Sciencemadness Discussion Board - Radium extraction from watch hands

Radium extraction from watch hands

Telyron - 29-9-2023 at 13:45

Hello, this is my first post.
I bought 300 watch hands with radioluminescent paint, I approximated an activity of 10uCi total, measuring only alfa and gamma with a LND7317 based detector, and I would like to turn them into a radium electroplating of a small metal disc.
I saw a couple of discussions on this topic, but none satisfied me with a definitive answer, so i figured I'd make a new one.
for those not familiar, radioluminescent paint is essentially a mixture of ZnS doped with copper, RaSO4 and some organic glue.
I wonder if once I have a method to try, if I could use some Strontium so that with a flame I can distinguish it very clearly from the copper in the Zns:Cu (the first one glows red while the second green) I know that Barium would be a better choice, but I dont know how I could verify its separation from ZnS:Cu giving very similar color flame.
for those about to write that is dangerous or illegal, where I live it is not illegal to do and when I am working with Radium I wear always gloves and a respirator with carbon filter, and have all windows opened with fans blowing Radon out.
I am not a native speaker nor a chemist so please don't save words for explanation thank you very much.

Sir_Gawain - 29-9-2023 at 14:59

Marie Curie's body is still so radioactive her coffin is lined with a thick layer of lead (to say nothing of her equipment and personal belongings). Point is, radium is not a good thing for amateurs to screw around with. Gloves and a respirator are not nearly enough protection. It's a cool project, except it will kill you in a few years.

violet sin - 29-9-2023 at 16:44

I don't get the flame color separation technique you're trying to go about. Are you meaning to reduce radium sulfate with elemental strontium? Using the flame test to determine endpoints?

I mean, your first step would be to separate the luminous paint from the hands .. and that's where I'd personally say "NOPE!! No thanks" because paint flakes of that nature scare the crap out of me. But if you're determined, build a glove box, do it in a water bath, something, anything to minimize the risk. Indoors with windows open and fans is NOT ideal, respirator or not. I mean it's a building, and I'd assume you've been in there before, and intend to go there again after your project ... with our a respirator.

Minimizing the processing with chems by elimination of the metal overburden of the hands means you can work smaller. Most the zinc sulfide has been beaten up by radium, and is useless, needs to be separated out. Have you any idea what that would leave you with quantity wise? How much radium do you suppose is total in there? How much has walked off with refuse, how many separate piles of radiological waste do you intend to dispose of?

I'm assuming it's a miniscule amount of active source. Calculate what you can, to see if it's feasible. Full separation that is. You'd have an easier time trying to plate out the copper and zinc.

Figure out of your Geiger counter is sensitive enough to see if you've ruined your building before making a forever mess

I'm sure there's some way to reuse the paint... It's just not for me, it's not really for an amateur and it can be really dangerous. Things seem easy on paper, real life is less direct

Think it through, stay safe

phlogiston - 30-9-2023 at 05:46

I think Telyron was planning to use the strontium to practice/test the procedure with. Sr chemistry is similar to that of Ra, and therefore most processes should work more or less the same. So, you could make a mock version of the paint with Sr instead of Ra and test your separation procedure with that. Once you are convinced it works (and verifying that is where the flame test comes in), you can do it on the real stuff.

To come back to Telyron's question: Whether you can use Sr depends mainly on two things:how similar does Sr behave in the steps you have in your separation procedure?
For instance, precipitation as a sulphate will probably work the same. But I am not sure conversion to carbonate by boiling in carbonate solution will work just as it will for Ba or Ra. Maybe it will, but I can't recall having read about that anywhere. You'll need to check for each step in your procedure.
The other thing is: For this to be a good test of your procedure, you'd want to use similar amounts of Sr as Ra, so in the microgram range. would you be able to detect microgram quantities of Sr with a flame test? I suspect that may be hard. Probably not a bad idea to test that first.

Telyron - 30-9-2023 at 07:32

Quote: Originally posted by Sir_Gawain

Marie Curie's body is still so radioactive her coffin is lined with a thick layer of lead (to say nothing of her equipment and personal belongings).

Marie Curie in her life, worked without any respiratory or protective equipment over 10 tons of pitchblende, which contains 80% Uranium oxides, and just 0.003% of radium, inhailing uranium dust is what killed her at the respectable age (for the time) of 66 years. She at last managed to have 1g of radium, if I am lucky I got 10 micrograms, so don't worry for my life.

[Edited on 30-9-2023 by Telyron]

Telyron - 30-9-2023 at 07:44

Quote: Originally posted by violet sin

I don't get the flame color separation technique you're trying to go about. Are you meaning to reduce radium sulfate with elemental strontium? Using the flame test to determine endpoints?

Have you any idea what that would leave you with quantity wise? How much radium do you suppose is total in there? How much has walked off with refuse, how many separate piles of radiological waste do you intend to dispose of?

I'm assuming it's a miniscule amount of active source. Calculate what you can, to see if it's feasible. Full separation that is. You'd have an easier time trying to plate out the copper and zinc.

Figure out of your Geiger counter is sensitive enough to see if you've ruined your building before making a forever mess

I will respond in order, the flame technique is exactly as phlogiston said, I want to replicate a mockup formula with brand new zinc sulfide and strontium or barium solphate in more quantities than what I have as radium, if it works for bigger quantities it will work for smaller too, and it's easier to detect (as phlogiston thrutfully said it's difficult to see a flame of few micrograms.)
You should know that a Curie is the activity of a gram of Radium, so having said I got 10 uCi means i got 10 micrograms.
my geiger counter has the most sensible probe commercially available, used by nrc personell to check contamination, and it shows the dust on my porch (that hasn't seen any radioactive source nearby) to be more radioactive than the desk i do experiments on, (after I clean it)so chill out.

Telyron - 30-9-2023 at 07:47

Quote: Originally posted by phlogiston

To come back to Telyron's question: Whether you can use Sr depends mainly on two things:how similar does Sr behave in the steps you have in your separation procedure?

The fact is that I don't have a procedure, I am asking for suggestions because I am no expert in this field... I am more prepared on radioactivity and engineering than chemistry.
I want to add that my end goal is building a radioisotope battery and for that I need all the beta emitting daughter nucleides of radium, so the procedure should be more focused on removing zinc sulfide doped copper, glue, rust and other contaminants, rather than getting only the radium solfate.

[Edited on 30-9-2023 by Telyron]

Sir_Gawain - 30-9-2023 at 07:56

This is not a good first chemistry project. How do you plan to deal with the waste and contaminated equipment? Also, I would not dream of attempting this in anything less than a sealed glovebox in a proper laboratory setting.

Telyron - 30-9-2023 at 08:15

Quote: Originally posted by Sir_Gawain

This is not a good first chemistry project. How do you plan to deal with the waste and contaminated equipment? Also, I would not dream of attempting this in anything less than a sealed glovebox in a proper laboratory setting.

I know, but we all got to start somewhere and this is what turns me on, I wouldn't have gotten into chemistry otherwise. The amounts of waste I am producing are undetectable, no increase in normal background radiation in dust taken up by a vacuum cleaner, even if I flushed it all down the toilet and it went straight to the water pad, it would be hardly noticeable look up the church rock uranium mill disaster, that is a environmental disaster 46 Curies of radioactive material, not 10 microCuries.
Anyway I am putting all towels I use to clean in plastic bags to take to a landfill, there is no other way.
I was planning on building a glove box, I could do it.

Sir_Gawain - 30-9-2023 at 08:19

I think your idea of practicing with other alkali earth metals is a very good one. It would give you an idea of the amount of radium contaminated waste you'd have to deal with. Is there any way you could use the unprocessed watch hands for the battery?

violet sin - 30-9-2023 at 09:03

"my geiger counter has the most sensible probe commercially available, used by nrc personell to check contamination, and it shows the dust on my porch (that hasn't seen any radioactive source nearby) to be more radioactive than the desk i do experiments on, (after I clean it)so chill out"

Ok then. LND7137 is a good detector, I had to refresh my memory on that number, as I had read it as a 712 when reading yesterday. And as we both know a LND -712 would NOT be the best choice. It's the smallest mica film alpha capable counter they make at LND.

As for calculating you've a few micrograms based off the activity you measure... Is that with all 300 watch hands facing he detector laid out flat .. or is that a haphazard measure of the near space to a bag of hands all laying this way and that? The sensors have conversion ratios for incoming vs. detected flux. If your machine isn't calibrated right, and stuff is laying about, that's not a great way to go about it. Just be aware of the shortcomings of quick assumptions.

A quick search approximates radium's activity as nearly 1,000,000 times that of uranium. So a very tiny amount of the former could cause an issue much larger than a measurable, visible amount of pure uraninite. Same goes for breathing it in. It's not to be waived off.

You think you could get a small, basically disposable, sonication bath for cleaning jewelry to worry off the paint from metal hands? Leave that thing running on a herd of your watch hands. Your first oder of operations is separation regardless of the following steps. Do that safely and confine your product/waste to manageable containers. I think that alone would ease the minds of those responding to your thread. I don't think anyone wants to just discredit your idea, but we sure encourage safety. Dare I say value it over a successful outcome 99% of the time.

Extractive chem is well documented. Look for their hard won information from the past.
https://babel.hathitrust.org/cgi/pt?id=uiuo.ark%3A%2F13960%2...

Sir_Gawain - 30-9-2023 at 09:11

Depending on what the watch hands are made of you might be able to dissolve them in nitric acid, leaving the radium sulfate behind. What you definitely don't want to do is scrape the paint off dry. The dust would get everywhere.

violet sin - 30-9-2023 at 09:36

Well, yeah, but in the book I linked above, one method uses nitric to start off the leaching process for radium. Wikipedia has radium nitrate solubility as 13.9 g/100 ml. You'd be better off leaving some stubborn parts of the paint on the hands, than dissolving the whole hands .. that just introduces way too much material to an already delicate amount of Ra.

The book has some good reading, and allows download as PDF. That was just one of MANY titles that popped up with a simple search. I highly recommend looking at what they offer there.

Sir_Gawain - 30-9-2023 at 09:45

Would nitric acid dissolve radium sulfate? I thought it was pretty insoluble.

Telyron - 30-9-2023 at 11:57

Quote: Originally posted by violet sin

As for calculating you've a few micrograms based off the activity you measure... Is that with all 300 watch hands facing he detector laid out flat .. or is that a haphazard measure of the near space to a bag of hands all laying this way and that? The sensors have conversion ratios for incoming vs. detected flux. If your machine isn't calibrated right, and stuff is laying about, that's not a great way to go about it. Just be aware of the shortcomings of quick assumptions.

I measured the hands in groups of 15 for tiny watch hands and singularly the bigger ones from alarm clocks, whole emission, then only beta and gamma with a plastic shield, then only gamma with a metal shied.
I then took the alpha and gamma counts and divided them by their respective 4pi efficiencies factors of the detector, sum it up and converted in Curies.
as I said it is the correct procedure, this estimate has an error of 20-35% maximum.
They already are in sealed leaded containers, don't worry.
the extraction document you linked I think is only available in the US I don't have a VPN yet, but I will look it up myself.
I want to wait to dissolve them anywhere until I have a clear procedure to undertake.

phlogiston - 30-9-2023 at 13:05

Quote: Originally posted by Sir_Gawain

Would nitric acid dissolve radium sulfate? I thought it was pretty insoluble.

No, it won't, but you can convert Ra sulphate to Ra carbonate by boiling extensively in concentrated sodium carbonate solution, and then dissolve that in nitric acid (or another acid), which was exactly how Marie Curie herself did it.

I guess one route might be to (1) separate the paint from the watch hands with an organic solvent that will dissolve the glue (2) boil the recovered paint (after evaporation of the solvent) in carbonate to convert the Ra to carbonate, (3) dissolve in hydrochloric acid to dissolve the Ra as chloride (4) filter (5) add sulphuric acid to the filtrate to predicate RaSO4.

I don't really know how to plate Ra onto a metal disc from there. I suspect that will actually be a very difficult thing to do. Is it really necessary for your end goal?

Quote:

if it works for bigger quantities it will work for smaller too

That is not necessarily true. When working with very, very small quantities as you would be, losses are much greater. It is all to easy to lose everything. Some techniques, like filtering, are not even possible in the same way as they are with larger quantities.
One way to make it easier is to add some barium as a 'carrier'. This will contaminate your Ra with Ba ofcourse, but it makes it much easier to work with precipitates etc, because at least you will have visible, macroscopic quantities to work with.

Quote:

Marie Curie's body is still so radioactive her coffin is lined with a thick layer of lead

This is a myth. Lead coffins were common at the time, it had nothing to do with radiation shielding. Her body was exhumed in 1995 and radiation measurements were performed. Her remains were only very slightly radioactive. Not at all detectable outside her coffin. You can read about it here:

https://sfrp.asso.fr/wp-content/uploads/2021/05/Exhumation-M...

[Edited on 30-9-2023 by phlogiston]

Sir_Gawain - 30-9-2023 at 16:04

Quote: Originally posted by phlogiston

Quote:

Marie Curie's body is still so radioactive her coffin is lined with a thick layer of lead

Huh. I guess you can't believe everything you read online. Who knew?

Sir_Gawain - 30-9-2023 at 16:47

Quote: Originally posted by phlogiston

Individually removing the paint from each hand (~300) sounds both tedious and messy. That's why I proposed removing everything else from the radium by dissolving in nitric acid. Hot nitric should remove the metal hands, glue and zinc sulfide. If the radium is to be used for a radioisotope battery, the resultant impure radium sulfate should work, correct? My main concern would be to limit the number of steps involved in order to decrease loss and the amount of contaminated equitment.

Telyron - 1-10-2023 at 00:39

Quote: Originally posted by phlogiston

I guess one route might be to (1) separate the paint from the watch hands with an organic solvent that will dissolve the glue (2) boil the recovered paint (after evaporation of the solvent) in carbonate to convert the Ra to carbonate, (3) dissolve in hydrochloric acid to dissolve the Ra as chloride (4) filter (5) add sulphuric acid to the filtrate to predicate RaSO4.

I don't really know how to plate Ra onto a metal disc from there. I suspect that will actually be a very difficult thing to do. Is it really necessary for your end goal?
[Edited on 30-9-2023 by phlogiston]

Thank you for the detailed route you proposed, but if I filter the solution how would I be able to remove the dissolved zinc sulfide and glue? or they just remain in the solution while I precipitate the radium to then being removed with a pipette...Would help using a centrifuge to precipitate radium sulfate at the end?
for adding some Barium sulfate to the mixture I don't know, if it is in big concentration would ruin my need for a punctiform source, maybe I could add a milligram without much problems... and while I am saying this I should add that I thought about electroplating because in order to use alpha particles to extract energy from the Radium, I need the source to be only 100 atoms thick or less (to minimize self absorption), and the only way I know of is electroplating... could anodic stripping mercury drop method work?

also I found this route in an older discussion:

"A separation sequence might be
o fusion with Na2CO3 and a nitrate, in a small platinum, silver, or nickel crucible
o Dissolve the fusion results in medium strength HCl or HNO3
o Adjust the pH, hit it with H2S to drop out Zn, Ni, and other such transition elements.
o Add a barium salt, and ppt the Ba+Ra as the sulfates."

I don't get a few things: what does fusion mean, thermal? (as in melt?)
how should I adjust the ph, with a common base? like NaOH)
Drop out means precipitate or dissolve?
Why does he say t to use a platinum silver or nickel crucible?
would this method work?

[Edited on 1-10-2023 by Telyron]

[Edited on 1-10-2023 by Telyron]

Telyron - 1-10-2023 at 00:45

Quote: Originally posted by Sir_Gawain

I don't know phlogiston might help in this, in the end I can't have any metal impurities however, cause then they would be electroplated too I think.
I could dissolve them all at once and keep the jar spinning to facilitate this process and then filter out the remaining solid watch hands with a strainer, to speed up the recovery.

Tsjerk - 1-10-2023 at 01:27

Quote: Originally posted by Telyron

I don't get a few things: what does fusion mean, thermal? (as in melt?)
how should I adjust the ph, with a common base? like NaOH)
Drop out means precipitate or dissolve?
Why does he say t to use a platinum silver or nickel crucible?
would this method work?

Really, if these are the questions you ask, please try this without radium first, a couple of times, before doing anything with. Better start with something a bit more elementary.

- Yes, fusion as in a melt.
- Adjusting pH up is generally done with a base, yes.
- Precipitate, it's already dissolved right?
- Imagine what happens with other kinds of crucibles when you melt a nitrate in them.
- probably when done correctly, but it seems you dont have any experience with chemistry, in that case; probably not.

[Edited on 1-10-2023 by Tsjerk]

Sir_Gawain - 1-10-2023 at 05:45

I'm pretty sure radium metal is way too reactive to electroplate in aqueous solution. Telyron, could you give us a diagram of the battery you plan to build? That might give us an idea of what could be substituted.

Telyron - 1-10-2023 at 10:03

Quote: Originally posted by Tsjerk

Quote: Originally posted by Telyron

Really, if these are the questions you ask, please try this without radium first, a couple of times, before doing anything with. Better start with something a bit more elementary.
- Yes, fusion as in a melt.
- Adjusting pH up is generally done with a base, yes.
- Precipitate, it's already dissolved right?
- Imagine what happens with other kinds of crucibles when you melt a nitrate in them.
- probably when done correctly, but it seems you dont have any experience with chemistry, in that case; probably not.
[Edited on 1-10-2023 by Tsjerk]

I plan on trying with Barium (or Strontium better) before doing anything, I don't want to risk 130€ of Radium.
I was insecure about melting cause I know that Radium has a melting point of 1200 degrees Celsius, maybe the sulfate fuses at lower temperatures.
I repeat that I am a non native speaker and its my first big chemistry project so I don't get all the things, but I think to have understood it all now.
Thank you.
what do you think about the two procedures phlogiston and this other user suggested? Is there a better one?

Telyron - 1-10-2023 at 10:05

Quote: Originally posted by Sir_Gawain

I'm pretty sure radium metal is way too reactive to electroplate in aqueous solution. Telyron, could you give us a diagram of the battery you plan to build? That might give us an idea of what could be substituted.

It is simply two halves of a metal tube inside another bigger tube where vacuum is applied, at one end I have the alfa and beta emitting source, with a magnetic field I deviate the particles (in opposite directions) and I should see a voltage across the two halves inside.

Tsjerk - 1-10-2023 at 10:13

Quote: Originally posted by Telyron

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]

violet sin - 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-

Attachment: rc000041.pdf (5.6MB)
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Attachment: ja02236a001.pdf (524kB)
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Telyron - 1-10-2023 at 12:17

Quote: Originally posted 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]

Tsjerk - 1-10-2023 at 12:32

How would you get sodium nitrate to 1500 degrees?

[Edited on 1-10-2023 by Tsjerk]

Telyron - 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...

phlogiston - 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]

Telyron - 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.

Telyron - 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...

phlogiston - 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?

Telyron - 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]

Cezium - 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]

Sulaiman - 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

j_sum1 - 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.

Sir_Gawain - 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 .