In this video I will be working with radioactive toxic heavy metals. I cannot possibly teach enough chemistry in a single youtube video for you guys to do this safely on your own. You're gonna have to go into it knowing a lot of chemistry if you want to recreate anything that I do here. Even I probably could have been a lot more safe. That said I think this video will be the longest on my channel for the year. It's jam-packed with information and I'm sure you guys will learn lots. So grab a snack settle in and enjoy. Hi, everyone! welcome back to cody's lab. So ever since my video on my, box of radioactive materials people have been asking me to refine some uranium ore into uranium metal, and today I'm finally going to do it. So this is a chunk of uranium ore from Colorado. You see with my Geiger counter here it is rather radioactive. As you can see we're approaching 30,000 counts per minute and this geiger counter only picks up the beta and gamma rays that come off of this rock so it is rather radioactive and there's a lot of uranium here. You can actually see the pitchblende, the black uranium oxide in the rock. It's in a sandstone matrix. Let's see if I can, uh, get some uranium metal out of it. So the first thing I need to do is grind to this rock up into a fine powder to give it as much surface area as possible and expose the uranium. Since I'm just doing a small 460 gram sample I'm gonna be using my hand crusher here. This is basically a pestle and mortar except I'm using an axle and a pipe cap, as my pestle and mortar. Now the dust from this is not exactly good to breathe so I am doing this outside on a breezy day. I'm staying upwind and I have designed this crusher so as to minimize the dust leakage. I'm also wearing a dust mask. The radiation that I'm working with here is really not a problem unless you ingest it, hence my precautions from breathing it in. Alright, so I'm just gonna keep crushing, nice and slow to minimize dust I might actually grind like this a little bit... So here's the crushed ore, still reading about 30,000 counts per minute. Now some of my patreons, did ask, why I didn't crush the or wet, you know, to keep the dust from getting up into the air. The answer to that is, well, it's a lot harder to crush things that aren't completely dry. You could go all the way to making a slurry and crushing like that, but then you got splashing problems. Anyway, this is still not as fine as I'd like. The particle size is still not small enough to expose all of the uranium grains and so I will be transferring this into a ball mill. This is actually a rock tumbler, but... Basically the same thing. All right there we go. There's our crushed ore. Now, to this I'm going to add some of these chrome steel balls. These will smash together and to grind the ore into a very fine powder Got this closed up. Okay, so this has been rolling for a couple of days now. Let's get this out of here and remove the balls and then we can start with the chemistry. So before I get this open I've actually got something I wanted to show you guys. You can, see this pipe right there, which I've got plumbed in from outside, where I've got a shop vac and if I plug this in right here *vacuum noises* We've got some airflow pulling this through water and outside. So now the dust, When i generate some, it's not gonna go into my lungs. Awesome. I can use that for chemicals too. So let's open this up. Now it looks like it's a lot finer. Still not like baby powder or anything Just run it through a sieve and get the metal balls out of it. I'm watchin' that dust just get sucked right on out. Awesome. Huh, all of the went through- well, most of it went through my screen here. That's a good sign. All right, so, there's a beaker, and I'm just gonna transfer the crushed ore into it. There we are. And to this I'm going to add a little bit of barium carbonate. You got about half a gram here. This is to boost the barium levels but also will sequester any sulfate ions that might be present. Now, to this I'm gonna, add some hydrochloric acid and that will start the dissolution of the uranium. So we're gonna, add quite a bit there The gasses coming off of this are primarily carbon dioxide, but there's also some hydrogen sulfide in there with it. Because there was a little bit of sulphide minerals in with the uranium. So after letting this sit for a while the reaction seems to have come to a stopping point. That means all of the carbonate and the sulfides have been destroyed. You'll notice I used a cheap acid for this step. If there was very much more carbonate I wouldn't have been able to use acid at all because it would destroy all the acid. For that, a carbonate leach would be used. I could have used a carbonate leach on this as well, but carbonate leeches are extremely slow. Now you might notice that the color the solution is a little bit green. Might be a little bit hard to see because it is still quite turbid. Let's actually take a small sample off of here, put it into a test tube, so you can see it a little better. To remove that turbidity I can employ my new toy here: A centrifuge. You can spin this up and it'll throw all those rock particles to the bottom. Alrighty Let's pull that out of there. Got a very dark green solution here. Let's actually put it in the light. Yeah, so now you can see through it and that it is indeed a green color. And this indicates that there is uranium dissolved into solution and it is in the +4 oxidation state. Now the thing is, I want the uranium to be in the +6 oxidation state and also not all the uranium will be dissolved. To solve both of those problems I'm going to be adding some nitric acid. This will also change the color from green to yellowish. Yeah, as you can see. Looks like it released a little bit of gas as well. One thing I like about uranium is all the different colors it makes. So let's plug the vacuum back in. *vacuum noise* We'll just add this to the rest of the solution. I'm gonna add the nitric acid just a little at a time, because it looked like it produced a lot of gas very rapidly. Yeah, I think that gas is actually nitrogen dioxide. You can, see this is the same gas that is produced when you dissolve any other metal in nitric acid. *vacuum noise* Looks like it stopped reacting and it looks like it has solidified. My guess is that is because there's a lot of uranium here and the room is currently at 0 degrees Celsius. I'm gonna have to either increase the temperature or increase the water and I think I'm gonna do both. So I have warmed it up a little and it's mostly fluid. Still rather turbid. We're just gonna add a little bit of water here, and see if we can get that to dissolve. So that's some distilled water. Just give this a little stir. I might have to pour it off into another container and add even more water. We'll see what this gets us. The goal here is to get it so that it's dissolved enough that I could run it through a filter. So I'm gonna use a vacuum filter for this and at first I'm just gonna take it off the pipette. See if it'll go through. Looks like we're good. All right, so I've diluted it and filtered it out. It's still a little bit turbid, but it's the best I could do. You can, see that it is still radioactive. Radioactive components are still in the liquid, although the water and this thick glass tube do provide a lot of shielding. Speaking of which, here's the rock that's left over after being washed with water several times. Put it up against the counter and it is still radioactive. It's not as strongly radioactive, though. So that means I was successful in removing most of the radiation from it. I think if I could have ground it up a little bit finer, maybe if I left it in the ball mill for another few days, I would have had a better recovery. As it is, I'm gonna save this and treat it as a low grade uranium ore sample. Anyway, this here is about ready to have the radium dropped out of it. I was hoping to have a little bit clearer solution, so that I'd have a pure product, but the radium is going to be contaminated with the calcium and barium sulfate anyway. But that is, of course, why I added the barium into there; it's to help pull the radium out of the solution. So for my source of sulfate ions I am going to be using just some sulfuric acid. So just add this in there, and that'll cause, the radium, barium, and probably calcium and lead, also, to be pulled out of the solution. Might be hard to tell on camera, but you can see that there is some cloudiness in there that wasn't there before, so... I think this might actually work. So it's the next day, we do have a layer of mud down on the bottom of the container. Excellent. Let's get that there and see how the Geiger counter reacts to it. So here's that mud. I just used the centrifuge to collect it and this is after washing it several times with water so there shouldn't be any uranium in here. You can see I'm still getting around 400 counts per minute and that's just off of this vial. It'll probably be even more once I have taken it out of here and removed the water. So here's the radium mud after being dried out. It's, uh... Turn on my Geiger counter... Ah, yeah, that's pretty radioactive. Looks like I'm getting almost 6000 counts per minute off of it. That makes sense because the radium should be producing about half the activity of the original or sample. Yeah, I didn't get all the radium, but you can see that this did work. It's actually rather probable that the tailings here contained a large portion of the radium. It never dissolved because it was already in the sulfate form. Anyway, this is not the main product I was looking for, so I'll set this aside; maybe I'll further concentrate the radium and make something out of it in a future video, but for now, let's go back to the uranium. For my next trick I'm going to be neutralizing all of the acids with some ammonium hydroxide and this will precipitate out the uranium, along with most of the transition metals. Just add a bunch in here. You can see the ammonium diuranate precipitating. Probably also got a lot of iron hydroxide mixed in with it. I need to go find a stir stick. *blow torch noise* Now I can this a good stir. So i'm just using some pH paper to gauge the pH. Looks like we're around eight. We'll go a little bit higher. I think ten, would be more than enough. Okay, that's, uh... That's a ten, so... Wonder what the chances are of this thing will settle out on its own. I might have to run this whole thing through the centrifuge That sounds fun. It's doable but it will be tedious. At least I'm not working with soluble uranium anymore. Think I am gonna call it a night, though. I'll let this settle out if it will. So another 24 hours have passed and as you can see it has settled out. It's about a third of the way, there. You notice this very nice purplish, blue coloring. I believe that's due to copper being complexed by the ammonia, and held into the solution. That's one reason why ammonia is used for this. Sodium hydroxide would also drop out the uranium in a similar way, but then it would also drop out the copper and absorb CO2 from the air, forming sodium carbonate, which could dissolve the uranium back. Anyway I'm going to decant this, then I'll figure out a way to further extract the water from this. Probably, gonna use a centrifuge. So I've transferred some of the slurry into this beaker, and I'm just using this to load, these centrifuge tubes. It would've taken a week to settle out that much. The worst part was that I had to wash it with water so I had to remix it and then separate it once again, but there we go, all ready for a carbonate leach. In case you're wondering what my plans are for the waste, this is the water that came off of the precipitated uranium, this probably contains a radon dissolved in there and there's not really much I can do to get that out besides, you know, letting it decay naturally... There's also copper, nickel, and various other salts in here along with traces of uranium, of course. I think my plan for this is to actually just store it until I get some warmer weather, then I'm gonna evaporate it down to a salt and cook it in the furnace and vitrify it into glass. Throughout this project I've also been accumulating these paper towels that have got the uranium on them, you know, if I drop a little bit of it you know I wipe it up and, well, here it is. I do plan on recovering it off of these. What I'm gonna do for that is actually just put it into this dilute hydrochloric acid solution and dissolve the uranium off of the paper. After a couple of washings I think the paper would be safe to throw away. Now of course once I've collected a bunch of stuff off the rags, I can add some ammonia to it to reprecipitate the uranium. Now I can just process this along with everything else. The ball mill and equipment, that stuff gets washed off normally, accepting, you know, I saved the wash water and the ball mule in particular, it's not gonna be used for anything else. In fact the next project I have planned for it will be the last thing it's used for. So anyway to reduce all the uranium I'm gonna be using a mixture of sodium carbonate, in this case, washing soda, combined with a load of sodium bicarbonate or baking soda. Get that dissolved into some warm water. I'll just mix this in with my mud. You might have to add more, but this will get it started. So I've got this set up in a hot water bath. I've got an air stone bubbling through it. I'll just let it sit here and leach for the next little while. So we're coming up on 24 hours later I'm gonna pull this bubble stone out of there so it can settle And we should have a uranyl carbonate solution. So after settling out overnight you can see half the solution is now a yellowish green color, and the mud, which is now more reddish has a smaller volume than it did last time I let it settle out, which means some of it has dissolved. this should have dissolved the uranium, vanadium, and molybdenum I just transferred out about half a liter. This is so I have plenty of room for the gas to bubble out. And now I'm just gonna set this into some warm water to heat it up. By the way, I'm using a piece of ball chain to keep the glass from directly contacting the hot metal. The reason I warmed it up is to help the carbon dioxide come out of solution, and also apparently ammonia. There we go. Just put a watch glass over it. And now I'm gonna acidify it. Any acid should work. I'm gonna use sulfuric acid because there's more of it in a smaller space and I'm just gonna add this in here slowly until a yellow precipitate starts forming. Should look about like this. I don't want to go to much more than that otherwise I'll redissolve the uranium. Yeah, I think, that's it right there. Right. Back into the hot water to boil off the rest of that CO2 then we can drop out the rest of the uranium. So now that I've reheated it to near boiling, I should be able to see that when I stir it, it doesn't really co2 anymore, just as I wanted. So now I'm gonna finish oxidizing it by adding some hydrogen peroxide. This is 35%. This should form a bright yellow precipitant which is actually my yellow cake. Added a little too much, too quickly. That's what this bowl is for. *laughter* Anyway, I've got it back into the beaker and you can see that it's a bright canary yellow. Very nice. I'm gonna keep adding peroxide so I can have an excess- I did it again didn't I? *more laughter* So anyway, you can see the uranium peroxide precipitating out. The hot solution, makes it clump together nicely. Theoretically, the vanadium, molybdenum, and other metals should remain in solution. So now I get to do this about five more times. So here's that uranium peroxide after I've concentrated, using the centrifuge. You see it's still wet, so I am gonna have to go put this in the desiccator to dry it out. I'm literally baking yellowcake. So this is the desiccator that I built for my sugar video. It's a fish tank with pans covered in calcium chloride to absorb the water, and it's also got an incandescent bulb for heating. This oughta dry this cake out in no time flat. See? It's already dry! Well, in reality it took about 12 hours, but here it is. Just gonna scrape this up into a powder. Looks like seventy six and a quarter grams. So here's my little bag of uranium peroxide. So this was 76 grams and I suspect that there's probably about 20 grams in various places that I'm still yet to recover, and I'm pretty sure I will recover it so let's say my initial recovery was about 75%, and then I'll probably bring that up to over 90% by the time I'm done. For now, though, lets get the Geiger counter going to see what that picks up on this. *Geiger counter clicking* So it seems to be up over 13,000 counts per minute, which is considerably less than the original rock sample, but consider that this weighs a lot less as well. It'll be interesting to see how its activity changes as those daughter products build up again. Probably a few months from now this will have twice the activity. But anyway I think I want to finish this off by producing a little bit of uranium metal. Let's see if we can do that. So I've weighed out about 6 grams of the uranium peroxide and i'm gonna bake it in my oven at apparently 700 degrees fahrenheit, or roughly 320 degrees celsius. This will convert it from the peroxide to the trioxide. So after cooking this for a little while, you can see it's changed colors to orange. Yeah, started off yellow, and now it's that. We got some uranium trioxide here. So, now I'm gonna transfer it over to this other beaker and I'm gonna dissolve it with some hydrochloric acid. Now that's dissolved, I'm going to add some dilute hydrofluoric acid. Yes, this is hydrogen fluoride. Approximately 3 molar. All right. Into this mixture, I'll add just a pinch of copper sulfate. This is to act as a catalyst. What we're trying to do here is, uh, we reduce the uranium from a +6 to a +4 and then the uranium tetrafluoride should precipitate out of solution. Of course, I am going to need a reducing agent, so I'm going to bubble some sulfur dioxide gas through this solution. To produce the sulfur dioxide I've got a little jar here with sodium metabisulfite. I'm just now injecting some acid to release the sulfur dioxide gas. There we go. We definitely got a change happening. The color is going more greenish. Presumably the uranium fluoride is precipitating. There it is. That looks like uranium tetrafluoride to me. So here's the green salt, all dried out. Let's weigh it here. Looks like we got about three point eight grams. Now the whole point of doing this to the uranium was to remove all oxygen from it. You see, if I were to just heat up the yellowcake with a reducing agent, it would just form uranium oxide. But this here should be much easier to turn into metal. Unfortunately, this is the hydrate of the salt. So I need to dehydrate it. Otherwise, the water will actually react to form uranium oxide. To solve this problem, I have transferred approximately one gram of the uranium tetrafluoride into this glass tube, hooked it up in a vacuum pump and I'm gonna gently heat it with a blowtorch. Hey, you can see the water boiling off. Well, it's not really boiling, it's dehydrating. It's being chemically separated from the salt. I'm going to heat it a little slower, I think it's beginning to react with the water vapor. If I were to heat this in air, the air would react with the uranium fluoride, forming uranium oxides. And, as I've mentioned before, uranium dioxide is very difficult to melt and I need to be able to melt it in order to produce the metal. Now that this is cooled off and I've removed it from the vacuum pump I'm going to drop in a one-tenth of a gram of lithium metal. Now this should react with the uranium forming lithium chloride and uranium metal. I'm gonna get it down in there and, conveniently, it's already encased in glass. So, now I'm gonna seal this off. And we're gonna put this down into the furnace and heat to 2,200 degrees Fahrenheit. Here's my glass with the dehydrated uranium fluoride and the lithium metal. Unfortunately, it broke while I was taking it off and let air in there and the lithium burned briefly. I might have to redo it. For my second attempt I've mixed in a little bit of calcium chloride and it seems to really help, with the dehydration process. It also melts and dissolves the fluoride and it actually protects it from further oxidation. At the temperatures I'm going to bring this to, the glass won't completely melt, but it will soften significantly, so to give it a little bit more strength, I'm gonna encase it in sand. The sand will also combine with the glass, forming a type of glass a little bit higher melting point. So this should keep the oxygen off of it. Put a lid on there, and throw this on the furnace. *furnace sounds* *boiling water hissing* *pop* Time for what we've all been waiting for. Yeah, pour off the sand here. Let's pull up that glass. Looks like it's relatively intact. *pounding* *harder pounding* *more pounding* That metal? Looks like it. Yeah, that's hard. It's not glass, is it? No, it's shiny! Yeah it's got a shiny underneath! Excellent! Let's drop that in some nitric acid to clean it up. All right. Into the acid. You hear how it rings when it hits the glass? *a very hard heavy material hitting glass* That tells me that it's a very hard heavy material. As you can see, I've dissolved a small amount of uranium off. It gives you that coloring to the solution. Let's pull it out. It's still kind of dark. Tells me it's not super pure. But there it is! A little bead of uranium metal. See what it weighs here... Right around a quarter of a gram. That's not bad at all. Although that's a lot of work for that quarter gram. I put it in a bottle of some kerosene to keep it from oxidizing further. There it is. It's still radioactive, but not a whole lot. There's not very much here. You might ask what I'm doing with the waste. You know, not all the uranium reacted and also, judging by all this broken glass here, you can see I've had a great number of failures. But, uh, this should be pretty easy, really. Just had some hydrochloric acid, just like that. Along with a little bit of nitric acid and basically treat this just like rock. With the one upside of the uranium that's here, being almost pure already. Just let this dissolve out, filter it, I can react this with ammonia to form relatively pure ammonium dye urinate. So, no further processing needed, just let it settle out of solution. Hope, you enjoyed I'll see you next time! *mechanical hissing* *mechanical hissing, clanking, and whirling, slowly getting faster*
now how did I know that this was going to be Cody'sLab?
"I have designed this crusher to minimize the dust leakage"
ADDS PAPER PLATE
LFMAO this guy.
Youtube's own Marie Curie! Hopefully with a happier ending.
God dam that was fascinating!
Is he wearing a pair of black leather gloves?
What do you think his lawyers said when he told them he was going to make yellow cake uranium?
I really don't know why companies are spending millions of dollars a day on milling uranium when anyone can just literally do it in their home/ backyard.