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Author: Subject: Quest for the elements
Agari
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[*] posted on 11-11-2015 at 15:24


Quote: Originally posted by j_sum1  
Good question. I know little. Except that there are a large number of variables to play with -- substrate, concentration, current density, temperature, agitation, surfactants, impurities and the presence of other ions.

My copper electrode is built up on a copper wire and is quite a dense solid mass. It looks ugly since I did a bit of electrolysis with carbon anodes and so it has fine carbon dispersed throughout. I get a small amount of Cu powder deposit but that is really minor. I don't get long dendrites but I guess the copper is probably dendritic on a smaller scale.

If I was aiming for a particular form, I would read the literature and follow a recipe.
My intention at some stage is to electrorefine my ugly electrode and produce a cleaner and more pleasant-looking copper sample for the element collection. So... if you come across a method that results in beautifully-formed crystals, I am interested.


As for the CuO thermite -- it's all over in a few seconds. It would easily be mistaken as a dust cloud -- perhaps sawdust unless you were up close. In a windy day, there would be perhaps a 20 second opportunity to notice something suspicious. For a small thermite you should get away with it fairly easily.

And then all that will be left to do is to collect the scattered copper,great! That is,if it is done inside or anywhere where it would be easy to collect the copper, or does it simply melt through any ceramic container and pour out in a manner similar to the iron thermite reaction, along with producing a large cloud of copper?

[Edited on 11-11-2015 by Agari]




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[*] posted on 11-11-2015 at 15:34


Quote: Originally posted by Agari  

And then all that will be left to do is to collect the scattered copper,great! That is,if it is done inside or anywhere where it would be easy to collect the copper, or does it simply melt through any ceramic container and pour out in a manner similar to the iron thermite reaction, along with producing a large cloud of copper?
[Edited on 11-11-2015 by Agari]


I don't think I would try this; the reaction already occurs explosively in the open. Confining it to try and collect the copper sounds like a really bad idea. Look up some videos to see what I'm talking about.

If you're after copper there are much better ways to get it. You can make solid copper by electrolysis on a copper wire, or you can get the powder by electrolysis on a graphite electrode. You can also put a piece of aluminum foil in a solution of a copper salt.
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[*] posted on 11-11-2015 at 15:39


All the CuO thermites I have done have produced a nice-looking brown cloud for a few seconds. There was no copper retrievable.
But if you include a slag material, a lot of the energy goes into heating up and melting the slag rather than boiling off your product. A good choice will allow the slag to float on top of the metal and protect it from the atmosphere.

I have little experience with these kinds of additions. I do know that some playing with the thermodynamics calculations is of great benefit. It seems to me that a decent thermite spreadsheet should be added to the list of things to do.

Beyond that, ask Blogfast. He is our resident thermite expert and has devised more than a couple of novel methods. He would be able to tell you off the top of his head what procedure is likely to work for copper.
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[*] posted on 11-11-2015 at 20:55


J_sum1,do you happen to have Cadmium or Phosphorus in your collection? If so,how did you obtain them?
Is there any good supplier that will sell white or red phosphorus? The reason I want white phosphorus is because it is more...rare than red phosphorus,looks better in my opinion,and is also more flammable of the two,so it could be considered unusual.




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[*] posted on 11-11-2015 at 21:02


I have Cd. I bought that from www.onyxmet.com. It was pretty cheap. i also have a NiCad battery that I intend to disassemble at some stage.

Onyxmet also sells red P. Sometimes. You should ask. And also ask about packaging and importing. Clearly there are issues there.

I intend to scrape some matchboxes for red P and then convert some to white. Obviously this will be small scale. I also have eventual plans to synthesise some white P using one of the successful methods outlined in the elemental phosphorus thread (see sticky.)

There are other allotropes of P but I will probably resort to buying those.
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[*] posted on 11-11-2015 at 21:06


Quote: Originally posted by j_sum1  
I have Cd. I bought that from www.onyxmet.com. It was pretty cheap. i also have a NiCad battery that I intend to disassemble at some stage.

Onyxmet also sells red P. Sometimes. You should ask. And also ask about packaging and importing. Clearly there are issues there.

I intend to scrape some matchboxes for red P and then convert some to white. Obviously this will be small scale. I also have eventual plans to synthesise some white P using one of the successful methods outlined in the elemental phosphorus thread (see sticky.)

There are other allotropes of P but I will probably resort to buying those.

There is a method of synthesizing violet P, but it seems far-fetched:
https://en.wikipedia.org/wiki/Allotropes_of_phosphorus#Hitto...
I just had to post that.




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[*] posted on 11-11-2015 at 21:07


There's a whole big thread on preparing phosphorus stickied in the General Chemistry forum. It's quite a task though, so it's understandable if you'd rather just buy it. Samples aren't hard to find, they're even on eBay.

Cadmium is actually on my to-do list for the near future. I ordered 150g of cadmium sulfide-hydroxide to experiment on. Once you make a water-soluble cadmium salt out of it, you can make the metal with electrolysis just like copper. For a cadmium thermite I have no idea, and I'm not too keen on trying it until I have some idea of what to expect.
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[*] posted on 11-11-2015 at 21:13


Yeah... I would avoid a cadmium thermite for the same reason I would avoid a lead thermite. Aerosol toxic metals are I think something to steer clear of.

On phosphorus, Rogeryermaw has a method in that thread that I think is worth emulating. He also has some youtube clips. But you should do your research, check safety issues, have an escape plan and act really carefully. Phos is rather unforgiving. It goes bang. It can gas you. It sticks to flesh, eats it and poisons you.
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[*] posted on 11-11-2015 at 23:32


Quote: Originally posted by j_sum1  

On phosphorus, Rogeryermaw has a method in that thread that I think is worth emulating. He also has some youtube clips. But you should do your research, check safety issues, have an escape plan and act really carefully. Phos is rather unforgiving. It goes bang. It can gas you. It sticks to flesh, eats it and poisons you.


I just read his post (Self note: Page 21), and it's a good process in theory,I should try it some time after my planned thermite experiment. As for the possible(?) synthesis of violet P, I don't know whether or not it is a feasible and practical to attempt,are there any flaws that you see in the procedure I mentioned earlier involving heating red phosphorus? The link to the Wikipedia article on the matter: https://en.wikipedia.org/wiki/Allotropes_of_phosphorus#Hitto...
It simply sounds too easy to possibly be true,maybe it's the temperature specified? Does the real procedure require something else to be done?
I am off for today though,it is late here and I still need phosphorus to work with.

[Edited on 12-11-2015 by Agari]




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[*] posted on 14-11-2015 at 22:40


Argh,I can't edit my posts for some reason.
What element is the OP of the thread currently after? I would like to perhaps obtain it too.




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[*] posted on 14-11-2015 at 22:41


I finally got red phosphorus,I will convert it to white tommorow.
I still can't edit my posts.




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[*] posted on 14-11-2015 at 22:43


I decided to do copper from thermite after I finish my entry for J_sum's contest.



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[*] posted on 15-11-2015 at 11:35


I'm currently working on manganese, to answer your above question.

I still don't know how you plan on getting anything but crude copper powder with the thermite.
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[*] posted on 15-11-2015 at 12:27


Quote: Originally posted by Upsilon  
I'm currently working on manganese, to answer your above question.

How do you plan to produce manganese? In my experience, manganese dioxide thermite is even more energetic than cupric oxide thermite, and attempts to electroplate manganese from aqueous solution more often yield oxides.
Quote: Originally posted by Upsilon  
I still don't know how you plan on getting anything but crude copper powder with the thermite.

In the relevant thread, I demonstrated a slower-burning copper thermite using sulfates. This produced a slag of sulfates, sulfides, silicates (from the bentonite the thermite was ignited upon), and bits of copper metal. Digestion of the slag in concentrated sodium hydroxide solution is (gradually) revealing particles of copper metal over 1/4" across. With some refinement, it may be possible to produce sizable copper globules from a thermite-type reaction.

[Edited on 15-11-2015 by MolecularWorld]




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[*] posted on 15-11-2015 at 13:43


Quote: Originally posted by MolecularWorld  

How do you plan to produce manganese? In my experience, manganese dioxide thermite is even more energetic than cupric oxide thermite, and attempts to electroplate manganese from aqueous solution more often yield oxides.


Earlier in this thread somewhere I posted my idea. I plan on electrolyzing molten semi-hydrated manganese(II) acetate. Completely anhydrous is too difficult to get but I can get it down to a low enough water content so that it won't attack the manganese metal too badly.
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[*] posted on 15-11-2015 at 17:30


Does anyone know anything about extracting yttrium from yttrium oxide (Y2O3)? I just received 30g of it today. Yttrium seems to be very high in the activity series (quite a bit above aluminum) so I don't know if a thermite would work. Perhaps it should be done
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[*] posted on 15-11-2015 at 19:23


Quote: Originally posted by Upsilon  
Does anyone know anything about extracting yttrium from yttrium oxide (Y2O3)? I just received 30g of it today. Yttrium seems to be very high in the activity series (quite a bit above aluminum) so I don't know if a thermite would work. Perhaps it should be done

I am not a thermite specialist,but a yttrium oxide thermite with added contaminants to make it less potent,such as MolecularWorld's copper thermite, could be done,in theory.
Edit(Finally):What is your(Anybody reading this) opinion on the conversion of red or white phosphorus to violet P that I linked in a previous post? It simply sounds too easy to possibly be true,but I can't put my finger on the reason why.

[Edited on 16-11-2015 by Agari]




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[*] posted on 15-11-2015 at 20:47


I've got a lead:
http://www.sciencemadness.org/talk/viewthread.php?tid=10249&...

This looks promising. My Y2O3 is supposed to be 99.95%+.
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[*] posted on 16-11-2015 at 21:27


I am going to try a silicon dioxide thermite reaction. The silicon dioxide will come from first synthesizing silicon tetrachloride by first passing chlorine gas through a bubbler of sulfuric acid and then to a reaction tube with silicon powder. The reaction tube will be attached to an ice-cold condenser and the sulfur dichloride contamination filtered using a piece of cotton. Silicon tetrachloride reacts with water to form hydrochloric acid and silicon dioxide as follows:
SiCl4 + 2 H2O = SiO2 + 4 HCl
I am going with a thermite reaction using already-bought silicon just for good memories,I know it is very inefficient.
I am still holding out on a copper thermite.

[Edited on 17-11-2015 by Agari]




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[*] posted on 16-11-2015 at 21:35


Agari, you could just use sand.
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[*] posted on 16-11-2015 at 21:42


Quote: Originally posted by j_sum1  
Agari, you could just use sand.

Pfft,what is fun about using sand though, when I could go with the more sophisticated route and use silicon tetrachloride?




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[*] posted on 17-11-2015 at 06:43


My experience with thermites seems a bit different than others. I tried a copper(II) oxide thermite and it went fairly slowly, and I still recovered very little copper metal. Possibly because I made the oxide and it may have had some contamination (it's been so long I don't remember with what, though). I've recovered decent BB-sized manganese pieces from a MnO<sub>2</sub> thermite, which to me seems only slightly more energetic than the regular iron oxide blend. The difficulty there of course is that manganese's boiling point is close to the melting point of alumina, so it's very difficult to get large pieces this way. But still possible to yield something for display.

I've done a number of different types of thermite, and posted the results in my thermite compilation video: https://www.youtube.com/watch?v=OwCHWO2EhbI
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[*] posted on 17-11-2015 at 14:38


I watched your thermite compilation with my class yesterday, MHS. I provided my own voice-over. And yes, your copper one was rather different from what I have experienced. One factor may be that my CuO is really fine. I typically get a brown cloud that I presume is metallic copper. And I have an empty flower pot left behind.
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[*] posted on 17-11-2015 at 15:15


Good luck with the SiO2 thermite Agari, I couldn't get anything worth saving from it. The metal(loid) always failed to coalesce effectively. I got blobs of it but they were actually just tiny grit-like pieces clumped together, and they weathered very quickly.
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[*] posted on 17-11-2015 at 17:24


So the manganese dioxide I started the manganese acetate experiment with has some amount of iron contamination, indicated by the yellowish color of the manganese acetate solution. I know it doesn't take much iron at all to cause some discoloration, but I just don't know how much I have. I've been thinking of ways to test it, and I may have something worth trying. If I precipitate out both the iron and manganese compounds by adding sodium carbonate, then react these carbonates with hydrochloric acid, what type of iron chloride would I get - (II) or (III)? I suspect that I would get (II). For what I have in mind, I need iron(III) chloride, so would I be able to add hydrogen peroxide to oxidize it to iron(III) without oxidizing the Mn(II) to some higher state? Wikipedia says that FeCl3 quickly reacts with oxalates to afford the [Fe(C2O4)3]3- complex.

Well, that's as far as I'm going to go with it for now. Too many "what ifs" already.
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