Sciencemadness Discussion Board

Dissolving Radium and Friends

IrC - 20-3-2006 at 23:13

Ok, so this question is lameass enough and I probably asked about it before so that it belongs in beginnings but what the hell it sounds like technochem to me. Besides, I perfected my YAG Laser nearly popping out my eye and don't have all the caps yet for my squisher so I needed some other mad science thing to do, prompting me to return to an old project.

I have all these radium watch hands and I want to dissolve the compounds off of them but not affect the steel hands nor have any Fe in with the result (by this I mean I don't care what happens to them I just don't want some acid or other that dissolves the Fe adding another item to be chemically seperated from the Radium). H2O is out, they rust! As near as I can find online the old hands were made from a glue, Radium bromide, and Zinc Sulphide. The radium may be some other salt I don't know but the Bromide was all I could find mentioned, and of course the ZnS is a given. I want the Radium by itself, if in salt form hopefully one easy enough to safely reduce to metal (or at least a useful salt that can be kilned without giving off war gasses or some other dipshit chemical). I have tried many chemicals in the form of organic solvents but I always end up having radiaoactive acetone or something, I just want the glue in solution, the ZnS somewhere else, and the Radium salt by itself. Possible?

Does anyone really know the true mix of ingredients in the old watch hands? Is the ZnS activated meaning likely I also have to deal with Ag or something like it? All I get on the net is useless information. As to the Fe yes I scraped the stuff out of many hands in earlier experiments, but it is impossible to do so without breathing in dust and even micro amounts here is likely very bad, prompting me to eliminate this step by dissolving the paint rather than scraping it. Even in acetone it takes weeks to months to dissolve and for some reason certain hands don't, meaning likely a different glue?

I must glow in the dark to feel alive!

Chris The Great - 20-3-2006 at 23:46

Try something like methylene chloride for the glue, I find it dissolves plastics much better than acetone, so you might have better luck. Chloroform would also work well. Once you do that, filter out the powder which will be the radium and other chemicals as they are probably insoluble in methylene chloride or chloroform. Dissolve it in water, radium bromide is soluble while the rest (zinc sulfide, Ag etc) shouldn't be. Then precipitate it, for example with NaOH to get the hydroxide (or maybe oxide).

Also, wouldn't a concentrated solution of radium bromide glow blue? That would be the coolest looking thing ever and it might be worth it to just stop at that point and have a glowing blue liquid in your lab.

From the CRC handbook, radium bromide, chloride, iodide and nitrate are soluble, while the sulfate and carbonate are not. I would presume the oxide to also be insoluble as well as the hydroxide.

Hope this helps, and if you do succeed TAKE PICTURES. Radioactive glow is one of the coolest looking things IMO.

BromicAcid - 21-3-2006 at 08:16

Being that the glue is an older type of glue there is a good chance that it is a water soluble glue (the kind made of hooves or wheat) rather then the organic soluble types normally used today. As such I go with water as your solvent of choice, just degass it first by bringing it to a boil so that you remove out the dissolved oxygen and try to reflux your watch hands in it without acess to the air, without oxygen your water shouldn't attack the iron too badly and if that's the case you'll either end up with a slightly gummy solution from the dissolved glue, or in the best case you'll just extract out the radium bromide which could then be crystalized. Not sure where you would go from there though, boiling down would seem to give a sticky paste.

12AX7 - 21-3-2006 at 13:10

How much radium is in there, would you guesstimate? Nanocurie? 1 Ci = 1g Ra so that's less than a fly's testicle. I honestly don't know how you can hope to process that little, even with thousands of glow-paint objects. Strontium and Barium hydroxides are relatively soluble so Ra(OH)2 is probably quite soluble as well, even in microliter quantities of H2O. Carbonate and sulfate, for that matter, are probably also noticably soluble when dealing with so little!

Tim

IrC - 21-3-2006 at 14:33

I really don't know but the activity is higher than any other source I have. I am sure I don't need more than microscale amounts at this activity level, as what I am after is alpha particles to smack into Be pieces to make neutrons. Every other source of alpha I can find has el-crappo for activity, and since IIRC I get something like one to thirty neutrons for every million alphas (shows how long I shelved this project, I used to remember the number!), I really do need a better alpha source than what I have been able to find. It is quite simply almost impossible to get any alpha source worth a nickel. Smoke detectors don't have much of a chunk of Am 231 and it does not do much. Maybe if I had a zillion but ever since that dumbass kewl made so much news with his smoke detector pieces that source has gone down. No more can you call a company and get the emitters for free or for next to nothing.

I did like the idea of glowing blue stuff laying around also. Add that to a bunch of untrained neutrons floating around and I can be happy.

Nick F - 28-3-2006 at 19:34

Hey, I'm doing the same thing myself! Mainly because I want some radium, although if I can get enough for decent neutron production then that would also be cool. Also, if you have enough alphas you can induce short-lived radioactivity in aluminium, magnesium, boron etc which would be interesting.

A useful link: http://www.orau.org/ptp/collection/radioluminescent/radiolum...

"Quoting Ed Landa: "zinc sulfide was mixed with a radium salt to yield products containing about 25 to 300 ug [one ug is essentially the same as one uCi] of radium element per gram. The more concentrated preparations (generally containing 215 ug of radium per gram to meet British Admiralty standards) were used on aircraft and ship instrument dials, while lower-grade materials containing about 50 to 100 ug of radium per gram of mixture were used on watches, switch markings, and other devices requiring less critical reading." According to a Department of Commerce Information Circular from 1930, the paint might contain "from 0.7 to 3 and even 4 milligrams of radium element to 100 grams of zinc sulfide. Impurities may be added to the zinc sulfide as follows: Cadmium, 0.05 per cent; copper, 0.001 per cent; manganese, 0.0002 per cent."

Ra-226 has six alpha emitting daughters, so actual alpha activity is seven times higher than the uCi figures given for radium. Clearly military items are best. I might go round my local army surplus store with my geiger counter one day, they have lots of cool stuff and I'm sure they'll have various dials etc.

My plan was to collect a load of paint (I'm currently dissolving the paint off with acetone, and if it doesn't dissolve then I scrape it off under the acetone), let all the solvent evapourate, add nitric acid in the hope of converting the zinc sulphide into the water-soluble nitrate with liberation of hydrogen sulphide, and then adding sulphuric acid to ppte insoluble RaSO4. I think this should work fine, I might even do some preliminary tests soon. I'm not going to attempt to produce metallic radium; I think losses with such a small amount of material would make this much too wasteful.

Radium occurs in uranium at something like 0.2 ppm if I remember correctly (I'm pretty sure it's that order of magnitude, at least). I'm thinking that it shouldn't be too hard to get hold of a few kg of pitchblende if you live in the right area (I know places in Cornwall where you can pick up big chunks of it from the ground), I'm sure it wouldn't be too hard to extract a mg or so of radium. It'd certainly be fun (I think maybe I'm getting complacent about the dangers of radioactivity)!

If you just want alphas for neutron production, you might be interested in: http://www.2spi.com/catalog/photo/statmaster.shtml

500 uCi of polonium-210 for $36. It'll be cheaper than getting gram quantities of radium paint.

Marvin - 4-4-2006 at 09:14

Chemical neutron sources are a mugs game and any radium you adsorb is with you for life. Polonium decays quickly so its not suitable either.

If you want neutrons in impressive numbers get the amateur scientist CD-ROM, last time I looked it was quite cheep from Tinkers Guild, and build the electrostatic accelerator. Unlike anything you'd be able to make with paint, this will produce enough neutrons to make things detectibly radioactive. 10^7 n/sec from a van der graaf and some vacuum work.

atomicproject - 4-4-2006 at 17:57

I am in the process of building the 1971 Scientific American particle accelerator. Like earlier stated, its main use will be the production of neuts. This method is guranteed to produce a tremendously greater output than the Ra/Be method. Plus, as Marvin implied, the chemical extraction processes you are thinking of is extremely messy and ultra hazardous. These processes create radioactive steam, smoke and particulate emissions that cannot be avoided. Any accidential inhalation will surely cause problems in the comming years. Dont forget, one microscopic airborne alpha emitter from Ra or U(etc) can get permanently lodged in your lung. Day after day, year after year that one particle is bombarding the surrounding lung tissue with alphas and gammas. Cancer will eventually develop. NOW, that scenario is if you were lucky enough to inhale just one microscopic emitter..........

The accelerator option is cheaper, safer(can be shielded), and provides a wealth of knowledge that is gained during its construction.

Once mine is finished, I will post photos.

IrC - 11-4-2006 at 10:33

There is no neutron production article on the CD as far as I can find, merely accelerating charged particles. I suppose that puts me back to a low velocity source of protons but the alphas from radioactive sources would seem to be far better as a source since they are leaving the nucleus with great energy. I find that it would be hard to go from a source of protons to neutrons in any way using materials easy to obtain. So Marvin I ask, do you have any good ideas on how to take lithium metal and heavy water (I have both) and produce lithium deuteride (or hydride). I have looked at many pages of patents and other sources. Or do you think lithium hydroxide made simply by putting Li metal in water (only using deuterium oxide in this case), would make a decent target for neutron production or is it important to have the hydride (deuteride) instead. Also, what the hell do you call it when Li and D2O is used, lithium deutroxide?

Below is a decent link on accelerators which some may find useful:

http://www.lbl.gov/abc/wallchart/chapters/11/0.html

http://www.theradicalremnant.com/stuff/acc.zip

Was the above zip file the article you were talking about?

Marvin - 12-4-2006 at 07:53

There are 2 major accelerator projects, one for electrons, the other protons/deuterons. You should find the article in the zip file on the CD. Its missing a few gif units which makes a few bits nonsensical, but its the right one.

You do not want lithium deuteride as a target. Its too moisture sensitive and evolves hyfrogen when it heats up, destroying the accelerator vacuum. If you can get liquid nitrogen, there are a lot of shortcuts to high vacuum and you can use the better frozen D2O target. Otherwise I would suggest D2O + P2O5 as in the article.

For a 200kev deuteron beam of about 2ma you can get 10^9 n/second with d-d (about 400W of power). For a 10-20ua current from a small van der graaf 10^7 is feasable if the thing works (about 2 to 4W of power).

Aside from the health aspects of heavy beta and gamma emissions of radium based neutron sources, the short halflife of the polonium based ones, its simply not possible to get enough of the material for useful neutron production. Even 10^4 n/sec would require a massive amount of radioactive material. For a radium based source you are throwing out about 100'000 times as much gamma as neutrons, who would even trust those few counts on a detector as really neutrons?

In terms of danger the accelerator is not safe. Not by a long way, and the amount of neutrons you can make with fairly trivial amounts of power is enough to make detectable, even hot (for short periods) radioactive material, in addition to throwing out a fair amount of X rays and gamma (1:1 ish gamma:neutrons) while its switched on. It does deliver the goods though, you only need the sheilding when its on and when its turned off, it is off.

atomicproject - 12-4-2006 at 08:09

Shielding is fairly simple by employing a concrete sleeve to surround the accelerator tube. Very easy to do by using PVC tubing as the inner wall and a larger cylinder(possibly a concrete form) as the outer. Pour hi-test concrete between the cylinders and let dry. The accelerator tube will be placed in the center cylinder.

As far as neutron production, I was planning on using Beryllium as an alpha target.

atomicproject - 12-4-2006 at 08:15

Yes, that is the EXACT same article.

Also see this link for a quick view of an already built unit(note the lack of shielding).

http://www.paradigmenergy.us/accelerator.htm

Marvin - 12-4-2006 at 08:38

I thought about alpha+Be or alpha+B, but the voltages required become unfeasable. Its the additional charge on both nuclei, if you arnt in the multiple Mev range its just going to bounce. Somewhere in the lanl documents is a graph of n production crosssection versus alpha energy for beryllium.

kazaa81 - 24-4-2006 at 16:13

Here is some data from CRC Handbook of Chemistry and Physics 85th edition:

Radium
Ra
CAS #: 7440-14-4
Mol. 226 g/mol
Form: white metal, cubic
M.P. 700°C
Density 5 g/cm^3

Radium Bromide
RaBr2
CAS #: 10031-23-9
Mol. 386 g/mol
Form: white orthocline crystals
M.P. 728°C
Density 5.79 g/cm^3
Soluble 70.6^20 g in 100ml H2O
Soluble in EtOH

Radium Chloride
RaCl2
CAS #: 10025-66-8
Mol. 297 g/mol
Form: white orthocline crystals
M.P. 1000°C
Density 4.9 g/cm^3
Soluble 24.5^20 g in 100ml H2O
Soluble in EtOH

Radium Fluoride
RaF2
CAS #: 20610-49-5
Mol. 264 g/mol
Form: white cubic crystals
Density 6.7 g/cm^3

Radium Nitrate
Ra(NO3)2
CAS #: 10213-12-4
Mol. 350 g/mol
Form: crystals
Soluble 13.9 g in 100ml H2O

Radium Sulphate
RaSO4
CAS #: 7446-16-4
Mol. 322 g/mol
Form: white crystals
Insoluble in H2O, acids

IrC - 24-4-2006 at 20:35

Good info. I am not a chem guru so I have to ask, if it says soluble in ethyl alcohol, would it also be soluble in isopropyl alcohol? Or acetone, or would they have mentioned acetone?

The_Davster - 24-4-2006 at 20:39

It really depends on the chemical, but a safe bet would likely be; probably, just not as soluble.

Accelerator Ideas

jpsmith123 - 26-4-2006 at 19:20

Building a small electrostatic accelerator was once an interest of mine as well.

I accumulated some stuff for it, but I never got around to building it (actually I built the Van de Graff, and that was a fun toy, but not the accelerator tube).

Although I was primarily interested in accelerating electrons, I got some Pd/Ag alloy tubes, closed on one end, that I was going to try to use as a controlled leak to admit D2 or H2 into the tube to accelerate deuterons or protons.

I thought it might be possible to make the Pd/Ag tube the cathode of an electrolysis cell and then control the flow rate of hydrogen into the accelerator by controlling the electrolysis current.

For the construction of the tube, I was considering trying to solder the electrodes to the glass with indium, rather than using wax or epoxy.

Anyway, your project piqued my interest in accelerators again a little bit.

Last night I was fooling around with a 3D EM simulator and I decided to try to model the accelerator column as described.

I'm probably doing something wrong, as I'm relatively inexperienced with this software, but it looks like the focussing forces set up by the electrodes, as specified, may be insufficient to overcome beam space charge, even for relatively low current beams. IOW, you might not get efficient beam current throughput in the accelerator column.

I've attached some pictures. The first picture shows the layout, the second shows the E field, and the third shows what I think are some proton trajectories (although they may be some kind of representative positive macroparticle trajectories or something - I'm still trying to learn how this software works, especially the particle tracking solver).

To get the particles (the software allows electrons, protons, or user defined particles), I defined as an emission surface a small circular plane slightly embedded in the sphere.

The sphere is at about 500 kv while the plate at the other end is at ground.

I was going to try to use a slightly conductive material to set the potentials of the grading electrodes, but the electrostatic field solver unfortunately does not accomodate resistive materials, so I just specified the potentials of the electrodes for a uniform E-field.

If I get some time later I'm may try to parameterize some of the geometry and then vary things and see if it looks any better.

Quote:
Originally posted by atomicproject
I am in the process of building the 1971 Scientific American particle accelerator. Like earlier stated, its main use will be the production of neuts. This method is guranteed to produce a tremendously greater output than the Ra/Be method. Plus, as Marvin implied, the chemical extraction processes you are thinking of is extremely messy and ultra hazardous. These processes create radioactive steam, smoke and particulate emissions that cannot be avoided. Any accidential inhalation will surely cause problems in the comming years. Dont forget, one microscopic airborne alpha emitter from Ra or U(etc) can get permanently lodged in your lung. Day after day, year after year that one particle is bombarding the surrounding lung tissue with alphas and gammas. Cancer will eventually develop. NOW, that scenario is if you were lucky enough to inhale just one microscopic emitter..........

The accelerator option is cheaper, safer(can be shielded), and provides a wealth of knowledge that is gained during its construction.

Once mine is finished, I will post photos.


Attachment: Pictures.zip (127kB)
This file has been downloaded 818 times

Electric Potentials

jpsmith123 - 27-4-2006 at 20:10



Potentials_2D.JPG - 51kB

A Field Emission Cathode

jpsmith123 - 27-4-2006 at 20:21

If you want to accelerate electrons, without the hassle of putting the target inside the HV electrode, or without the hassle of putting batteries (for a filament supply) inside the HV electrode, a do-it-yourself field emission cathode might be a possibility.

Here's a paper describing what seems a fairly easy to make, robust, relatively high emission cathode material, using multiwall carbon nanotubes and epoxy. I'm thinking other materials like castable ceramic might work well also and have a lower vapor pressure than the epoxy.

Attachment: Zettl_1.pdf (99kB)
This file has been downloaded 1080 times

The_Davster - 20-7-2006 at 21:34

Figured this would be of interest to someone here, assuming it does contain radium:
http://cgi.ebay.ca/Watch-Clock-Oil-Grease-Solution-Radium-Se...

IrC - 26-7-2006 at 10:24

Waste of money! No trace of radioactivity of any kind. I can get better readings out of a bowl of vegetables. I thought about trying to get my money back as the guy is clearly using false advertising in his auction but I doubt he even is aware of it. Just a little bottle of ZnS activated glow in the dark paint and some bottles of oil. Which by the way I have several of now, anyone needing to do any precision machine work give me a jingle.

Thanks for the link Rogue, was worth a try anyway as hard as it is to find any radium anymore. Just posting this to save anyone else the expense.

pantone159 - 26-7-2006 at 13:03

I think most/all 'radium' paints have no radium in them. My guess is that they are just phosphor paints, intended to refresh old hands whose phosphor has gone bad. It is the phosphor that wears out, not the Ra-226. (Unless you are talking thousands of years.) So 'radium' means 'intended for watch hands containing radium', NOT 'contains radium itself'.

Theodore Gray has some comments about some completely dead 'radium' paint that he got:
http://www.theodoregray.com/PeriodicTable/Elements/088/index...

I should have chimed in with this when I saw rogue scientists' post, maybe I would have saved you (IrC) some money. My bad. :(

IrC - 26-7-2006 at 14:50

Actually not a big loss, the oils are extremely high quality. I am sure they will be useful somewhere as I fix many things, and if it is some activated ZnS this would be useful. Glows in dark well after shining a light on it, need to do some tests to determine what it really is. I should be able to moisten some and notice H2S as well as checking out its reaction to gamma in the dark.

The_Davster - 26-7-2006 at 20:26

My apologies, I see you even bought two sets.

IrC - 26-7-2006 at 21:13

It wasn't that expensive assuming this powder is some good silver activated ZnS. Was thinking about playing around with building a screen for scintillation.

I was wondering why the oils are so exotic unless they must be of ultra purity so as not to gum up precision watch mechanisms. If I ever get into designing nanotechnology maybe I can build them a small ocean with a low pollution content.

PacketStorm - 27-7-2006 at 05:55

IrC you mentioned detecting gamma with damp ZnS - does that work? I thought it only responded to alphas.

Also, I wanted to mention a good way (that I found at least) for making a pretty effective scintillation screen with powdered ZnS.

I took some clear packing tape, tapped out a very small pile of ZnS on it and smeared it around on the adhesive side until I had a very thin layer - just to the point where the tape lost its stickiness. Obviously you know that you must keep the layer extremely thin in order to see through from the other side (non sticky) and not absorb too many alphas on a frontal layer that is blocked from view.

Put your alpha source on the ZnS side and enjoy the show! Mine reacts quite well to an Am-241 source from a smoke detector. I've been wanting to get a microscope to view the scintillations - primarily to get a higher magnification and also to get my face and eyes away from the source when using the magnifying glass method. Am-241 gives off a fairly weak gamma, but I still don't like having my face down within 3" of it when looking at the scintallations. :o

IrC - 27-7-2006 at 06:48

No, I mentioned smelling damp ZnS, to see if it was ZnS by noticing the rotten eggs smell of H2S.

Oh yeah I forgot, there is a silver activation process that lets it detect gammas, which was also what I mentioned checking for.

Not likely what this stuff is though, it's probably just ordinary ZnS.





[Edited on 27-7-2006 by IrC]

PacketStorm - 27-7-2006 at 09:56

Quote:
Originally posted by IrC
No, I mentioned smelling damp ZnS, to see if it was ZnS by noticing the rotten eggs smell of H2S.

Oh yeah I forgot, there is a silver activation process that lets it detect gammas, which was also what I mentioned checking for.

Not likely what this stuff is though, it's probably just ordinary ZnS.


Gotcha - I re-read your post and I see now what you were saying.