Prepping 12 Buckets of Gold Waste Solutions for Palladium recovery Step 1 Silver Recovery

[00:00:03]Hi, I'm Victor. Welcome back to the lab.

[00:00:05]In this video, we're going to continue processing my gold refining waste solutions. In these 12 buckets of copper and basemental nitrates, the silver has already been processed out via the salt line sugar method. I do expect to find some silver chloride in the bottom of these buckets, but my main prize is the palladium or any leftover precious metals that might still be in solution.

[00:00:25]Before we begin, I have a small surprise. I got an orange bucket, y'all.

[00:00:31]Just as before in the video regarding the sugar and light waste solutions, this is not the first bucket nor the last. I think it's bucket number seven or so. I've set up a vacuum rig to remove the copper and basement nitrate solutions. I don't want to disturb any silver chloride at the bottom of the buckets. The plan is to remove the solution and then concentrate all the silver chloride down to one bucket for processing. After we process the silver chloride, we can then work on precipitating out any palladium or any other precious metals that might be in solution. You might ask yourself, where would those PGMs even come from? First, a lot of the sterling silver I used for importation is antique stuff from the 1800s, an era where separating out the PGMs was incredibly tough. But second, they could have been trapped with the original gold I started with. During the nitric acid parting step, metals like palladium dissolve right along with silver and other base metals. That means if there were any trace PGMs in either the antique silver or the gold, they'd be sitting right here in this liquid.

[00:01:28]That's going to be the main prize we're hunting for after we process the silver chloride. There is another benefit worth noting while I'm getting the nitrate solution off the silver chloride. It's the amount of lab storage space I'll be recovering from processing these buckets and the buckets themselves.

[00:01:44]The vacuum pump I'm using is new and I'm still dialing it in. This is why I'm not filling up the flask to the 2 L mark. I also don't want any splashing inside the flask to get down the vacuum line and ruin the pump. I could also turn the pump off before I remove it from the solution. However, the solution in the tube would then run back into the bucket, disturbing any sediment in the bucket, which is what I'm trying to avoid. I could also filter the sediment off the solution. However, if you ever tried to pour 12 buckets of nitrate solutions into a smaller filtration setup or into a smaller beaker to then filter, it's often an accident waiting to happen, at least for me. So, I prefer this method to reduce any chances of an accident. Here, I'm weaning the bucket using a wooden block to get as much of the solution off the silver chloride as possible.

[00:02:45]That's going to do it. Now that all the solution is removed, I'll get the remaining silver chloride and any other sediments into a bucket where I'm concentrating.

[00:02:53]First, I'll get all the sides rinsed down and try to move all the sediment to one side of the bucket so I can pour it more easily.

[00:03:03]Now, I realize the lighting here is not the best, but I do plan to have that fixed in the next video. I am still in the process of setting up this new lab.

[00:03:16]This bucket I have labeled silver chloride cons.

[00:03:26]Now we'll take our cons bucket and pour it into a beaker.

[00:03:35]I'm still trying not to disturb the sediment with this decant so I can further isolate the solution from the silver chloride I allowed to settle.

[00:03:44]I do have to be slow and careful. I can't really see what I'm pouring or when exactly it'll pour. And I'm going from a large bucket to a smaller beaker.

[00:03:52]And that can create the opportunity for accidents.

[00:04:07]One more to I think I'll have it.

[00:04:48]Let's get this silver chloride and any other sediment in beaker so we can work with it.

[00:04:53]Now, because I use a double pour and lean method, which I'll be using or demonstrating later, I often don't have much that gets poured over into my waste solutions. However, these material sediments still must be removed and processed to maintain high purity. Now, what I'm pouring into this beaker represents all the pourover from those 12 buckets of waste solutions. It is a testament as to how well the double pour and lean method is in keeping my silver chloride or refined gold precipitants out of my waste solutions.

[00:05:22]So really the less I get here indicates to me that when I refine I only lose a fraction of the material being refined to any rinses I do.

[00:05:37]Yep. I think we got it all in the beaker. get these sides rinsed down and clear off this workspace so we can begin processing the silver chloride. First step is going to be rinsing any copper and basemental nitrates off. So, the more water I add and swirls I do are all for the benefit of getting the solution rinsed off.

[00:06:07]However, before I get to that, let me clear out this fume hood there. All clear. And for a bit of housekeeping, I'm going to label this.

[00:06:22]A G C L Cons.

[00:06:30]You know, setting up this new lab for the first good day of work and going through these 12 buckets has taken most of the day. So, I think I'm going to call it here and I'll get back at it in the morning. I'll see you then.

[00:06:51]Good morning. It's day two of processing the gold refining waste solutions. Today we're going to work on the silver chloride. I'll start by getting a baseline to see where we are as far as how much copper nitrate we still have in solution that we need to get rinsed off.

[00:07:05]I'll do that by getting a sample and testing it with ammonia, which is a very sensitive test for copper in solution.

[00:07:12]Normally, I would either use a 10ml beaker or a spot plate, but the one I use broke in the mood of the new lab.

[00:07:18]So, I'm using some disposable plastic spoons as a temporary standin until my new one arrives. Couple of drops of our solution.

[00:07:40]Couple of drops of ammonia.

[00:07:58]Now, I'm not seeing any color change here. Maybe a hint of a thought of the faintest color of blue, but there's no way I'm trusting it's free of copper nitrate without at least a few rinses.

[00:08:08]So, let's get set up and start rinsing the copper and base metal nitrates off of the silver chloride.

[00:08:17]Remove this label.

[00:08:28]This I don't consider a rinse. This would be a decant.

[00:08:36]The misting is just water and it breaks surface tension allowing any floaters to sink.

[00:09:09]This is the first edition of rinse water which would start the first rinse.

[00:09:16]Not really sure why I decided to play three card monty here with the beakers and the dishes, but I square it away in a second.

[00:09:23]I believe my fune is off or rather I'm just not settled yet in a new laugh.

[00:09:29]When I stir or agitate, I do it for 30 seconds and then I allow everything to settle for a minimum of 5 minutes or until it appears that the solution is cleared up three card monty anyone.

[00:09:46]This is that double pour lean and settle method I was referring to earlier. It keeps your rinse materials out of your waste solutions and really is the best method I have found so far for doing so.

[00:09:57]misting to break surface tension with this method. I call this the pouroff beaker.

[00:10:25]This is the decanted solution that I will now pour off into my waste solution bucket. As you can see in the bottom of this beaker, by pouring off into a pouroff beaker first, we saved all that from ending up in our waste solution bucket. And with each rinse and subsequent pour off, it really adds up fast.

[00:10:42]This is now the first pour off of rinse water into our pouroff beaker.

[00:10:48]As that sediment in our pouroff beaker builds up, we can pour it back into our main beaker at any time to reclaim it.

[00:11:09]I know what's off. For you guys to have the best possible view, I need to shuffle my beakers around one more time.

[00:11:15]I think that's what's bothering me, trying to arrange things so that you guys have the best possible view. Now that all that's settled, let's get to rinsing.

[00:11:34]Heat. Heat.

[00:11:59]That's four additional rinses. Time to test with ammonia. That's four additional rinses after it had already tested negative for copper in solution.

[00:12:07]Let's confirm that one more time before we move on to the last stage. Converting the silver chloride to silver oxide.

[00:12:13]Again, I'll be using my patent pending disposable plastic spoon testing platform.

[00:12:49]That's looking pretty negative to me. No color change, no blue. I'll give it just a sec to give it time to react just to be sure.

[00:13:05]That's definitely negative.

[00:13:10]I'm adding about 400 ml of water just to give the lie enough room to react.

[00:13:16]With this little amount of water, I'll have to be careful with how much lie I add at one time. I don't want to cause a boil over.

[00:13:26]Reclaiming the silver chloride that got poured over into my pouroff beaker.

[00:14:07]This is the lie I'll be using. Sodium hydroxide. It's a drain opener, readily available and cheap.

[00:14:16]This is another of my personal adaptations. I find that once you open these containers of lie, they don't do a good job of keeping out moisture. But these Chinese soup containers are amazing at keeping it out. So once I open the bottle, that's where it goes. I am having to break this down a bit.

[00:14:32]That's cuz it came from a bottle that I didn't put in this container right away.

[00:14:36]So it got a bit of moisture in it.

[00:14:39]Crushing it up like this helps it to dissolve and not splash when it goes in.

[00:14:47]I'm going to start with two spoons. With this little water, heat management is going to have to be on point.

[00:14:55]Now, we stir until the temp starts to go back down. That means that all the lie we put in has reacted for the most part and generally safe for the next edition.

[00:15:07]The ambient temp is around 20C and the water is at room temp. So, that's our starting point.

[00:15:17]As you can see, with just two spoons, we got a 10° jump in temp. And it may take a minute for it to dissolve fully. So, if you're not careful, you can get a compounding effect really quickly, which is why you have to wait till the temps back off before you make the next addition. I also keep one of my squirt bottles in the mini fridge and some ice on hand if needed.

[00:15:39]lock and edge glass. So, it's a good idea to keep all your glassware as wet and rinsed down as possible.

[00:15:52]What I'm looking for is for the sediment to turn black. I periodically check to see the progress. When it hits jet black, we're done.

[00:16:04]That's the temperature fall I was looking for. Now, I can add more L.

[00:16:15]I'll add two more spoons here and see where that gets us.

[00:16:44]That's a non degree bump.

[00:16:52]Oh, let me go see what she's barking at.

[00:17:28]The temps falls. Time to add more.

[00:17:40]I think I'm getting close to being done.

[00:17:42]So, I'm going to slow down and add one spoon at a time now. It's not quite there, but it's close.

[00:18:11]As you can see, that temperature jumps up quick.

[00:18:27]I'm going to keep adding L like this until the powder in the beaker is black.

[00:19:03]And that's it. Jet black. Next, we'll reduce the silver oxide to metallic silver with sugar. The same sugar I use in my coffee. It did take a little longer than I expected to get it all converted to silver oxide. It was a bit stubborn till the end. Every time I checked it, it seemed to be just a shade of gray and not fully jet black, but it finally all turned. I would like to take a moment to say thanks for sticking with me while I built out and moved into my new lab. I know it took a minute, so I would just like to say thanks. This first day in the new lab with hands-on glass instead of saws and hammers has been fun and also revealed some needed improvements like lighting. But for now, I think we're going to make this part one and finish the reduction to silver in the next video. And after that, we're going to go after that palladium and any other precious metals that might be in those buckets of copper and base metal nitrates. That being said, I'd like to thank you for watching. I really appreciate it.