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Author: Subject: Radium extraction from watch hands
violet sin
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[*] posted on 1-10-2023 at 11:02


Reading old papers like said above offers a diverse wealth of information about the manipulation of radium in solution. The stuff that I was reading was like 1914. One an indepth solubility study on pure sulfate and the other a paper on processing from carnotite mineral for the use of vanadium, uranium in glazes and commercialization of radium content.

The sulfate is soluble In strong sulfuric acid, precipitates from Sol on dilution. Heat dissolves more, but of course it's relative, and a small amount, so things like +50% increase can be ... misleading a bit. Weak nitric will dissolve some, stronger acid strength will diminish solubility.

The radiochemistry of radium
US atomic energy division, December 1964


The solubility of pure radium sulfate
Journal of American chemical society, March 1918


I still suggest advanced knowledge on your radiation safety/detecting and electronics don't really help here. Being capable of measuring your success or failure is very handy of course.

Fusion with a carbonate seems rough given the lack of experience and limited tooling.

Dissolving all the metal of the watch hands seems to yield a method of freeing the paint residues, but so much extra is in play at that point, untangling your desired product seems unlikely.

You don't need a sparkling pure radium sulfate product, but you don't want to end up with it spread too far across all your steps, it's after all a very small amount.

Again I'd suggest working the paint off under liquid, possibly using a jewelry sonicator bath and some appropriate solvent or etch to help, maybe using a nifty small scale flask with pointy bottom (forgot the name).

Plating out radium isn't going to happen in water based on all the reading I've been doing. They did mention something about reducing the azide... Hahahahahahahaha no thanks.

I've no interest in trying to make someone look unintelligent, nor myself look a genius, because I'm not. But when I hear some of the things people say, and read what they intend to do... It's a bit scary. Disregard for radium, dust, accidental spills or breaks and the potential loss of an outbuilding doesn't seem like a fair trade for a "because I wanted to" type project.

If you didn't think it was a big deal, others reading it might. So do it smart, do it small scale, and figure out how to get from reclaimed paint to plated metal first. You may have to settle for salt impregnated ceramic or oxide coating on your metal disk. Don't know if you can get a conductive underlayment or not.

And with that I'll leave this to y'all, I've done my free time reading for the time being. Thanks for the opportunity to learn more on an interesting subject, and best of luck, stay safe

-VS-

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[*] posted on 1-10-2023 at 12:17


Quote: Originally posted by Tsjerk  


You not being a native speaker is not the problem, you not understanding what a melt is, is the problem. This has nothing to do with your lack of knowledge of the English language but with your lack of knowledge of chemistry.

If you were asking about fusing another metal than radium this might not be that big of a problem, but that is not the case here.

[Edited on 1-10-2023 by Tsjerk]

The user wrote fuse not melt, I know what melting is, I do bronze sword as one of my hobbies, I simply couldn't understand how would I get a temperature of 1500 degrees celsius to fuse radium properly, I have a propane furnace, not a oxiacetilene or electrical one.
I think the only difference is that one method melts the solid components while the other to boil the solution...

[Edited on 1-10-2023 by Telyron]
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Tsjerk
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[*] posted on 1-10-2023 at 12:32


How would you get sodium nitrate to 1500 degrees?

[Edited on 1-10-2023 by Tsjerk]
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[*] posted on 1-10-2023 at 13:01


Quote: Originally posted by Tsjerk  
How would you get sodium nitrate to 1500 degrees?

[Edited on 1-10-2023 by Tsjerk]

you said fuse, what temperature does the mixture have to reach? Radium melting point is at 700 degrees, copper (of the doping) at 1000... zinc 1700... I think maybe he meant boiling, unless just one component have to melt that does it at a lower temperature...
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[*] posted on 1-10-2023 at 13:15


Not a native speaker either, but my understanding is that:
melting = heating a material so that its state changes from solid to liquid
Fusing = melting a mixture of solid materials so they can mix (and sometimes react) in the liquid state

Similar but not the same.

With regard to that 'fusion' step. You are not melting radium metal (there is no radium metal in that paint, as you know), so the melting point of Ra is irrelevant.
You are fusing the mixture of materials (Na2CO3 and a nitrate), so the relevant melting points are in the range of the melting points of those salts. The actual melting point of the mixture may even be a bit lower than that of the pure salts (which is often the case with mixtures).

It's allright that you don't know, after all none of us were born with knowledge like this, but the fact that this wasn't already clear to you is indeed a sign that your chemistry knowledge isn't as good as it should be to attempt a project like this safely and successfully. I agree with Tjerk, that's not a language problem.

I also think you are seriously underestimating the difficulty of working with microgram/milligram amounts. A milligram of precipitate in more than a few milliliters of solution is going to be invisible. Its going to be a very, very fine coating on the wall of your glassware, which you can't actually see. Yes, centrifuging will help. But you really need more than a mg of barium.

I'm also wandering if Ra is actually the best material for your needs. I don't know very much about using isotopes directly for generating voltages, but I think any alpha or beta emitter will do. You can easily buy perfectly good Am241 sources. More uCi of activity, and much safer (no chemistry needed, and plated thinly onto a solid support for your convenience).

[Edited on 1-10-2023 by phlogiston]




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[*] posted on 2-10-2023 at 12:28


Quote: Originally posted by violet sin  
Reading old papers like said above offers a diverse wealth of information about the manipulation of radium in solution. The stuff that I was reading was like 1914. One an indepth solubility study on pure sulfate and the other a paper on processing from carnotite mineral for the use of vanadium, uranium in glazes and commercialization of radium content.

The sulfate is soluble In strong sulfuric acid, precipitates from Sol on dilution. Heat dissolves more, but of course it's relative, and a small amount, so things like +50% increase can be ... misleading a bit. Weak nitric will dissolve some, stronger acid strength will diminish solubility.

The radiochemistry of radium
US atomic energy division, December 1964


The solubility of pure radium sulfate
Journal of American chemical society, March 1918


I still suggest advanced knowledge on your radiation safety/detecting and electronics don't really help here. Being capable of measuring your success or failure is very handy of course.

Fusion with a carbonate seems rough given the lack of experience and limited tooling.

Dissolving all the metal of the watch hands seems to yield a method of freeing the paint residues, but so much extra is in play at that point, untangling your desired product seems unlikely.

You don't need a sparkling pure radium sulfate product, but you don't want to end up with it spread too far across all your steps, it's after all a very small amount.

Again I'd suggest working the paint off under liquid, possibly using a jewelry sonicator bath and some appropriate solvent or etch to help, maybe using a nifty small scale flask with pointy bottom (forgot the name).

Plating out radium isn't going to happen in water based on all the reading I've been doing. They did mention something about reducing the azide... Hahahahahahahaha no thanks.

I've no interest in trying to make someone look unintelligent, nor myself look a genius, because I'm not. But when I hear some of the things people say, and read what they intend to do... It's a bit scary. Disregard for radium, dust, accidental spills or breaks and the potential loss of an outbuilding doesn't seem like a fair trade for a "because I wanted to" type project.

If you didn't think it was a big deal, others reading it might. So do it smart, do it small scale, and figure out how to get from reclaimed paint to plated metal first. You may have to settle for salt impregnated ceramic or oxide coating on your metal disk. Don't know if you can get a conductive underlayment or not.

And with that I'll leave this to y'all, I've done my free time reading for the time being. Thanks for the opportunity to learn more on an interesting subject, and best of luck, stay safe

-VS-

Thank you for all the research you did, I will read the papers you attached.
I wasn't planning on dissolving the metals, I think it would contaminate too much with similar behaving elements, only add barium sulfate as a carrier (I think I am supposed to add it as the salt and not in elemental form)
I could get the necessary items to fuse it, its not a big deal, as I said I am planning to use this project to get into chemistry.
I did not get what issue you said will make using detectors, theoretically the only decay that emits gamma radiation is Ra226--->Rn222 so I should be able to use a gamma only detector (GM pancake as I have or scintillator that I will get in the future) to see wether what precipitated is radium or it remained in the solution.
What did you mean in "Precipitates from solution on dilution"? if I add solvent the radium precipitates? I always knew (from the base chemistry course we have at engineering school) that to make a solute precipitate you need to oversaturate the solution therefore adding solute or removing solvent... (or using a centrifuge)
I will inform myself on oxide deposition, but anyway pyrotronics made radium smoke detectors so some literature on how to get it onto something in a thin layer without coming apart should exist.
I am not a fool, I will before do a mockup isolation using some element of the same periodic group (barium or strontium) try to see the result with some method (I thought of flame test but I am opened to suggestions)
then I will try as soon as I get the procedure right with a small batch of hands, then with the whole set.
Again I don't think it to be easy that's why I asked for help here...
About safety I am not very concerned, I have a very sensible detector, I use a respirator, wash everything all the time, wear gloves, ventilate the area to minimise radon build up etcetera. I will perform the extraction in a garage I am about to rent, far from homes and where nobody will ever live.
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[*] posted on 2-10-2023 at 12:41


Quote: Originally posted by phlogiston  
Not a native speaker either, but my understanding is that:
melting = heating a material so that its state changes from solid to liquid
Fusing = melting a mixture of solid materials so they can mix (and sometimes react) in the liquid state

Similar but not the same.

With regard to that 'fusion' step. You are not melting radium metal (there is no radium metal in that paint, as you know), so the melting point of Ra is irrelevant.
You are fusing the mixture of materials (Na2CO3 and a nitrate), so the relevant melting points are in the range of the melting points of those salts. The actual melting point of the mixture may even be a bit lower than that of the pure salts (which is often the case with mixtures).

It's allright that you don't know, after all none of us were born with knowledge like this, but the fact that this wasn't already clear to you is indeed a sign that your chemistry knowledge isn't as good as it should be to attempt a project like this safely and successfully. I agree with Tjerk, that's not a language problem.

I also think you are seriously underestimating the difficulty of working with microgram/milligram amounts. A milligram of precipitate in more than a few milliliters of solution is going to be invisible. Its going to be a very, very fine coating on the wall of your glassware, which you can't actually see. Yes, centrifuging will help. But you really need more than a mg of barium.

I'm also wandering if Ra is actually the best material for your needs. I don't know very much about using isotopes directly for generating voltages, but I think any alpha or beta emitter will do. You can easily buy perfectly good Am241 sources. More uCi of activity, and much safer (no chemistry needed, and plated thinly onto a solid support for your convenience).

[Edited on 1-10-2023 by phlogiston]

Thank you for the clarification, the issue was that fusion in my language means the passage of a material from solid to a liquid phase, so I immediately thought of melting the metals, which looked strange to me.
I wasn't aware of this process of melting salts at a lower temperature than the pure metals, but makes sense, water liquefies at 273 kelvin while its component only a few Kelvin.
I know I lack chemistry notions, also if you can suggest somewhere to start studying it, its a knowledge poorly thaugth in schools...
About how difficult it would be I know, but I did the investment now I can't leave them to decay without doing anything... so I need a very thourogh procedure and the right equipment.
Americium crossed my mind, I thought about it all day ahahah
the main problem is that its decay mainly consists of alphas, litle beta and very few gammas. So to make a battery by differentiating the beta and alpha fluxes would be very weak (I already tried using 4 americium pellets without seeing any voltage)
Also another problem is that to have a similar activity from americium I should fuse 18 sources together, and they are plated onto tungsten and covered in platinum or gold foils, I don't have the slightest idea on how to fuse them successfully...
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[*] posted on 2-10-2023 at 14:36


Quote:
I know I lack chemistry notions, also if you can suggest somewhere to start studying it, its a knowledge poorly thaugth in schools...


I think your approach of thinking of a fun project you are enthusiastic about and then trying to learn whatever you need to know is a very good way. Actually experimentation is also very valuable and useful. The problem is that you picked a first project that is very risky, very unforgiving for mistakes and difficult (even if it wasn't dangerous). It is really something that most experienced chemists, even professional ones, would hesitate to do (if they would at all). You do not have this hesitation because you do not have all the experiences of things that can go wrong. It would be wise to gain experience with other things first, and consider coming back to this project in a few years time. The radium isn't going anywhere soon. Just store it somewhere safely.

Quote:
I did the investment now I can't leave them to decay without doing anything...


This is called the 'sunk cost fallacy'. Look it up if you want.
But, like I said, you can also just store them for now and when you have much more experience in a few years, come back and reconsider if this is really something you want to do still.

Quote:
the main problem is that its decay mainly consists of alphas, litle beta and very few gammas. So to make a battery by differentiating the beta and alpha fluxes would be very weak (I already tried using 4 americium pellets without seeing any voltage)


I suspect the problem was NOT that you need beta particles. You can make an atomic battery with alpha particles just fine, the beta's are not going to make much of a difference. Before starting this whole project of purifying the Ra, are you sure your battery design can even work even if you have Ra? From your description, it sounds like you are going for a direct charging capacitor-type of atomic battery. Am-241 would be suitable for that, and you don't need a point-like source. You can just use the discs. But the currents that atomic batteries like this produce are absolutely tiny, its hard to even be able to measure the voltage/current without a carefully designed measuring circuit. How did you measure your battery voltage?




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[*] posted on 3-10-2023 at 06:47


with a microamperometer, but I suspect the main problem, other than the low activity was having no vacuum and small neodium magnets.
First I was going to increase the activity and then the other two parameters.
Anyway, a powerfull source is the base of future iteractions of the design, I could even try using semiconductor junctions, energy recovery from spherical propagation and direct magnetic flux generation.
The problem is if I don't do it in the near future, not being any other chemical process that excites me rather than as accessory for a physics experiment or engineering build, I may not ever get into chemistry. So I would do this in a few years with about the same chemical expertise, but maybe with less time.
So I appreciate your concern, but I will continue gathering informations until I am ready to start the mockup extraction.
Thank you profoundly however for all the tips and warnings.


[Edited on 3-10-2023 by Telyron]

[Edited on 3-10-2023 by Telyron]
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[*] posted on 5-10-2023 at 10:40


Dont be disappointed by results. Even if you manage to extract most of your Ra. Eg 1Ci of Ra-226 gives around 0.01uA of current... So for 10uCi its 0.1pA - hardly measurable by common meters.
Heart pacemakers with TEG battery contained between 3 and 8 Ci of Pu. And without hard gamma of radium....

[Edited on 5-10-2023 by Cezium]
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[*] posted on 6-10-2023 at 00:42


I too think that learning by doing is an excellent way to learn.
I also agree that you have chosen a VERY challenging first project.
Not that you could not do it,
but there are many skills and lots of knowledge that you should acquire first.
... Assuming that you value safety.

Some things I've learned;
Contamination spreads much more than I expected.
eg I strongly recommend that you try something simple like carefully adding a small ammount of potassium permanganate to water in a test tube.
Then spray/mist some water over your work area, hands etc.
And/or make up a small quantity of silver nitrate solution, then go expose your hands to sunshine for a few minutes.

I know that if you are willing to learn, and take advice, you can gain enough skill and knowledge to either complete your project - or modify or abandon this project.

Some members (like me) take risks that would make professional chemists run away screaming,
Others are incredibly over cautious.
Good luck




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[*] posted on 6-10-2023 at 00:52


This is not a project I would consider for even a second.
Clock hands that still glow faintly in my element collection is as close as I ever want to get to radium.

I do however recommend reading The Radium Girls by Kate Moore. I am not suggesting that your propsal has anything like the same risk profile as what these women were doing. But it us a great read, helps you appreciate the history of the watch hands you now possess, and lends a great deal of perspective to the hazards of radiochemistry.

As others gave suggested, there is no downside to shelving the project for a few years and learning some skills.
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[*] posted on 29-12-2023 at 09:34


If anyone is thinking of doing something like this, do a practice run with denatonium benzoate as your radium. You’ll be surprised how much it gets everywhere .



“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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