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Author: Subject: Preparation of elemental phosphorus
blogfast25
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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
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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
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 Quote: Originally posted by Rogeryermaw 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
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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
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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
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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 International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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 International Hazard Posts: 537 Registered: 7-9-2010 Member Is Offline Mood: Reactive No problem that is the reaso that I publish it on the internet ! aax Harmless Posts: 13 Registered: 23-9-2010 Member Is Offline Mood: No Mood  Quote: Originally posted by Rogeryermaw 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 Harmless Posts: 13 Registered: 23-9-2010 Member Is Offline Mood: No Mood Quote: Originally posted by blogfast25  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. I haven't seen any posts concerning what is actually going on during this reaction... [Edited on 23-9-2010 by aax] blogfast25 Thought-provoking Teacher Posts: 10334 Registered: 3-2-2008 Location: Old Blighty Member Is Offline Mood: No Mood  Quote: Originally posted by aax 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 Harmless Posts: 13 Registered: 23-9-2010 Member Is Offline Mood: No Mood Quote: Originally posted by blogfast25  Quote: Originally posted by aax 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] I read in a previous post that P was released without silicon dioxide added. (NaPO3)6 - Sodium hexametaphosphate Al - Aluminium SiO2 - Silicon dioxide Rogeryermaw International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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 Harmless Posts: 13 Registered: 23-9-2010 Member Is Offline Mood: No Mood  Quote: Originally posted by Rogeryermaw 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 International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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] peach Bon Vivant Posts: 1428 Registered: 14-11-2008 Member Is Offline Mood: No Mood 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 Harmless Posts: 13 Registered: 23-9-2010 Member Is Offline Mood: No Mood  Quote: Originally posted by Rogeryermaw 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 International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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 Bon Vivant Posts: 1428 Registered: 14-11-2008 Member Is Offline Mood: No Mood aax Registered: 23-9-2010 <------------------ Yesterday Posts: 5 Search Preparation of elemental phosphorus Preparation of elemental phosphorus Preparation of elemental phosphorus Preparation of elemental phosphorus Preparation of elemental phosphorus  Quote: Originally posted by aax 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.  Quote: Originally posted by aax 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 Thought-provoking Teacher Posts: 10334 Registered: 3-2-2008 Location: Old Blighty Member Is Offline Mood: No Mood 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 International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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 Bon Vivant Posts: 1428 Registered: 14-11-2008 Member Is Offline Mood: No Mood  Quote: Originally posted by blogfast25 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.  Quote: Originally posted by Rogeryermaw 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 Thought-provoking Teacher Posts: 10334 Registered: 3-2-2008 Location: Old Blighty Member Is Offline Mood: No Mood  Quote: Originally posted by Rogeryermaw 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. Higher up there is strong research evidence that in the case of the Ca3(PO4)2 + C reaction, silica plays a vital part. That's where the idea of including silica in the metaphosphate - Al mix came from. Silicates, like glass, tend to have lower melting points than actual silica... Rogeryermaw International Hazard Posts: 654 Registered: 18-8-2010 Member Is Offline Mood: No Mood 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. there is already much stink from the extreme leftists that phosphates are bad for the environment so with this new development that may just be another nail in the coffin. may want to stock up while it's cheap and available...check dharmatrading on ebay. it's under$6 a pound before shipping. i've ordered from them twice and received my orders quickly. 3 business days or less from west coast to mid south.

reactants are measured and in the oven drying now. many photos taken.

[Edited on 24-9-2010 by Rogeryermaw]

[Edited on 24-9-2010 by Rogeryermaw]
Rogeryermaw
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and for aax: if you want to know the cost per run it's almost negligible. but you have to build a furnace which requires a body, refractory compound, fuel, forced air induction, associated piping ect. it's the first run that's gonna cost you. there are so many variable possibilities to the setup that a proper cost analysis is impossible.

ok fellas. everything is ready. i have to go pick my daughter up from school. when i get back and set her and my son up with 'toons and a snack i'll get on it!

i have noticed that running the synth with double the stoichiometric amount of silica has kept the slag volume low.

[Edited on 24-9-2010 by Rogeryermaw]

[Edited on 24-9-2010 by Rogeryermaw]
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 Sciencemadness Discussion Board » Fundamentals » Chemistry in General » Preparation of elemental phosphorus Select A Forum Fundamentals   » Chemistry in General   » Organic Chemistry   » Reagents and Apparatus Acquisition   » Beginnings   » Responsible Practices   » Miscellaneous   » The Wiki Special topics   » Technochemistry   » Energetic Materials   » Biochemistry   » Radiochemistry   » Computational Models and Techniques   » Prepublication Non-chemistry   » Forum Matters   » Legal and Societal Issues   » Detritus   » Test Forum