Sciencemadness Discussion Board

Radioisotope Identification

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neptunium - 19-9-2013 at 19:23

I recently acquired a gamma/x ray spectrometer and I was curious to find out if anyone would pay to get samples analyzed for radio isotopes ?

the charge would be minimal (like 15 bucks) and you would have to ship the sample to be measured .

no high activity samples and no short isotopes...

let me know maybe I`ll start a business and quie this stupid job....

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: changed subject by request]

[Edited on 17.12.13 by bfesser]

bfesser - 19-9-2013 at 19:25

If you're located in the contiguous United States, I'd be interested.

neptunium - 19-9-2013 at 19:26

Detroit MI

neptunium - 20-9-2013 at 15:44

alright let me calibrate it , try it all and explore all the features and I will post pictures and results
Thanks Bfesser

neptunium - 26-9-2013 at 07:50

I have been messing with my spectrometer and this is my first spectrum for Am 241, its pretty amazing how it picks up all the x rays at low energy!
I still need to play with it and figure out why it wont capture higher energy (sensitivity issue I think)
but this is just a first test!


PMCA2-tmp.bmp - 949kB

neptunium - 26-9-2013 at 09:27

I changed the detector and plugged in a scintillation probe
and tried Co60 ...

this is what I obtained



co60 scintillation 2.bmp - 949kB

neptunium - 6-10-2013 at 09:49

made some improvement with the optical coupling between the photomultiplier and received a much bigger NaI(Tl) crystal

here is 10 minutes of acquisition with 2 pound of potassium hydroxide overlay with 10 minutes of blank background

if you look carefully there is a peak as expected in the 1460 Mev area ...
that's natural radioactivity !



compare K40.bmp - 949kB

neptunium - 6-10-2013 at 10:05

here isa a much better photopeak at 1170 Mev with Cobalt 60...



improved Co60.bmp - 949kB

bfesser - 6-10-2013 at 15:28

I only have a very basic understanding on how to interpret these spectra, but I think they're really cool, nonetheless! I find the <a href="https://en.wikipedia.org/wiki/Potassium-40" target="_blank"><sup>40</sup>K</a> <img src="../scipics/_wiki.png" /> spectrum to be particularly interesting. Thank you for sharing these, and please don't hesitate to post more. [edit] Is there any chance you could upload full-resolution spectra somewhere? Does the software support exporting to PDF or the like? Also, I'd like to know a little bit more about the instrument itself, perhaps even see a few photos.

[Edited on 6.10.13 by bfesser]

neptunium - 6-10-2013 at 18:40

sure . the detectors are a cadmium telluride semi conductor for the x rays from Amptek

http://www.amptek.com/xr100cdt.html

it may support pdf format I don't know I`ll check it out.
and an older model (though still very functional !) ADMCA multi channel analyzer 8000 channel

http://www.amptek.com/mcasoft.html

and a NaI(Tl) scintillation crystal from a Bicron 1.5M2.25/1.5L couple with a Hamamatsu photomultiplier running at 1500 Volts.
with a power supply Keithley 247 high voltage supply .

10061322192.jpg - 91kB


I am probably going to up grade to a 3inches crystal detector soon and maybe a cryogenic germanium detector later....


10061322112.jpg - 76kB

entire set up

10061322132.jpg - 80kB

semi conductor x rays detector

[Edited on 7-10-2013 by neptunium]

[Edited on 7-10-2013 by neptunium]

neptunium - 7-10-2013 at 10:02

here is Ba133 .... pretty powerful stuff! and increadibly accurate!!



ba133.bmp - 1.3MB

neptunium - 15-10-2013 at 09:43

i set it up for x ray spectroscopy/diffraction...



setup.bmp - 834kB


I first did a naked spectrum of the x ray tube at 40 kV ...
its too bad I cant see the K shell electron typical peaks I was expected! but I only have a 40 000 Volt generator!



x rays max 40kv.bmp - 949kB


judging by the amount of x rays coming out of this thing I don't think I am going to do these analysis very often!
also , not too many people interested although I thought this was a great analytical way for unknown elements and even isotopes!

I`ll continue to post every so often we ll see...

[Edited on 16-10-2013 by neptunium]

bfesser - 16-10-2013 at 07:22

I'm still very interested, and am enjoying these updates. I have some mineral specimens that I'd very much like analysed, but I'm too poor at the moment.

neptunium - 16-10-2013 at 10:01

i am still tweaking with everything but I enjoy it a great deal! I wouldn't charge anyone for some analysis!
U2U me for more details ..

bfesser - 16-10-2013 at 10:17

Quote: Originally posted by neptunium  
the charge would be minimal (like 15 bucks) and you would have to ship the sample to be measured
Regardless, I'm too poor for even the shipping, at the moment. When I find a job, I'll send a few specimens. I'm especially curious to see if my <a href="http://en.wikipedia.org/wiki/Trinitite" target="_blank">Trinitite</a> <img src="../scipics/_wiki.png" /> generates an interesting gamma spectrum (if any). It's only weakly radioactive (by <a href="viewthread.php?tid=25882">my Geiger counter</a>;), so I'd suspect it would require a rather long sampling time and a decent amount of shielding from background. I'm a little surprised that nobody else has shown interest.

[Edited on 20.10.13 by bfesser]

neptunium - 16-10-2013 at 10:46

yes a lot of young guys.....gotta start somewhere!

I am sure your trinitite will give a nice spectrum ! I don't have any trinitite so its exciting to see what it holds!
anyway , hope you get a job soon ! I know how it sucks !let me know

because of its origin (plutonium bomb) and its age (1945) it contains mostly Cs137 and some heavy elements which means that you own a few unreacted atoms of plutonium and some fission elements isotope born in a nuclear runaway chain reaction ....I don't think it gets any cooler than that!!

[Edited on 17-10-2013 by neptunium]

neptunium - 16-10-2013 at 16:22

that's a cool little Geiger counter you got! radiation detection equipment used to be so much cheaper before the Fukushima plant disaster in 2011..
ebay still has a few opportunities if you are lucky enough...

vulture - 27-10-2013 at 16:17

http://www.wired.com/wiredscience/2008/10/video-the-scotc/

What's the "range" of this thing? Could you detect x-rays from lightning?

watson.fawkes - 27-10-2013 at 16:48

Quote: Originally posted by vulture  
What's the "range" of this thing? Could you detect x-rays from lightning?
The video shows using old-style dental X-ray film as a detector to show that their little machine is indeed generating X-rays. As an X-ray detector, emulsion film is ordinarily limited to photograms, a kind of shadow photography. These are camera-less images, which is good for X-rays, because X-ray imaging optics are, let us say, not inexpensive. If you want to get X-ray images of remote objects, such as lightning, you'll need an optical train.

vulture - 28-10-2013 at 01:51

Quote:

If you want to get X-ray images of remote objects, such as lightning, you'll need an optical train.


I don't want images, it just would be cool to be able to detect those x-rays. The link with the scotch tape was another fun thing to try with his detector.

watson.fawkes - 28-10-2013 at 06:35

Quote: Originally posted by vulture  
I don't want images, it just would be cool to be able to detect those x-rays.
Film has good spatial resolution, but very poor temporal resolution and not-so-great dynamic range. If you want to detect x-rays with film, mask off half of it with lead bricks, and put it near the launch pad of a lightning rocket under a thunderstorm; it's about the only way you'll possibly get enough exposure. Dental X-ray film never came with storage instructions to keep it in a lead cabinet in case of thunderstorm, for example.

Scintillation detectors, though, have both lower detection limits and good temporal resolution. That's a much more fruitful route for an amateur to be able to detect some signal of any type.

Also, see this: Lightning Captured by X-Ray Camera—A First. The camera has 30 pixels and weighs 3/4 ton.

neptunium - 12-11-2013 at 19:43

x rays from lightning sounds interesting but incredibly difficult to set up!
here is what I do with 40Kv !





airfreshnerX.bmp - 108kBhandX2 - Copy.bmp - 108kBmeterX_C.bmp - 428kB

neptunium - 16-12-2013 at 14:09

can this be moved to a poll ? or no?

radioactivity testing

neptunium - 16-12-2013 at 14:26

would anyone be interested in some radio isotopes identification ?
no high activity (>10uCi) and no short half lives isotopes.

I didn't use the poll option the last time but you can check out
a few spectrum in the market study poll segment
also I am about to receive and work on a high purity germanium detector and its supply of LN2...




[Edited on 16-12-2013 by neptunium]

phlogiston - 16-12-2013 at 15:29

Probably, neutron activation analysis would be tremendously useful to many experimenters here, since, as amateurs, we tend to improvise when sourcing materials and thus often have to resort to poorly characterised chemicals (which has been the source of countless problems and unexpected results).

Is that something you can do as well? And if so, what neutron sources do you have at your disposal/sensitivity can you reach?

[Edited on 16-12-2013 by phlogiston]

neptunium - 16-12-2013 at 17:13

no I do not own a neutron source , but I was considering building an alpha linear accelerator with a thin Be sheet I have..
the sensitivity ? let me put it this way, the sodium iodide crystals let me detect K40 in a pound of potassium hydroxide
the Cadmium Telluride diode lets me pick up the x rays from a cathode ray tube instantly, and the High purity Germanium detector I just order (if it works) would let me see through a complicated spectrum of multiple isotopes.
the sensitivity is not the problem. with enough time I could pick out a few thousand atoms (or less) given they are all radioactive.


here is an (old) source of Cobalt 60 with the NaI(Tl) crystal


improved Co60.bmp - 949kB

the two peaks are clearly separated and visible

here is ba133 with the CdTe detector



ba133.bmp - 1.3MB

and this is Americium 241...

PMCA2-tmp.bmp - 949kB

I will post more when I get the HPGe detector and some liquid nitrogen


let me be clear, I cannot detect molecules or stable isotopes and a neutron activation would depend on the cross section of the element you are trying to activate .
also some isotope generated by neutron activation have a really short half life and cannot be shipped for analysis nothing would be left to detect!

only long lived isotopes (T/2>about 10 hours) can be successfully detected.

[Edited on 17-12-2013 by neptunium]

bfesser - 16-12-2013 at 17:35

Quote: Originally posted by neptunium  
can this be moved to a poll ? or no?
Yes. Done.

hyfalcon - 16-12-2013 at 18:44

I've got an unknown metal alloy that has stumped me on the wet analysis. I would love to have you take a look at a sample.

neptunium - 16-12-2013 at 22:26

sure! if I can activate it that should be no problem! u2u me I`ll tell you where to send it...
please understand that I travel a lot for work and might not be able to perform the analysis for some times.
hope your not in a hurry!

DJF90 - 17-12-2013 at 01:40

I think this is really cool but I don't think you'll get the exposure you deserve due to the thread title. Change it to "Anyone interested in radioisotope analysis" or the like and I'm sure you'll improve your audience greatly. It might even be more suitable to move this to "Chemistry in General", as topics in Misc quite often don't get the attention they deserve.

bfesser - 17-12-2013 at 05:58

This isn't a Chemistry topic. I agree with changing the title, though. <strong>neptunium</strong>, just let me know.

neptunium - 17-12-2013 at 06:09

yes I was trying to change it to radio isotopes identification, but couldn't figure out how to do it!
and it should have been in technochemistry maybe?

sorry I `ll be more careful next time .

Marvin - 17-12-2013 at 08:50

I'm concerned by the hand image and the lack of shielding around the bare X-ray tube. Is that a film exposure or a fluoroscope? Have you calculated exposure?

neptunium - 17-12-2013 at 11:00

I am not using it as a XRF I was just testing the detector response...it would be too dangerous to run it naked like the picture! yes I have calculated the exposure...that's why I stopped!
Beside the tube heats up a lot and wouldn't function very long anyway..
So NO X ray spectroscopy ! sorry


[Edited on 17-12-2013 by neptunium]

neptunium - 25-12-2013 at 17:50

....gonna do some neutron activation soon though! :)

neptunium - 29-12-2013 at 16:37

i got this 0.5mCi of Po210 on ebay so i made a poor man`s neutron source to see if i could activate this sample of mystery metal sent by hyfalco and this is what i got...


compare.bmp - 1.2MB

this is only about 30 minutes of exposure in a neutron oven... the 809Kev peak of the Po210 is clearly visible ,
however the area highlighted before that in the ROI (Region Of Interest) is particulary interesting...
arround 400 to 600 Kev is where the radio isotope of the mystery metal lay...
i am going to let it sit over night and see if anything else shows up on the gamma spectrum...

note
the red area is a background radiation without anything in front of the detector, the spectrum overlay on the background lets us appreciate the difference between the two spectrums and allows us to see minute amount of radiations..

neptunium - 30-12-2013 at 14:17

i ran the analysis again with the x ray detector and i think the sample must contain Ta (tantalum)
the stable isotope is Ta181 and after neutron activation we should expect to find Ta182.
although the activity is barely above the background radiations, most of the expected gamma and X rays are present !
this is not to say that ta is the only element in the sample but rather the most neutron sensitive (higher cross section).
here is the x ray spectrum compare with the background.



compare x.bmp - 1.3MB

i know it might not look like much but its pretty hard to mess up the calibration on this detector so i remain confident that Ta is present.
i dont know where the sample came from but Ta is often use in alloys because of its chemical stability 9corrosion resistant ) so it doesnt really suprise me .
what does suprise me is that i was able to detect it ! this is a very powerful and non destructive method of analysis and i find it mind blowing!

bfesser - 30-12-2013 at 14:30

Very cool. If you want, I can supply you with an FTP account to upload full resolution images (>800px). It would make it much easier for us to see what's going on in these spectra. Just U2U me if you're interested.

neptunium - 30-12-2013 at 14:54

yes the resolution is sort of crapy but we can kinda tell the energy scale at wich peaks occurs ...
again this is a very powerful non destrutive analytical way of determining elements presence. every chemist on here should be all over this!!!

[Edited on 30-12-2013 by neptunium]

bfesser - 3-1-2014 at 15:45

neptunium (or anyone interested), I found these <a href="http://www.ebay.com/itm/Hamamatsu-X-Ray-Phosphor-Screen-With-Fiber-Optic-New-/131069478644" target="_blank">phosphor screens</a> <img src="../scipics/_ext.png" /> while searching for PIN photodiodes to use in <a href="viewthread.php?tid=25882&page=3#pid313842">&gamma;-ray detection</a>, and thought you might find them useful for amateur X-ray imaging applications. The seller claims they're also somewhat sensitive to &beta;. [edit] Check out their other mad science type items, I see some nice stuff.

[Edited on 3.1.14 by bfesser]

neptunium - 3-1-2014 at 20:58

interesting indeed... i used a similar screen for the x rays (previous pictures)
some of them glow green others blue ... but the amount of radiation needed for the glow to be visible is colosal.
alpha particles can be viewed with a weak source (few micro curies) on a spintariscope if you let your eyes adapt to the darkness..
i would love to know what type of phosphor he uses, although no spectroscopy can be done with a scintillator this thin, for 30 bucks i might give it a shot!

[Edited on 4-1-2014 by neptunium]

neptunium - 29-1-2014 at 21:35

got a new bigger detector !!!!! this a a harshaw "well type" so 360 degrees detection for more accurate sample analysis !


new dec.jpg - 33kB

I did a quick 15 minutes background ( black line ) followed by a 15 minutes of 2 lbs potassium hydroxide ...

k40 resised.jpg - 73kB

don't let the size and resolution of the picture fool you this is natural radioactivity very visible! no doubt about the 1460Kev peak !

bfesser - 30-1-2014 at 05:51

Very nice. I'm not familiar with what a Harshaw "well type" detector is. Does this put a size limitation on the sample dimensions (does the sample need to fit inside a well in the detector)?

neptunium - 30-1-2014 at 07:20

you got it ! It may sound like a restriction but you gain on activity measurement (detect faster ) since the sample is "inside " the scintillation material.
However it works just as well with a bigger sample like the 2lbs jar of KOH just sitting on top of the detector. Harshaw is just the brand name like Bicron or canberra

bfesser - 30-1-2014 at 08:07

I see. I did look up the Harshaw name, and found a site for old employees of the company, but not much on the detectors. What are the well dimensions of your new detector?

neptunium - 30-1-2014 at 10:41

the number on the detector are 12SW12-w4 the hole is about 2 in deep and 3/4 in wide
these little glass bottle are a perfect fit.


0130041335.jpg - 73kB

neptunium - 30-1-2014 at 10:53

check out this beautifull well defined Co60! the materialisation peak at 511Kev is clearly visible!

<a href="http://www.scimad.org/users/neptunium/Co60.jpg"><img src="http://www.scimad.org/users/neptunium/Co60.jpg" width="200"></a>

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: hosted image(s) at scimad.org/scipics2/]

[Edited on 2.2.14 by bfesser]

neptunium - 31-1-2014 at 10:51

been playing with this data analysis software fitzpeak to look at my spectrum and it seems like a powerful tool!
here is the report after calibration andanalysis


Attachment: Main Report.txt (3kB)
This file has been downloaded 1250 times
and here is the detail spectrum
Untitled 2.bmp - 911kB

neptunium - 1-2-2014 at 16:10

for the one or two interested i am boiling off snow (yes it snowed again) because i read snow is a good filter
for atmospheric dust including radio active nuclide!

so when i have enough boilled off i 'll run an analysis to see what kind of radio pollutant i could find!...
stay tuned for updates! soon....

bfesser - 1-2-2014 at 16:19

Interesting. The graphs you're posting are difficult if not impossible to interpret, due to the images having been resized. Please look into a better way of posting images. (I've explained several methods in previous topics, and think I even sent you a U2U with FTP account information.) At the very least, email copies of the full resolution images to me, and I can upload them and edit them into your posts, on your behalf.

neptunium - 2-2-2014 at 08:24

being snowed in i collected some outside and melted it add some more melted it etc...
after collecting about a gallon of water i boilled it down to about 300 ml and pour 50ml in a small glass bottle that fit the dector...
started the acquisition and went to bed.
after 5 hours of collection this what i had.

<a href="http://www.scimad.org/users/neptunium/5_h_snow.jpg"><img src="http://www.scimad.org/users/neptunium/5_h_snow.jpg" width="200"></a>

i thought that little hump was Cs137 at 661Kev from the Fukushima accident (hlf life 30 years) but no .
the software indidcated I131 and Bi214 .
i am not sure what it is actually but its definitely there.
the other peak left little doubt iT IS K40...
but i found it interesting because not too many element have a peak at 632Kev...

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: hosted image(s) at scimad.org/scipics2/]

[Edited on 2.2.14 by bfesser]

bfesser - 2-2-2014 at 08:34

Quote: Originally posted by neptunium  
after collecting about a gallon of water i boilled it down to about 300 ml and pour 50ml in a small glass bottle that fit the dector...
Did you acquire a baseline on the empty bottle?

neptunium - 2-2-2014 at 08:43

yes i did but it should have been 5 hours too to be accurate and i only did 1 hour...

<a href="http://www.scimad.org/users/neptunium/1_hour_blank.jpg"><img src="http://www.scimad.org/users/neptunium/1_hour_blank.jpg" width="200"></a>

the K40 is barely visible because i was not standing there . in this basement (my lab) the main source of K40 is me !
i will get some lead shielding as soon as i get some money again!
whatever is in there is drowned in background radiations...

[Edited on 2-2-2014 by neptunium]

<!-- bfesser_edit_tag -->[<a href="u2u.php?action=send&username=bfesser">bfesser</a>: hosted image(s) at scimad.org/scipics2/]

[Edited on 2.2.14 by bfesser]

neptunium - 12-6-2014 at 18:27

what hapen to the charts?? does my browser needs updates ? or is everything gone ?

Metacelsus - 13-6-2014 at 06:33

I can't see them.

neptunium - 5-8-2014 at 05:31

i have a new detector much more performant with a better resolution,
i`d like to post graph as updates but i dont know what happened to the older ones....

neptunium - 20-8-2014 at 09:25

i recently acquired some modest quantities of the mineral called monazite . A source of rare earth and Thorium...
The gamma spectrum with my new improved detector clearly shows the isotopes from the decay chain of Th232



monazite 50.bmp - 561kB

after calibration the main peak is label as U235 or Ra226 wich doesnt really matter because if one is present we can deduce it either came from the other or the other must be there too .. also identified are isotopes of Pb, Bi, and Ac!
Also i have a small amoun of Euxenite ..


euxenite50.bmp - 561kB
notice how the same peak appear on both spectrum indicating the presence of the same isotope..i beleive it to be Bismuth
i will redo the calibration with more care to be sure ...
but i find it quite interesting that U235 is clearly present in both rocks in much greater amont in Euxenite though
i have enough to seperate uranium ,Thorium and other element chemicaly but probably wont do it .;)
although it would be interesting to see how the spectrum changes...


[Edited on 20-8-2014 by neptunium]

neptunium - 21-8-2014 at 07:54

the previous spectrum of Co60 was somehow erased..
this is what my new detector resolution is able to accomplish!


cobalt6050.bmp - 561kB
the two main peak at 1173.24Kev and 1332.5 kev are clearly seperated the small one over at 2.5Mev is just an addition peak.
The lower energy peak is the back scattering ( i need to built a shield)
and here is Barium 133 ...


Ba13350.bmp - 561kB
i get a much better resolution with the semiconductor detector but the surface area window being so small, it barely see higher energy gamma...it is in fact an Xray sopectrometer.

neptunium - 21-8-2014 at 13:44


here is the identification of a sample of euxenite...
euxenite ID.bmp - 2.2MB

neptunium - 22-8-2014 at 13:27

here is monazite


interestingly enough, Ra223 is a daughter of U235 with a half life of 11 days whereas Pb212 come from Th232 wich is more likely since this is monazite...but with a half life of only 10 hours ... my calibration might need an update!

monazite.bmp - 3.6MB

The Volatile Chemist - 14-9-2014 at 15:13

You should post some of your spectra as a reference on the sciencemadness wiki! They would be very useful.

neptunium - 15-9-2014 at 05:28

great idea! thanks Volatile.!

The Volatile Chemist - 15-9-2014 at 13:48

Sure!I'm thinking about getting the equip. for this within the next few years.

neptunium - 16-9-2014 at 07:16

from personal experience the most important piece is the detector. if you go with a cheap one you wont get the resolution regardless if you go semi conductor or scintillator.
after that there is plenty of amplifier counter and software (free) to get a good clean signal processed.
good luck and have fun! i know it is for me!

neptunium - 8-8-2015 at 10:48

I have order a steel shield inside of what i have melted some lead for the detector...
it cost me way more than i thought it would and left a bitter taste in my mouth.....untill

resized well.jpg - 680kB

I am not finished with the lead melting process (over 200lbs is involve) the whole set up is looking a lot better than before .



resized lab.jpg - 814kB


and i had some interesting results with a substance i would never have suspected to contain any active material..
Zirconium dioxide
here is the gamma spectrum of about 2 lbs of ZrO2.



zirconium oxide.bmp - 2.9MB

after careful calibration i was able to identify the natural element involve in the weak radio activity of this otherwise neutral substance...





zirconium oxide spectrum.jpg - 296kB
click on the picture for better viewing.
I am running an X-ray spectrum right now but the detector being way more sensitive and much smaller this will take a while .Each peak will be a lot more defined but it only reads the spectrum untill about 330Kev ...so more results to come.


i beleive the chemical similarity of group 4 with the lanthanides (and actinides) allows some of those metals to be present in each other ore...
it would be interesting to see if they could be detected in Titanium and Hafnium salt as well...
we already know how Yttrium and some rare earth are often found with Thorium and vice versa..
maybe Zirconium is a big part of the impurities in Uranium processing..



[Edited on 8-8-2015 by neptunium]

annaandherdad - 8-8-2015 at 13:29

neptunium, this is very interesting! I did not know of the existence of this thread.

Where did you get your monazite?

I fear that your spectrometer is too costly for my budget, but I'd love to be able to play with such a thing.

neptunium - 8-8-2015 at 21:27

there is (was?)a guy on ebay selling it for cheap...
I acquire every pieces over the course of a year or 2 ... it was a long process but it paid off! some parts are cheaper than others thats true...

neptunium - 9-8-2015 at 12:18

Monazite is a Thorium rich ore but still contain small amount of Uranium, when Euxenite is clearly a Uranium rich mineral.
the gamma spectrum clearly confirmed the presense of both Th and U and the decay chain of each isotopes and also quantify
those metals ..
here is the 2 spectrums for comparaison


monbazite euxenite compare 2.bmp - 2.2MB

careysub - 9-8-2015 at 12:50

Quote: Originally posted by neptunium  
there is (was?)a guy on ebay selling it for cheap...
I acquire every pieces over the course of a year or 2 ... it was a long process but it paid off! some parts are cheaper than others thats true...


I just bought 1 lb of monazite ore for $21 on eBay $15/lb plus $6 shipping), it was sourced to New Mexico.

If any SM members live in North Carolina there is a river that is a good source of monazite sand, much easier than gold panning. Unlike the ore (perhaps), monazite sand is usually concentrated monazite. I am sure monazite sand would find willing buyers here.

neptunium - 9-8-2015 at 19:29

yeah!.........you should send me a sample!

Texium - 9-8-2015 at 19:39

Quote: Originally posted by careysub  
Quote: Originally posted by neptunium  
there is (was?)a guy on ebay selling it for cheap...
I acquire every pieces over the course of a year or 2 ... it was a long process but it paid off! some parts are cheaper than others thats true...


I just bought 1 lb of monazite ore for $21 on eBay $15/lb plus $6 shipping), it was sourced to New Mexico.

If any SM members live in North Carolina there is a river that is a good source of monazite sand, much easier than gold panning. Unlike the ore (perhaps), monazite sand is usually concentrated monazite. I am sure monazite sand would find willing buyers here.
I've taken a look at that area of NC too. It looks very promising indeed. I know that there's a couple of members who live within a few hours of there. I mentioned it to them once in the Skype group a while back, but didn't discuss it a whole lot. I'll bring it up again and see if they're interested in it. I'd definitely like to get a sample too.

annaandherdad - 9-8-2015 at 19:52

Hi, careysub, I just bought 1lb of that monazite, too. It was a good deal.

A while back I spent a lot of time thinking about thorium, and I looked for monazite. There was none available, so now it's surprising to see it. I did find some thorium nitrate reagent, and bought a small amount.

To tell you the truth, I hesitated to buy the monazite, since I'm not sure I'll use it for anything and the radon is a concern. Also, some day someone will have to dispose of it. Actually it was the radon which caught my interest in the first place, since it has a dramatic effect in a cloud chamber (this is the radon in the thorium decay chain, not the one in the uranium chain).

But something tells me it's going to get harder and harder to get things like this, so I decided to take it.

careysub - 10-8-2015 at 14:35

Quote: Originally posted by annaandherdad  
Hi, careysub, I just bought 1lb of that monazite, too. It was a good deal.

A while back I spent a lot of time thinking about thorium, and I looked for monazite. There was none available, so now it's surprising to see it. I did find some thorium nitrate reagent, and bought a small amount.

...
But something tells me it's going to get harder and harder to get things like this, so I decided to take it.


You got that right. The seller tells me that the monazite deposit has been assayed with microprobe technology at 7-9.5%. This is by far the cheapest source of thorium I have seen in the couple of years I have been looking.

Here are some papers on this monazite source:
https://nmgs.nmt.edu/publications/guidebooks/downloads/62/62...

http://geoinfo.nmt.edu/publications/periodicals/nmg/10/n2/nm...

http://deepblue.lib.umich.edu/bitstream/handle/2027.42/32413...

http://pubs.usgs.gov/sir/2010/5220/downloads/SIR10-5220.pdf

Keep your monazite in an airtight box (or outside, it is after all, a rock). The radon risk is nothing to sneeze, but you simply need to have proper storage. The risk from thorium radon is much less that with uranium due to the very short half-life (55 seconds) but thorium ore often contains uranium as well. The Petaca monazites apparently always have less than 1% U however.


[Edited on 10-8-2015 by careysub]

neptunium - 1-10-2015 at 07:05

here is for your consideration Radium 226 (old Radium dial...)
some daughter of Ra226 are visible (nevermind the cursor on Tl)
giving Radium`s half life this should be interesting ...
the scale at the bottom has been calibrated.

radium 226.bmp - 2.9MB

[Edited on 1-10-2015 by neptunium]

The Volatile Chemist - 5-10-2015 at 12:27

Very nice work! I live in Ohio, perhaps eventually a trip to NC would be fun.

careysub - 5-10-2015 at 18:25

BTW - melting lead for a detector shield seems like wasted effort. Why not just pour in lead shot?

Random sphere packing density is about 0.64, so you would need to increase the volume of the shield by about 50%, the final density would be about 7.26, if you used plaster to fill in the space and make it a solid block, the density would increase to 7.66. Vibrating the lead might increase the density somewhat by causing it to settle.

neptunium - 6-10-2015 at 08:23

ahem I think you got the wrong page budd...

careysub - 6-10-2015 at 10:32

Quote: Originally posted by neptunium  
ahem I think you got the wrong page budd...


If directed to me: do I not read on this thread:
"I have order a steel shield inside of what i have melted some lead for the detector... it cost me way more than i thought it would and left a bitter taste in my mouth.
...

I am not finished with the lead melting process (over 200lbs is involve) the whole set up is looking a lot better than before ."
?

neptunium - 7-10-2015 at 01:21

my apologies Careysub I don't know what I was thinking....
Yes the lead shots seems like a good idea... I have already started with the melting and its almost done .
WalMart has this stainless steel container thick enough to melt lead in on an open flame or electric stove.
i should have thought of that .... in the future.

neptunium - 11-12-2015 at 08:34

just received a sample of Coffinite U(SiO4) the Actinium is way up in this one ! but the 3 peaks for Uranium and Radium are clear.
Also, notice the Pb210 at 46Kev...

coffinite.bmp - 2.9MB

IrC - 12-12-2015 at 02:47

neptunium have you ever tried this software? If so how does it compare to software such as the program you are using.

http://sourceforge.net/projects/opengamma/

I find what you are experimenting with to be very interesting but I admit I have never accumulated the equipment and software to actually do it. So I am thinking about building such a device but I have a question. Do you have to look at the energy peaks and then compare to tables of various gamma emitters to identify the element or isotope or does your software have graphs which indicate this (built in tables)? I notice in the image you posted it merely shows the peaks and energy levels.

http://www.amptek.com/products/gamma-rad5-gamma-ray-detectio...

grad_b.png - 13kB

As example in this graph from their page one would not know merely by looking at the image what materials were shown without the inclusion to the graph stating UO2, 133 Ba, Th (lantern mantle). When you are operating your equipment is there a feature where identification is given or as I asked do you have to compare your energy readings to charts? I am seriously thinking it is time I had such capability but I need to learn more in order to build it and pick the right software. Buying a commercially made setup is beyond my budget for mere experimenting where no money return is anticipated, to me this is more of a fun addition to a life long hobby. I noticed the window in the image you posted showing Ac-228 but am unsure if this is called up automatically (auto ID function). I downloaded all their software just to install and study the program operation assuming it will run minus the specific model detectors they indicate. I noticed their page indicates the software only functions with their devices.

While I intend to build my equipment I find it helpful to first study what others have done, have you looked at the following:

http://beeresearch.com.au/

https://www.youtube.com/watch?v=xPeKkzhf2TU



[Edited on 12-12-2015 by IrC]

phlogiston - 12-12-2015 at 03:19

Once equilibrium has been reached, which should be the case in a mineral sample, shouldn't the ratios of isotopes be always the same?
Or are you comparing it to the levels of U-decay chain isotopes? Ie. is your sample's Th/U ratio higher than typical for this mineral?

[Edited on 12-12-2015 by phlogiston]

neptunium - 12-12-2015 at 12:39

Irc,
Yes the equipment was rather expansive despite already being obsolete .
but it gets the job done !
the pocket MCA i have only runs with that particular software . i am not computer skilled enough to reprogram it or even built some adaptor hardware.
so the software is free and works well with the hardware.
Any other software would have to accept the format in which the spectrum is saved to be able to display it.

The detector i used are both temperature sensitive (not by much) but require a calibration everyday.
i use a known source of CO60 with its 2 main peak at known value to calibrate the spectrometer.
once you have the position of 2 or 3 peaks the scale readjust itself according to the energy input you`ve provided during calibration.
now you are ready for an unknown sample.
peaks will slowly rise (depending on the activity you can time the length of acquisition ex: 30 000 count total over 1 minute over 500 bq depending on source geometry dead time etc...you get the idea)
The software come with a series of library (in analysis from the top main panel)
a few isotopes were pre installed so when a peak is at a known energy level that matches one in the library , the software flag it for you with the little window you saw...
i also have 2 enormous book with every known isotopes and the energy of each gamma, x rays, beta and alpha, down to 0.00% probability.
there is a great software you can also download free
http://rad-decay.software.informer.com/4.0/
sorry lost the direct link.

once you`ve eliminated the very short lived like Fr and At, the very unlikely like Cm, or the truely exotic one its a lot simpler.
keep in mind that the NaI detector is very good at simple identification but with all the possible isotopes out there it is sometimes difficult or impossible to identify one with certainty. also the lower the energy the higher the imprecision .

its fun to find K40 in your ashtray i think, or monitoring the radioactivity of grass and dirt!

Phlogiston,
No i think its a pretty standart piece of rock to be honest! its not higher or lower than any other ore U and Th are usually mined from.
a lot of isotopes will show on my spectrometer , it doesnt mean the ratio is off or it contain more or less of anything,
you are correct when you said the ratio reaches an equilibrium after a while, unless you start seperating each element, it will stay that way.




IrC - 12-12-2015 at 14:50

Thanks I will look into that software you linked. I have had a detector in my storage for years that I never toyed with due to no access to LN2. In my small town UFO's would be easier to locate and no doubt any source is a few hundred miles away. However it looks like your setup does not need it so I am wondering how well my detector would function without the cooling. It states 3KV for operating voltage on the tag but I cannot find specific listing of it on the Canberra site. It is a GC 520 Standard Electrode Coaxial Ge Detector (SEGe) with a 7935-2 portable cryostat. I have no other equipment originally designed for it so obviously some reverse engineering of the internal circuitry and building my own circuitry is needed. All I have is the detector itself seen in the pics. As you can see in the end view pic there is a fitting for LN2 in and another for a vent. The PDF I found on their site does not mention my specific detector as it is old and no doubt the company is little interested in it. I have yet to find a search function on the site.

Canberra1.JPG - 103kB Canberra2.JPG - 72kB

Attachment: SEGe-detectors-C40021.pdf (179kB)
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What do you think of operating this detector removed from the cryostat, using it as part of a new design. How important is the cooling to LN2 temperatures for the kind of work as you are doing, is there any chance of harming the detector running it at room temperature. Possibly I can come up with some type of Peltier electrical cooling for it although cryonic temperatures would not be reached.

The Volatile Chemist - 12-12-2015 at 15:40

At the very least, looks cool and great :P
Would be cool to see it running if you had some LN.

neptunium - 12-12-2015 at 16:53

oh my god you do have the holy grail of gamma spectroscopy!!!!!!!!!!!!!!!!!!!!!!!!
DO NOT under ANY circumstances operate this detector without cooling you`ll fry it !
please tell me you have not !!!
what you have in your possession is the ultimate detector my friend!
it will (with liquid nitrogen) detect AND identify ANY and EVERY isotopes known!
the Germanium semi conductor WILL totally fry if you try to run it without its cooling .
please oh god PLEASE tell me you have NOT tried it yet ?

neptunium - 12-12-2015 at 16:54

is this the one for sale on ebay for like 5000 ?

neptunium - 12-12-2015 at 16:56

This detector requires liquid nitrogen and a preamplifier and an amplifier before the MCA
i think there is a gamma ultima from canberra capable of running it on ebay right now!

IrC - 12-12-2015 at 17:08

No it is not on ebay, I've never even considered it before. Seldom been taken out of my storage, every few years I will look at it, search for data until I give up, think about taking it apart to draw out all the circuitry and connections since with no data I will never be able to use it. Simply must have a circuit diagram or the original equipment designed to go with it. No never powered, put in storage and never used. Every few years I think about reverse engineering it then consider it may be damaged if I try and it is just too perfect to risk. So I put it away hoping someday to find the information so I can study it fully. What is it that would fail if powered at temperatures above LN2? So far I have never found detailed information on its internal construction, other than what Canberra shows for newer models. Do not worry I have no intention of doing anything that would harm it, the very reason I have simply stored it forever.

Just read your post fully and so it is the Ge detector that would be damaged. Which indicates it must be very similar in design to what I see for newer models. For a long time I thought it might be a PM type circuit with a hyperpure Ge crystal on the end but studying newer models it appears the Ge is itself connected to the 3KV. So what you say makes sense. But not to worry I am good at what I do in electronics and would never connect voltages blindly to several connectors without understanding the circuit complete and having knowledge about the device itself. Which is why its lived in storage so long. I had considered the cooling was about noise not protection. Are you saying the Ge cylinder would avalanche under voltage unless a minimum temperature is reached? Explains why the label stating do not operate until cooling has been going for 4 hours is on it.


[Edited on 12-13-2015 by IrC]

neptunium - 12-12-2015 at 19:46

the semi conductor which is a tiny rectangle inside the cylinder, operates on the displacement of electron within the matrix , when a gamma ray hits it, a bunch of electron (proportional in number according to the incident energy of the gamma) a series of electrons and holes appear within the matrix and the electrons move to the anode and the holes move to the cathodes, generating a small current proportional to the incident gamma. thus the signal is very sensitive .
the downside is that the detector size and density are both low enough to be inefficient when compare to a scintillation detector but the upside is that the signal is very accurate and represent the gamma energy very faithfully .
when used without cooling ,the Ge matrix is vibrating and the high voltage generate a wide current that destroys the arrangement of Germanium atom within the matrix permanently. once it has been powered without cooling, it can never be operated again.

IrC - 12-12-2015 at 20:05

Interesting. After reading your concerns I did a little searching and found this:

https://en.wikipedia.org/wiki/Semiconductor_detector

"The major drawback of germanium detectors is that they must be cooled to liquid nitrogen temperatures to produce spectroscopic data. At higher temperatures, the electrons can easily cross the band gap in the crystal and reach the conduction band, where they are free to respond to the electric field, producing too much electrical noise to be useful as a spectrometer. Cooling to liquid nitrogen temperature (77 K) reduces thermal excitations of valence electrons so that only a gamma ray interaction can give an electron the energy necessary to cross the band gap and reach the conduction band. Cooling with liquid nitrogen is inconvenient, as the detector requires hours to cool down to operating temperature before it can be used, and cannot be allowed to warm up during use. Ge(Li) crystals could never be allowed to warm up, as the lithium would drift out of the crystal, ruining the detector. HPGe detectors can be allowed to warm up to room temperature when not in use."

Which indicates the type most easily damaged when warm is Ge(Li), where the Li migrates such that it cannot even be stored when not in use at room temperature since the Li will still migrate. However mine is not the Li type so I lucked out there I have stored this thing for years unused. Appears it can handle that just fine but when powered we are back to the scenario you just mentioned. Sadly that means all I can do is store it I am never going to easily obtain LN2 around here and I have no intention of trying anything that can harm, its simply too valuable. Back to my PM NaI/Tl project I guess. You said it is a tiny rectangle but the specs I find at Canberra all indicate it is much larger. Look at the pic at the top in HPGe_alt.pdf, this is what the Ge detector looks like, fairly large.

Attachment: HPGe_alt.pdf (662kB)
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http://www.canberra.com/products/detectors/germanium-detecto...

Another example, not a tiny X but much larger and cylindrical.

Attachment: SEGe-detectors-C40021.pdf (179kB)
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[Edited on 12-13-2015 by IrC]

neptunium - 15-12-2015 at 16:50

Yes its a real pain...but for the classic Germanium semi conductor detector As long as you don't apply high voltage at room temperature you should be fine.
Some device called a cryocooler are sometimes available on ebay. The word got out a few years ago (when they were selling for 200 bucks ) that one may generate liquid nitrogen with one of these device .and now its difficult to get one under 500 dollars.
Anyway . by simply bringing the cold part of a cryocooler directly in contact with the cooling can inside the LN2 dewar, it should be possible to use without LN2.
Indeed, one would have to be careful and thermally isolate the 2 part and another power supply had to be brought in for the cryocooler, which has to be cooled itself (air or water cooling) and as always wait long enough for the detector to reach its operating temperature.
I thought about doing it for a while. .

IrC - 16-12-2015 at 15:31

I looked at prices for coolers, grand range or higher. Combine that with a grand for the cheapest used preamp, no access to LN2 here, thinking I really should just put it on fleabay. Pointless to just store it forever, will never have it running. Maybe I can just buy another NaI/Tl crystal and finish my project which came to a halt when I kept getting bad NOS mica window tubes. Never got a reply on my restoring crystal questions and I have seen decent ones for what they want to restore the one I have. If nothing else getting a good one frees me up to try my hand at fixing the old one for another PM tube. Those I have several of as well as the plastic scintillators but personally the plastic scintillators are crap compared with NaI/Tl which will detect Gamma in the range of 130 Kev to 1.3 Mev. The plastic may be good enough standing at ground zero but not very useful for high sensitivity. I have several of those of varying types. Not impressed at all compared to my old but still working Precision 111B and Mount Sopris SC129. These I converted with inverters to operate on 4 C cells to replace three Hg filament batteries, a 22.5 and two 67.5 volt batteries.

Another circuit which works well for the PM tube:

Attachment: scintillation_probe.pdf (99kB)
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neptunium - 16-12-2015 at 16:57

I agree that's the choice I went with when I put my set up together. Unless you can get LN2 delivery every so often why bother?
NaI crystals can have impressive resolutions . mine is an old one as well 3"x3", which is plenty.
The only problem is the fragility if it gets banged up during transport or dropped . cracks could appear within the crystal and ruin it permanently.
I have heard of LaBr3 as a better, denser and faster detector then sodium iodide but that have not found their way to ebay and the after market yet. Also I have a very small non hygroscopic and very dense (perhaps better) BGO (Bi4Ge3O12) but it's so small I cannot do anything with it.
CsI are good but still pretty expensive.
As of today, if its not open or cracked, and as a home scientist/experimenter, I think you can't go wrong with the NaI.


IrC - 18-12-2015 at 14:09

If you have time and it does not burn up too much of it can you post an in depth (hands on to the home amateur if you will) description of how you do what you are doing in this thread? Along the lines of the way Peach used to do write-ups showing all equipment, assembly and operation also covering the software and performing measurements. Over time of course as you can. I ask because reading dry texts is not as helpful as one would wish. Always they assume a great amount of knowledge and experience on the part of the reader. Never do they cover the subject in a way that would guide a home builder. Also useful would be ways to calibrate the instrument for persons who do not have calibrated sources like your Co60. Say some kind of OTC like smoke detector hacking or lantern mantle Th or maybe some ore sample such as is seen on fleabay often.

neptunium - 18-12-2015 at 16:11

Sure Its no problem. I am not home right now but as soon as I get back for the holidays I will put together the schematic with description and pictures .I was actually looking at a website I could build and forward here.
I have the same problem with some descriptions I totally understand what you mean.
Give me a few days

neptunium - 26-12-2015 at 22:48

as requested here is a break down of the equipment i use to produce the gamma spectrum of various radioactive compounds..
first the detector


NaI detector.JPG - 314kB
this one is a sodium iodide thallium doped scintillation detector, its 3 inches by 3 inches it has two BNC connectors (not pictured)
one for the high voltage DC power supply


high voltage power supply.JPG - 326kB
and one for the amplifier .
it doesnt matter what type of high voltage and amplifier you are using as long as its a DC HV and is very stable and the amplifier is rated for gamma or X rays spectroscopy.
I found that NIM BIN are very affordable ,easy to assemble ,very versatile and very rugged .


amplifier.JPG - 336kB
here you can see (above) a rate meter that produces a live display of the activity of the sample placed in the detector.


MCA.JPG - 781kB
next is the most important and expansive part of the spectroscopy system.
the Multi Channel Analyzer or MCA.
it turns the signal out of the amplifier into a digital, readable signal for the computer to display a spectrum, it only reads voltage NOT energy, the calibration must be done to reflect on the energy scale.
for that i use a known source of Co60 (availlable to anybody without a license) for about $75 from spectrum techniques/
Cobalt 60 has 2 very visible peaks at 1172Kev and 1332 kev respectfully


first calib.bmp - 2.9MB
knowing that , the software allows a calibration and by telling it where those two peaks are , the program readjust the scale to match the energy level corresponding to the energy of the known peaks.



calib2.bmp - 2.9MB
now we are ready to place a sample of unknown origin and by knowing the energy at which each peaks will show up we can determine the radioisotope responsible for it.
this next sample is a concentrated of thorium ore.
the software has a bank of energy peak already uploaded in its database so we can move the cursor on the spectrum where the peaks are and it will automatically match it with a peak in its records.
if not, there is plenty of books, data sheets, software, the internet, etc.. to look for the energy level of any peaks found on the spectrum.


thorim sep.bmp - 2.9MB
here the 63.3 Kev line matches the Thorium234 energy line.
there is always a certain level of uncertainty (as in science in general) and the detector is not precise enough to seperate very closed peaks (within about 15Kev) but it is good enough for a reasonable estimate of the radio nucleide involved.
it is precise and sensitive enough to detect potassium 40 in ashes or even bananas, the spectrums can be saved and compare to others which allows to determine with accuracy the presence (or absence ) of Radium228 in pottery and dirt.
but it only detect gamma rays with energy between 50Kev and 3000kev, which is where most radio gamma emitters are.

IrC - 27-12-2015 at 02:25

Very nice. I keep forgetting to ask you but do you know of a way sans the LN2 and other equipment to test the Canberra to be sure it is working? Got it as surplus from a lab that had closed down.

neptunium - 27-12-2015 at 08:41

nope! the only way would be to use a cryocooler or an helium cryo pump, this detectors MUST be cooled

IrC - 27-12-2015 at 12:44

I thought so as well but still have the number for the person who ran the maintenance dept. for all equipment in the lab. Said it was as pristine as a model that age can get, was never run without all safeguards in place and never allowed to get near even the highest safe temperature. Was still in perfect condition the lab merely ran out of grant money and cutbacks ended hope for new grants. They sold surplus all equipment to cover debts to contractors. What sucks is he said all the other pieces to the system were in a different lot that sold way below cost. I could have had it all but during those years I was not familiar with this detector and never bothered looking at the amplifiers. Far too expensive now so I guess I will consider ebay.

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