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Telyron
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Radium extraction from watch hands
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.
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Sir_Gawain
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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.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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j_sum1
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Thread Moved
29-9-2023 at 15:18 |
violet sin
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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
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phlogiston
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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.
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"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer |
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Telyron
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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).
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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]
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Telyron
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| 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
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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.
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Telyron
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| 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?
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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]
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Sir_Gawain
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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.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Telyron
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| 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.
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Sir_Gawain
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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?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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violet sin
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"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...
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Sir_Gawain
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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.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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violet sin
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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.
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Sir_Gawain
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Would nitric acid dissolve radium sulfate? I thought it was pretty insoluble.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Telyron
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| 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.
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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.
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phlogiston
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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]
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"If a rocket goes up, who cares where it comes down, that's not my concern said Wernher von Braun" - Tom Lehrer |
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Sir_Gawain
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| Quote: Originally posted by phlogiston |
| 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] |
Huh. I guess you can't believe everything you read online. Who knew?
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Sir_Gawain
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| Quote: Originally posted by phlogiston |
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.
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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.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Telyron
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| 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]
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Telyron
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| Quote: Originally posted by Sir_Gawain |
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. |
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.
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Tsjerk
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| 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?
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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]
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Sir_Gawain
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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.
“Alchemy is trying to turn things yellow; chemistry is trying to avoid things turning yellow.” -Tom deP.
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Telyron
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| Quote: Originally posted by Tsjerk | | 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] |
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?
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Telyron
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| 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.
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Tsjerk
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| Quote: Originally posted by Telyron |
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? |
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]
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