radioman123 - 2-4-2022 at 11:25
Hello!
I have recently been having problems with my uranium extraction. I followed Carl Willis's page
https://carlwillis.wordpress.com/2008/02/20/uranium-chemistr...
but when I get the carbonate leach step, everything falls apart. The liquid is neutralized, then the CO2 is boiled out, but when I add H2O2 (3%)
nothing happens. I am told a yellow precipitate should form, but the solution just stays exactly the same. I tried adding ammonia solution to
re-precipitate the uranium, but the liquid just darkens. What am I doing wrong? Could the ore be an issue? It is from New Mexico.
Thanks!
radioman123
[Edited on 4-2-2022 by radioman123]
unionised - 2-4-2022 at 11:53
Was the uranium solution "the right colour"?
radioman123 - 2-4-2022 at 11:57
The solution was not green when I extracted it, it was yellow. After adding acid to neutralize it, it was almost clear. Not sure if this is a problem,
but I am beginning to suspect it is.
unionised - 2-4-2022 at 12:14
This may be a stupid question but was the rock radioactive?
radioman123 - 2-4-2022 at 12:17
Yeah, it was radioactive. I bought it from a mineral dealer and it looks like carnotite.
unionised - 3-4-2022 at 03:34
I guess you don' have access to lots of test kit.
But the borax bead test is a good way to track where uranium is.
The green fluorescence under UV is hard to miss.
radioman123 - 3-4-2022 at 05:26
I do know of that test, so I'll try it. Thanks!
violet sin - 3-4-2022 at 13:02
Out of curiosity, Grant's New Mexico, from Rockhound_Steve? Think he uses a Ludlum 2200 rate meter/scaler with 44-9 pancake probe.
how hot was it described as?
What did they test it with?
Do you have means to test it your self?
Rough size in grams?
..................................................................
I've a pile of rocks but no chem or extraction done, as it's impractical, unsafe, highly frowned upon in my workspace. But I'm reading the website you
linked.
How fine was your ore crushed?
What's your oxidant during acid leach step? Bleach like the article?
-if step one leaching doesn't come out right color, you may not have much in sol. to move on with? Shortcuts in crushing/processing or reagents can
limit returns. He has the bolded statement "Acids will only extract significant uranium if it is in the U(VI) oxidation state"
----------------Beginning of carbonate leach step----------------------
HCl Acid leach( green sol) + ammonia ==>[pH 5 - ppt. yellow]==>[pH 10]==> ppt. green/brown,
(decant/wash/settle x 3-5 times) keep ppt. for carbonate leaching.
(Ammonia Ppt. from 2l of acid sol.) + (Baking soda/washing soda @ pH 10.5) + heat + time = yellow pregnant solution.
Preggers sol is acidified to pH 3/boiled ^CO2 gas
27% H2O2 added to sol.= ppt
guess the pH drops and requires adjustment w/ carbonate leach sol back to 3.5 pH ==> final yellow uranyl peroxide.
---------------------------------------------------------------------------------
With that break down, it seems like you might never have gotten it(much) in solution from the material, it might have needed more oxidation. Then
your peroxide for dropping yellow oxide should use high strength not 3% at the end of it.
I'd check into upgrading your oxidant inventory and see if you can get better results. Be sure to have good fine ground material, check pH at various
points in the process and see if your on track.
..,..........................................................
Do you have lab notes on how it went and what you did? Compare to the page and make sure your not just trying to drop uranyl peroxide straight from
the acid leach sol. with weak 3% H2O2
I like it when people do the fun stuff that interests me, I can spectate without all the cleanup headaches my self. I'll stay tuned, to see what you
turn up. Photos encouraged 
Thanks for sharing, and hope this helps.
Violet sin
BTW, last night I spent several hours measuring rocks last night with 3 meters and a couple different moderators to keep the sample I range. One
side was bottoming out my pancake probe. Super rough comparisons because of flawed spatial orientation of the various detectors. Finished up like 4
am with a page of notes and some super boring vid of frustrated attempts at manipulating things hahaha.
A uraninite/tyuyamunite sample rated at 118k cpm by Rockhound_Steve on hottest side. Black side is much less hot, not rated by him.
Conclusion my GQ GMC320+(v4) may have counting issues? With high output sources up close, seems to jack WAY up some times if introduced too rapidly.
Radiacode-101 only sees ~3x on hot side vs. weak side. And approximate results have to be determined with the pancake probe b/c it was full range and
I had no repeatable standoff setup to keep it in range besides cardboard/plastic poster board (thanks arkoma, a versatile material indeed). More to
do before anything can be discerned
radioman123 - 3-4-2022 at 15:22
Thanks for the pointers! Yeah I did buy the rocks from him. I have a simple CDV700 for testing, and it was maybe 100-300 grams. I think I will
definitely try more concentrated peroxide. I did not crush the ore finely at all, since I was doing a test run. I will try in a few days (school/stuff
going on) on a little larger scale with the concentrated peroxide and better crushing methods. I did use bleach but I might try some nitric acid, too.
I think you are right, I barely extracted any uranium at all, since the radiation level was barely above background! I think it was a low-grade rock
anyway, maybe 1500 cpm at most on my pancake probe.
Cheers,
radioman123
[Edited on 4-3-2022 by radioman123]