reaction?

Try thoroughly oven drying all ingredients before the next run...

Rogeryermaw - 4-9-2010 at 06:37

those are excellent suggestions. thanks. i will dry the ingredients first and consider the reactor disposable as they are rather cheap to build and can be left to "air out" far away from the house. as for the formula: i ran (NaPO3)6=32g + Al=14g + SiO2=20g. unfortunately i did not weigh the product but i will after this run as i have dug up an old plastic tub i can fill with water to work under. i will put the liquid phosphorus into a small glass container of hot water and draw the P4 into a syringe. with a test tube with a glass wool filter under the water in the tub i will slowly pass the P4 through the glass wool to clean it and then just pour the contents of the tube into a glass dish to cool so the P4 can be broken up and stored in an amber bottle with water.

now that you mention it there must have been moisture in the ingredients that yielded H2 because as the vapors bubbled through the water some of them ignited as they surfaced indicating PH3. no worries though as i figured it was just safest to stay well clear of the output till the reaction was completed.

[Edited on 4-9-2010 by Rogeryermaw]

Rogeryermaw - 4-9-2010 at 17:41

ok i ran the synth again with the same measurements and i yield about 2 grams of phosphorus every time but there is significant loss through turbulence. when the bubbles break the surface and churn the water there is a good bit of P4 that burns away so i need to work on my receiver to beat this problem and increase yields but i will keep you all abreast of any new developments...now then... can anyone point me toward a thread that has a good workable synth for PCl3 and or POCl3?

blogfast25 - 5-9-2010 at 10:58

PCl3 can be obtained from direct union of the elements, not sure about POCl3. There must be threads on both on this forum: search and ye shall find...

What do you want with these two lovelies?

woelen - 6-9-2010 at 00:05

@Rogeryermaw : Thanks for sharing this great result with us and congratulations with this result!

I consider this a major breakthrough, because it makes phosphorus available also for US-based home chemists. I have many interesting things to share which require the use of phosphorus and it is so sad that a big part of the amateur chemistry community cannot obtain this element. Your efforts show that this can be changed.

I myself can buy red P and I have made a small amount of white P from that. Especially if you do not make large quantities of phosphorus, I would leave it under water as white P. From a synthetic point of view, white P is much more useful. It dissolves in quite a few solvents and it tends to react more completely. With red P I always notice that part of it does not react or does so very slowly. This part must be some less reactive kind of phosphorus (violet P?). I have the impression that red P is not a single chemical entity, but a mix of all different kinds of phosphorus, which have a different degree of reactivity.

Rogeryermaw - 6-9-2010 at 06:22

@ woelen thank you very much. i will keep some of the P4 as white but also want to use the red for projects because it is less toxic and does not react quite as violently as white.

@ blogfast PCl3 is of interest to me because you can turn it into POCl3 by bubbling O2 through it with stirring under an inert atmosphere. POCl3 is of interest to me because the first "science" i fell in love with was electronics and POCl3 is a good dopant for layering silicon for home brew electronic transistors.

[Edited on 6-9-2010 by Rogeryermaw]

blogfast25 - 6-9-2010 at 07:14

Quote: Originally posted by woelen

@Rogeryermaw : Thanks for sharing this great result with us and congratulations with this result!

I consider this a major breakthrough, because it makes phosphorus available also for US-based home chemists. I have many interesting things to share which require the use of phosphorus and it is so sad that a big part of the amateur chemistry community cannot obtain this element. Your efforts show that this can be changed.

I'm guessing that much could be gained from actually scaling down the reactor somewhat and simply using bunsen heating or a propane flame torch, to produce small amounts of P4 without much hassle or risk... Perhaps with an improved condenser...

woelen - 6-9-2010 at 09:55

I'm sure a lot can be optimized and tailored to one's personal needs, but the most important thing is that there is reported success and that white P is not only synthesized, but also isolated in more than microgram quantities. I have seen many other reports before, but that always was in the line of that some white glow could be detected, indicating that some posphorus is formed, but never have I seen before that a macroscopic blob of white P was isolated. That is the good thing of this achievement.

I personally have enough white P with 10 grams or so, good for a few nice demo's but of course, if you want to make PCl3 or whatever chemical, then it is nice to have a little more.

Rogeryermaw - 7-9-2010 at 07:15

a couple points of interest i have noticed after several runs: the slag formed is quite foamy due to the gasses evolved forming bubbles. it will expand to roughly 3-4 times its original volume so be sure there is plenty of space in the reactor. if your slag reaches too far and expands in the pipe outside of the furnace it will solidify and block the flow of P4. dry reactants are important for reducing the amount of P4 lost to the production of PH3. also i am still testing with this but it seems the reaction happens in phases. first the heat expands the air in the pipe and there will be some bubbling of gases in general (probably last traces of moisture and atmospheric gases) then when reaction temp is reached there may be a bit of PH3 evolved but the P4 definitely seems to come over last. my most successful run involved heating far beyond when i thought the reaction was complete...near a full hour of the most intense heat i could muster. also if you use hot water to collect in the condenser needs to be more deeply submerged as the hotter your H2O is the slower it will cool the P4 gas. if the P4 gas doesn't cool fast enough it will remain gaseous and surface, igniting and becoming a total loss. i will not attempt to claim that suckback is not a danger but i have not encountered it yet so i am trying to get more creative with my condensation setup to increase yield. any progress will be reported here.

blogfast25 - 7-9-2010 at 07:49

The foaming is normal of course, even w/o PH3. I was just looking at the slag in the crucible of my only run with NaPO3/Al/SiO2 and it's highly bubbly/foamy (now frozen of course). I wonder if there's an inert ingredient that could be added to reduce the slag viscosity and thus facilitate releasing the P4. Something like ordinary salt (NaCl) with an MP of 801 C might just be the ticket. The eutectic NaCl/KCl has an even lower MP at 658 C.

Slag fluidisers (or fluxes) are very commonly used where slag viscosity is high, see also the use of CaF2 (fluorite) as a flux in Thermite reactions or other metallurgical reductions... The salt would condense way before the P4 of course...

A low melting flux can improve contact between the reagents, and even depassify Al because it 'dissolves' Al2O3...

[Edited on 7-9-2010 by blogfast25]

Rogeryermaw - 7-9-2010 at 08:52

those are very interesting ideas worth exploring. perhaps the P4 can bubble out with less resistance if the melt is less viscous. definitely worth investigation... one last thing i forgot to mention: a syringe with a 20 or 22 gauge needle is perfect for drawing out the product without contaminants. just be sure to keep it warm and when you "inject" it into your storage container (also warm) don't push too fast or small globs will surface and ignite. after you complete this operation just cap and allow to cool.

blogfast25 - 7-9-2010 at 11:40

Interesting about the syringe...

I would try one with 10 w% of NaCl (or eutectic if you can get some) on top of the charge (100 charge + 10 salt). Powder the (dry!) salt in a mortar and see if makes any difference. I think it might...

Rogeryermaw - 7-9-2010 at 21:27

your advice has been pretty solid. it would be foolish to ignore you now. i will run it. i am also in the design stage for a larger run with new furnace with firebrick...well generally less ghetto all around. that painting of hennig brand(t) gave me more than one idea! i am thinking about a cook pan of stainless...with a lid...latched shut or perhaps a breakable tack weld...with piping threaded into it and adapted to soft copper tubing outside of the brick furnace. closer to the scale they would have run in older days...(hmmmmm)

i broke off a small chunk and put it in a vial so i could watch it glow...

[Edited on 8-9-2010 by Rogeryermaw]

blogfast25 - 8-9-2010 at 05:01

your advice has been pretty solid. it would be foolish to ignore you now. i will run it. i am also in the design stage for a larger run with new furnace with firebrick...well generally less ghetto all around. that painting of hennig brand(t) gave me more than one idea! i am thinking about a cook pan of stainless...with a lid...latched shut or perhaps a breakable tack weld...with piping threaded into it and adapted to soft copper tubing outside of the brick furnace. closer to the scale they would have run in older days...(hmmmmm)

i broke off a small chunk and put it in a vial so i could watch it glow...

[Edited on 8-9-2010 by Rogeryermaw]

Re. the flux, only a test can show whether it works or not but it really feels like one of these situations where reducing the viscosity of the melt can only be beneficial...

Higher up, I suggested a design based on a stainless steel teapot, you know, the ones with distinct spout. Then weld a bent steel or copper tube onto the spout, leading into the condenser. Heat by inserting the whole thing into a furnace or by Bunsen/propane flame torches/Meker burner. But I never followed up on it...

Rogeryermaw - 9-9-2010 at 07:24

teapot's not a bad idea. half the work is done for you...have to keep in mind...need one where the spout is not connected to the body at a low point or the spout will fill with slag and the melt will be pushed out of the spout when gases develop in the chamber.

Rogeryermaw - 21-9-2010 at 07:07

had to order more NaPO3. just came in so i can continue with this line of experimentation. i'm going to give the NaCl idea a try to see if it can help with releasing the gas. i'll let you know what i find.

metalresearcher - 21-9-2010 at 10:38

Propane is a good option. I can reach 1400-1500oC easily with propane with forced draft with a simple $10 airbed inflater.
As long as you insulate the furnace chamber well you can reach it witin 15 minutes starting from a cold furnace.

See my experiences with iron casting on www.metallab.net/propanefurnace .

Rogeryermaw - 21-9-2010 at 12:23

thanks for the link. that is some nice work and i hope you don't mind my thievery but i'm going to steal some ideas from you. there is a fireplace supplier not too far from me that sells refractory cement and high alumina firebrick.

metalresearcher - 21-9-2010 at 22:59

No problem that is the reaso that I publish it on the internet !

aax - 23-9-2010 at 10:01

thanks for the link. that is some nice work and i hope you don't mind my thievery but i'm going to steal some ideas from you. there is a fireplace supplier not too far from me that sells refractory cement and high alumina firebrick.

You ran the experiment multiple times and experienced positive results on multiple occasions. It is time to post a detailed report and a video that will be around for ever. Please include any purification techniques, estimated cost per run, estimated time per run including preparation and clean up, and if possible how to convert it into red phosphorus.

aax - 23-9-2010 at 11:35

Quote: Originally posted by ScienceSquirrel

Correct. I'd use a 10 - 20 % excess of Al.

I haven't seen any posts concerning what is actually going on during this reaction...

[Edited on 23-9-2010 by aax]

blogfast25 - 23-9-2010 at 12:40

I haven't seen any posts concerning what is actually going on during this reaction...

[Edited on 23-9-2010 by aax]

That's because probably no one knows with any degree of certainty. Plausible reaction paths are:

1) Heat dissociates small amounts of NaPO3:

NaPO3 (l or s) ---> 1/2 Na2O (l or s) + 1/2 P2O5 (l or g)

2) Heat dissociates small amount of P2O5:

P2O5 (l or g) ---> 1/4 P4 + 5/2 O2 (g)

3) Al scavenges O2 under great development of heat: enthalpically speaking this is what drives the overall reaction:

3/2 O2 (g) + 2 Al (l) ---> Al2O3 (s) + much, much heat (about 1,670 kJ/mol in standard conditions)

4) Na2O and SiO2 combine:

Na2O (l or s) + SiO2 (s) ---> Na2SiO3 (s or l)

Reaction 4) may also help push step 1) to the right...

[Edited on 23-9-2010 by blogfast25]

aax - 23-9-2010 at 15:50

I haven't seen any posts concerning what is actually going on during this reaction...

[Edited on 23-9-2010 by aax]

I read in a previous post that P was released without silicon dioxide added.

(NaPO3)6 - Sodium hexametaphosphate
Al - Aluminium
SiO2 - Silicon dioxide

Rogeryermaw - 23-9-2010 at 16:33

without SiO2 to bind the sodium i have a feeling the reaction may not proceed. umm...where would i post a video? youtube is populated by fools waiting to kill themselves. it would be irresponsible to show them how to make a chemical that can kill with less than 50mg. i would love to share this with the chemist community and am willing to do so any time.

@ blogfast: i had a can of brake cleaner that was empty and i pulled the valve out. turned out to be a perfect fit for the 3/4 nipple i am using at the end of my reactor. i can't tell how much the NaCl helped but on this run i tripled the reactants and quadrupled the P4 output.

i would be glad to run it again and make a video if i knew a RESPONSIBLE place to put it. any ideas? i'm sorry i just really don't want the ATF at my door for showing idiots how to make the filler for deadly incendiary weapons, or giving the meth cooks a way to circumvent the authorities.

aax - 23-9-2010 at 16:55

where would i post a video? youtube is populated by fools waiting to kill themselves. it would be irresponsible to show them how to make a chemical that can kill with less than 50mg. i would love to share this with the chemist community and am willing to do so any time.

You read my mind... The solution is a title that consists of numbers only. Leave the rest of the fields blank.

Rogeryermaw - 23-9-2010 at 17:24

or could i perhaps post a private video on their server and just post a link here? i have plenty of reactants to run the synth several more times so i could run it tomorrow. tell you what i will run it and record it. then i'll post it as soon as we figure out how to keep it private while allowing science madness members to view it. so tomorrow i will run it again and record.

here is a look at what i have produced so far. after i melt and filter it again i doubt i will even lose a tenth of a gram.

DSCN0036.JPG - 70kB

you can tell by color which pieces are older.
if the scale is hard to read it says: 11.7 grams

[Edited on 24-9-2010 by Rogeryermaw]

[Edited on 24-9-2010 by Rogeryermaw]

peach - 23-9-2010 at 18:09

When you host the video, just click 'private' or 'not listed'.

Normal yougoddamntubers won't be able to see it, but you can then show it to specific groups.

In private mode, people will have to be subscribed to you and then you select them. In not listed mode, you simply post the link out to specific people (e.g. PM it on the board - DO NOT post it directly on the board. This forum is the reference standard for drugs / bombs, you'd be surprised where your posts turn up, how many are watching and how few are taking part).

You'll probably want to use private mode and have us all subscribe to you (which is a good idea if only so other science madness people can follow what you're up to more easily). It also means, should your link fall into the wrong hands, it's not going to appear posted all over the 'how to cook meth' threads.

I have spent a while thinking about this as well. As there are some videos I'd like to make that boarder too close on things that'll end up being reference material for cook along drugs, or that some angry guy could potentially make a reasonable weapon out of. Unfortunately, some very handy elements or chemicals are also handy for making mountains of drugs, nerve gas or high explosives. Cue, waking up in bed, balls naked at 4am, surrounded by six armed officers.

Or it'll just go wrong for someone without a bit of experience. There are tons of people watching youtube now setting up 'labs' at home. I expect a lot of them are teens. Previously, you'd have to hit the books and search engines to work out how to do something, usually being massively distracted by other possibilities and having to dig through other things to get to where you were going. Learning along the way. With the advent of youtube, a lot of those people now see a video and think "oooooo, that's easy, it only took ten minutes!". You'll often see in the comments for the million hit chemistry videos (the kewl ones), "I've done ... now what can I use any of this for?", repeated ad infinitum. So they have zero idea why they're doing something.

All youtube videos are now limited to 10 minutes to cut the piracy down (ARRRRR), even if you apply for a director / zen / whatever account (only the people who registered for them ages ago are allowed long videos). Which will encourage you to compact videos. The polar opposite of what the beginner needs. You can download free software to cut and paste clips together.

The standard youtube chemist will need you to explain a mole, as they try to make phosphorus.

How many of us would like to see some videos of Len's sodium method running and described? How many youtuber teens do you think would raid that? How many do you think have ever handled strong base solutions, let alone molten base, molten sodium, hydrogen gas or 50a+ of juice as separate entities, with that method needing it all in one place?

Not a lot.

[Edited on 24-9-2010 by peach]

aax - 23-9-2010 at 18:48

or could i perhaps post a private video on their server and just post a link here? i have plenty of reactants to run the synth several more times so i could run it tomorrow. tell you what i will run it and record it. then i'll post it as soon as we figure out how to keep it private while allowing science madness members to view it. so tomorrow i will run it again and record.

here is a look at what i have produced so far. after i melt and filter it again i doubt i will even lose a tenth of a gram.

you can tell by color which pieces are older.
if the scale is hard to read it says: 11.7 grams

[Edited on 24-9-2010 by Rogeryermaw]

[Edited on 24-9-2010 by Rogeryermaw]

I think a link would work fine... Someone is eventually going to make a video of this reaction anyways.

Rogeryermaw - 23-9-2010 at 19:06

I think a link would work fine... Someone is eventually going to make a video of this reaction anyways. [/rquote]

possibly so but if it was that easy the phosphorus thread wouldn't be eight years old. don't push so hard. it makes you seem like one of the bad guys.

also if someone else wants to post it then please do. it will absolve me of guilt when this synthesis is misused.

i have no fear for the likes of peach, blogfast, polverone or many of the other chemists i have followed who show their knowledge and experience but these days, in the usa, our government has a way of protecting the ignorant and persecuting the independent. if i give a tool to be used and that tool ends up hurting someone i could be in litigation for years...or worse. i have a family to think of...
[Edited on 24-9-2010 by Rogeryermaw]

[Edited on 24-9-2010 by Rogeryermaw]

peach - 23-9-2010 at 21:03

aax
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It is time to post a detailed report and a video that will be around for ever. Please include any purification techniques, estimated cost per run, estimated time per run including preparation and clean up, and if possible how to convert it into red phosphorus.

I think a link would work fine...

You're asking for a lot more than I think you realize.

I'll host it for you if you like Roger, although I think you'll be okay so long as you set it to private. Besides, you probably know who's been most active in this thread.

blogfast25 - 24-9-2010 at 04:21

Hard to prove but I think the salt's probably increased yield somewhat...

Good work, Roger!

On the question of silica much debate has been held upstairs. Personally I don't believe it's indispensable but that it helps a lot.

Video? A good set of pix would satisfy me totally...

Rogeryermaw - 24-9-2010 at 07:29

ok i'm on it today. certainly no one minds if i don't post the mundane details like chopping wood for the fuel? hard to video my self running the chainsaw and all...talk about unsafe!

since silica is basically glass it probably makes the melt more viscous but since i have it on hand and its use has been successful so far i'm going to keep it the mix for now.

peach - 24-9-2010 at 08:19

Video? A good set of pix would satisfy me totally...

True, but youtube's free and can convey so much with so little effort on the now defunct reader's part, so it's easier to avoid little questions that may be answered by seeing something and hearing about it in video form. And it's fun to watch something that's not TV. The labs are now using things like google to store and mine data between each other, which massively speeds things up.

ok i'm on it today. certainly no one minds if i don't post the mundane details like chopping wood for the fuel? hard to video my self running the chainsaw and all...talk about unsafe!

After much filming of reactions and related things, I can assure you balancing the camera on something or getting a cheapo old, thrown away tripod is a great idea (both of mine are someone else's junk, and I didn't buy the camera either). A tripod is good even if it's just one of these tiny desktop things, so you can balance the camera on a brick and then point it where you want it without wedging things underneath and having it topple half way through. Trying to handle glass full of hot chemicals, the 240V mains or a chainsaw with a camera in the other hand is not fun at all.

I'm searching out local science or industrial places at the moment, like accelerators, plasma fusion experiments, x-ray light sources and, if I can find anywhere still doing it, I'll see if I can find a phosphorus plant (although, there's only one in Europe I think). A phosphorus plant would be an amazing video for this thread.

ICI have a huge chemical facility 15 minutes from my house (it's miles long and wide). And I've been trying to get into the QuickFit glass blowing workshop with a camera (It's in Stone, Staffordshire if anyone's close). I also know a contractor for one of the nuclear plants and have a family member who works in a fairly high up position at one of them (quite a famous one where plutonium is bred), I'm working on a visit to the reactors

; that's going to take effort and paperwork (needs the government to say it's okay), and I seriously doubt they'll want me making videos of the inside. But.... if you don't ask....

The technicians get really excited and helpful when they realize someone is actually interested and not doing a 'not in my backyard' on them. I got a page long reply from one of them all about waste disposal when I made the joke that it was more decayed when it came out the reactors than when it went in, and that I'd buy it all if they wanted.

[Edited on 24-9-2010 by peach]

blogfast25 - 24-9-2010 at 09:09