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Author: Subject: Quest for the elements
Upsilon
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[*] posted on 28-9-2015 at 16:31
Quest for the elements


I'm soon to embark on a journey to collect as many of the natural elements as I can by isolating them from compounds containing them. Obviously some will need to be purchased, like the noble gases, but I want to produce as many of them myself as possible. Sure I could just buy samples, but I would find no enjoyment in that.

Needless to say some elements will be more difficult to isolate than others. I will need advice from you all on occasion when I come across a difficult problem. Instead of making a new thread every time I run into an obstacle, I'll just let this thread serve as a sort of journal for my experiences in trying to isolate elements, which I will also use to outsource advice from the community.

And to start it off: I need help with beryllium. Its compounds aren't particularly useful in chemistry so they are virtually impossible to find. However, it does find use as a component in some alloys. It is also found in some fairly common minerals, such as beryl and bertrandite.

That being said I see two viable options. I can try and refine it out of a mineral (research suggests treating crushed bertrandite with sulfuric acid leaves a water-soluble sulfate, but sulfate of what?), or I can try to separate it from an alloy. I have noticed that beryllium-copper alloys are used in certain golf club heads, which aren't terribly expensive. Perhaps treatment with some HCl would tear out the beryllium and leave the copper behind?
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elementcollector1
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[*] posted on 28-9-2015 at 16:42


I believe plante1999 posted our only thread on extracting beryllium compounds, and he used crushed raw beryl.
http://www.sciencemadness.org/talk/viewthread.php?tid=23007
Beryllium-copper is expensive and has low beryllium content - best to go with the mineral.

Remember, Be is fairly toxic!

[Edited on 9-29-2015 by elementcollector1]




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Velzee
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[*] posted on 28-9-2015 at 16:44


I'm no expert, but since beryllium has a slight higher melting point than copper, could you just heat the club up to melt the copper out, leaving Be behind?



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Little_Ghost_again
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[*] posted on 28-9-2015 at 16:51


I think you can get it from microwave ovens! be careful though as breathing the dust is bad news. Its normally like a ceramic disk in the magnatron, so find an old microwave and bingo



be.jpg - 130kB
found this on google I think its the pink bit :D

[Edited on 29-9-2015 by Little_Ghost_again]




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Upsilon
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[*] posted on 28-9-2015 at 17:09


Quote: Originally posted by elementcollector1  
I believe plante1999 posted our only thread on extracting beryllium compounds, and he used crushed raw beryl.
http://www.sciencemadness.org/talk/viewthread.php?tid=23007
Beryllium-copper is expensive and has low beryllium content - best to go with the mineral.

Remember, Be is fairly toxic!

[Edited on 9-29-2015 by elementcollector1]


Will definitely be looking into that. Seems like a mammoth task but a fun one as well

Velzee, alloys have one specific melting point. Take solder for electrical circuits, for example. It is composed of tin and lead, leading to a material that melts at a significantly lower temperature than either of the constituent metals.
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[*] posted on 28-9-2015 at 17:34


If you came across an (expensive) alloy of Cu/Be (Used for non-sparking tools, at 4%Be) you could have a go at isolating it from that.
For me, it was an element I bought for a couple of bucks.
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[*] posted on 28-9-2015 at 18:06


Obtaining Be compounds (typically BeSO<sub>4</sub> if you're taking an aqueous route) from Beryl or some other source is only a small part of the problem. Isolating the metal, if that's what you desire is far far harder and possibly very hazardous as a process.

Quote: Originally posted by Little_Ghost_again  
I think you can get it from microwave ovens! be careful though as breathing the dust is bad news. Its normally like a ceramic disk in the magnatron, so find an old microwave and bingo




found this on google I think its the pink bit :D

[Edited on 29-9-2015 by Little_Ghost_again]


Please post the link.

Oh, this one?

https://www.youtube.com/watch?v=4Zev8Ws4P1Y

He couldn't tell Be from his *rse. Low level info that should be ignored.


[Edited on 29-9-2015 by blogfast25]




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Upsilon
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[*] posted on 28-9-2015 at 19:09


Quote: Originally posted by blogfast25  
Obtaining Be compounds (typically BeSO<sub>4</sub> if you're taking an aqueous route) from Beryl or some other source is only a small part of the problem. Isolating the metal, if that's what you desire is far far harder and possibly very hazardous as a process.

[Edited on 29-9-2015 by blogfast25]


Yes, I would need to learn what to watch out for with isolating it. I'm still quite far off from doing any of this yet, but when I get to it, it'll almost certainly be by electrolysis (either of a molten beryllium salt in an inert atmosphere, or in propylene carbonate if I can ever get that to work).
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[*] posted on 28-9-2015 at 22:47


You could akways practise isolating Mg from epsom salt and when you had perfected that, move onto Be.
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Little_Ghost_again
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[*] posted on 29-9-2015 at 00:28


All I did was post a pic of the part needed, why is that low level information to be ignored?

[Edited on 29-9-2015 by Little_Ghost_again]




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[*] posted on 29-9-2015 at 07:05


BeO ceramics can also be found in high power (RF) transistors. It has excellent thermal conductivity.



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[*] posted on 29-9-2015 at 07:59


I found this on eBay:
http://ebay.com/itm/WHOLESALE-2lb-Lot-GREEN-BERYL-AQUAMARINE...

Seems like a really good deal; for this purpose it would be better to buy rough, ugly samples like this instead of the really good-looking crystals.
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[*] posted on 29-9-2015 at 08:55


I would be really careful handling Be. If Be powder is inhaled it can cause beryllium lung disease if you are susceptible. I have no Be or Be compounds in my lab and don't ever plan to.

Be was once used for nuclear fuel fabrication. Many of the fabrication workers now have this lung disease. Many lawsuits and much money is now involved.




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[*] posted on 29-9-2015 at 09:11


Quote: Originally posted by Little_Ghost_again  
All I did was post a pic of the part needed, why is that low level information to be ignored?



Because the video maker only states that it's Be ceramic but provides nothing to back that up with. Anyone can make such claims.




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[*] posted on 29-9-2015 at 09:16


Quote: Originally posted by Magpie  
I would be really careful handling Be. If Be powder is inhaled it can cause beryllium lung disease if you are susceptible.


Unless you're working with Be (or compounds) based powders, ordinary precautions (don't inhale or ingest) should suffice. We're not talking about mass fabrication here.

Originally the element was called 'glucinium' because its 'salts' taste sweet.

[Edited on 29-9-2015 by blogfast25]




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[*] posted on 29-9-2015 at 09:21


Quote: Originally posted by Upsilon  
I found this on eBay:
http://ebay.com/itm/WHOLESALE-2lb-Lot-GREEN-BERYL-AQUAMARINE...

Seems like a really good deal; for this purpose it would be better to buy rough, ugly samples like this instead of the really good-looking crystals.


Really good looking crystals of this stuff are gems or at least semi-gems and would be seriously expensive. https://en.wikipedia.org/wiki/Emerald

But even for these 'ore grade' pieces I would seek reassurance (like a certificate) from the seller. Then, good luck processing it: it's incredibly hard stuff, see also the link higher up. http://www.sciencemadness.org/talk/viewthread.php?tid=23007&...

[Edited on 29-9-2015 by blogfast25]

[Edited on 29-9-2015 by blogfast25]




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[*] posted on 29-9-2015 at 11:37


Quote: Originally posted by blogfast25  
Quote: Originally posted by Upsilon  
I found this on eBay:
http://ebay.com/itm/WHOLESALE-2lb-Lot-GREEN-BERYL-AQUAMARINE...

Seems like a really good deal; for this purpose it would be better to buy rough, ugly samples like this instead of the really good-looking crystals.


Really good looking crystals of this stuff are gems or at least semi-gems and would be seriously expensive. https://en.wikipedia.org/wiki/Emerald

But even for these 'ore grade' pieces I would seek reassurance (like a certificate) from the buyer. Then, good luck processing it: it's incredibly hard stuff, see also the link higher up. http://www.sciencemadness.org/talk/viewthread.php?tid=23007&...

[Edited on 29-9-2015 by blogfast25]


Thanks for the info. I'm going to be making my own little arc furnace at some point; hopefully I can actually get that hot enough to melt the beryl. Would definitely make it much easier to break apart. If not, a good old sledgehammer ought to do the trick.
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[*] posted on 29-9-2015 at 12:58


Quote: Originally posted by Upsilon  


Thanks for the info. I'm going to be making my own little arc furnace at some point; hopefully I can actually get that hot enough to melt the beryl. Would definitely make it much easier to break apart. If not, a good old sledgehammer ought to do the trick.


An arc furnace would be a good tool here: heat your pieces until they melt (or nearly melt), then quench them in cold water. The vitrification process changes the crystalline structure dramatically and the material then becomes much, much easier to grind. Grind under water to avoid dust.

As regards the sledgehammer, that's probably not a great idea unless you have an extremely strong surface you'll simply mostly be hammering beryl pieces into that surface.




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[*] posted on 29-9-2015 at 13:17


Reading your link to the Be experiments in the penultimate post reminds me of why i first came here and stayed.

Science, Chemistry, Facts, Experiments, Results !

There are even chemical equations in there to accompany the photos.

Time to turn SM around and re-take that Fascinating high ground and get back to some actual interesting Science instead of all these random chat-room style random Lizard Alien type comments that appear all the time.





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[*] posted on 29-9-2015 at 14:15


I've long contended that in recent years all that is good about SM, evidence based amateur science in a nutshell, is in decline. Although it's subjective and impossible to prove, that's what my perception tells me.

A turnaround would be great but I'm not holding my breath.

aga: if you're interested in experimentation with Beryl with the aim of preparing some BeO or BeSO<sub>4</sub>, let me know.

[Edited on 29-9-2015 by blogfast25]




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[*] posted on 1-10-2015 at 12:34


I will set aside the beryl experiment for later when I have better equipment, then. Next I would like to discuss phosphorus. My only phosphorus-containing compound is trisodium phosphate. Given the ability to make phosphoric acid from it, I have found the following half-reactions in the table of reduction potentials:
H3PO4(aq) + 2H+ + 2e- -> H3PO3(aq) + H2O (-0.276 V)
H3PO3(aq) + 3H+ + 3e- -> P(red) + 3H2O (-0.454 V)
H3PO3(aq) + 2H+ + 2e- -> H3PO2(aq) + H2O (-0.499 V)
H3PO2(aq) + H+ + e- -> P(white) + 2H2O (-0.508 V)
P(red) + 3H+ + 3e- -> PH3(g) (-0.111 V)
P(white) + 3H+ + 3e- -> PH3(g) (-0.063 V)

This suggests that these reactions occur in the presence of an acidic reducing agent, such as oxalic acid:
2CO2(g) + 2H+ + 2e- -> H2C2O4 (-0.430 V)

Based on this information, the first reaction is thermodynamically favorable:
H3PO4(aq) + H2C2O4(aq) -> H3PO3(aq) + 2CO2(g) + H2O

But after this, not even the reaction involving red phosphorus is thermodynamically favorable, let alone the one involving hypophosphorous acid (which is an intermediate to white phosphorus).

I'm not going to be picky about which type of phosphorus is in my collection (though it would be cool to have both), but I won't get either of them at 1M concentration at 25C. The question then becomes, how can I alter the reaction conditions to increase the favorability of, to keep things simple for now, the phosphorous acid to red phosphorus reaction, without going too far causing the formation of phosphine gas? I am aware of phosphine's toxicity and would prepare for its formation regardless, but its formation signals the loss of elemental phosphorus, which I don't want to happen.
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[*] posted on 1-10-2015 at 14:18


I hate to be a spoilsport, but ASAIK there is no practical way to reduce the phosphate anion to solid phosphorus, or even phosphite, in aqueous solution.
H3PO4(aq) + 2H+ + 2e- -> H3PO3(aq) + H2O (-0.276 V) vs
2CO2(g) + 2H+ + 2e- -> H2C2O4 (-0.430 V) reduction potentials may imply
H3PO4(aq) + H2C2O4(aq) -> H3PO3(aq) + 2CO2(g) + H2O
but in reality it will never work.
Time for the experts in aqueous phosphorus chemistry to weigh in.
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[*] posted on 1-10-2015 at 14:51


Quote: Originally posted by softbeard  
I hate to be a spoilsport, but ASAIK there is no practical way to reduce the phosphate anion to solid phosphorus, or even phosphite, in aqueous solution.
H3PO4(aq) + 2H+ + 2e- -> H3PO3(aq) + H2O (-0.276 V) vs
2CO2(g) + 2H+ + 2e- -> H2C2O4 (-0.430 V) reduction potentials may imply
H3PO4(aq) + H2C2O4(aq) -> H3PO3(aq) + 2CO2(g) + H2O
but in reality it will never work.
Time for the experts in aqueous phosphorus chemistry to weigh in.


I don't know whether the above scheme would work (I'm very sceptical about it) but one should understand that thermodynamics says NOTHING about kinetics. A thermodynamically favourable scheme does not mean that it will proceed at any appreciable rate.

Do you see a lot of coal (carbon) burst spontaneously into flames? If not, ask yourself why! :D:D (Hint: C + O2 ===> CO2 is highly thermodynamically favourable).

[Edited on 1-10-2015 by blogfast25]




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[*] posted on 1-10-2015 at 15:12


Quote: Originally posted by blogfast25  


I don't know whether the above scheme would work (I'm very sceptical about it) but one should understand that thermodynamics says NOTHING about kinetics. A thermodynamically favourable scheme does not mean that it will proceed at any appreciable rate.

Do you see a lot of coal (carbon) burst spontaneously into flames? If not, ask yourself why! :D:D (Hint: C + O2 ===> CO2 is highly thermodynamically favourable).

[Edited on 1-10-2015 by blogfast25]


I feel like this is true mainly for these half-reactions involving solids and gases (like your example of C + O2). Like in my H2S experiment in the other thread, the reaction is thermodynamically favorable, but both substances had to be melted to overcome the kinetic barriers (btw, I tried that experiment again and posted some goodies there). Perhaps with aqueous solutions, these barriers are overcome by the act of ionizing the substances? I don't know for sure; perhaps I will conduct this experiment this weekend or sometime during next week.

[Edited on 1-10-2015 by Upsilon]
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[*] posted on 1-10-2015 at 15:58


Well upsilon.
If it is phosphorus you are after then you can always scrape it off the side of matchboxes.
If it is phosphorus chemistry you are interested in then that is also not a bad start point. You can sublime to convert from red to white and this also acts to purify it. There are a few solvents you can play with also. There are a few threads around on oxygen and chlorine compounds of phosphorus.

If (as I suspect) it is the synthesis you want for your element collection and you want a reasonable sized sample, then this thread will be too small to contain the issues. Fortunately, there is a lengthy thread stickied on the production of white phos. There is lots to read there but it is almost guaranteed to answer any question you might have. The alchemists boiled down urine but there are other methods. SM member rogeryermaw is probably the person who had the most success. He also has a youtube clip showing his methodology. I like it. It is OTC (or almost). But there are significant hazards and phosphorus doesn't play fair. Be real careful and read up first.

Actually, let me emphasise that point. Do some reading. For most of the threads you have started, there are already significant threads discussing the question. There is a wealth of information on these boards and it is good to respect the expertise that has already been freely offered. There is also an advantage in having all the related information together in one place.

You and I have similar goals with regards to our element collections -- with the exception that you seem to want to tackle the difficult ones first. I think it is wiser to work up to the difficult/hazardous.
Here are some projects that I have either done or are on my short list -- all inspired by what I have read on SM
  • boron from borax
  • titanium from TiO2
  • silicon from sand
  • silver from old coins (There is a story behind that one.)
  • chromium from stainless steel cutlery
  • potassium from KOH (See the sticky. I have failed once at this and am keen to attempt again.)
  • sodium from electrolysis of NaOH
  • liquid chlorine
  • make my own gas discharge tubes

At present I have around 45 elements and probably almost 100 different samples. Phosphorus, neodymium and lanthanum are on my list too but they can wait until I upskill and accumulate the necessary equipment. Anyway, we should compare notes. U2U me if you want.
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