Palladium Recovery From Silver Cell Slimes pt1

hello you do viewers Street tips here I've had some a no basket filters from my electrolytic silver cell I've had those been saving those up and I find that accumulated since radon and so what we're going to do today is try to extract the precious metals from those used an old basket filters and we're going to do that for you right now [Music] this is impure silver shot it's mostly silver but silver is a carrier of platinum group metals and gold it's added to this Dacron filter basket atop my silver cell and an electric current is passed to it the electric current dissolves the silver are leaving the gold and platinum group metals behind as slimes as the silver dissolves it passes through that Dacron filter basket and goes into this silver cell it passes through electrolyte there and plates out as absolutely pure silver crystal on the inside of that stainless steel bowl and today what we're to do is we're going to get the silver cell slimes out of these baskets for you my electrolytic silver cell is full of pure silver crystal crystal right now so I'm going to begin the harvest of it by taking the the anode basket out and putting it in this bowl right here and then what we're going to do is demonstrate how to recover the precious metals out of these these used an old baskets take my an old bar and I put that in a beaker that's full of distilled water over here take the cover off the anode basket I set that aside because I'll reuse that and then I take the the slimes kind of a a bunch of murky mess in there this is the platinum group metals maybe some gold and stuff it's the slimes is left behind from the silver cell the refining operation I'm supposed to do okay to begin this what I'm gonna do is take one of the filters here it's full of the slimes and I'm gonna take still water go ahead and let it rinse out into the beaker here it's a big pieces off with some distilled water then once I got it rinsed off transferred over to this other beaker go to the next [Music] [Music] [Music] now what I'm going to do is add some money this is full of the slimes and distilled water go ahead and add a little bit of nitric acid and start to dissolve an out the silver in the lady the little night - gasp they had about [Music] I guess it's gonna be about 100ml here place it on heat [Music] let it dissolve leading me I've set up another burner in here I'm going to add some distilled water to these these used filters here then I'm gonna hit it with some nitric acid by about a hundred 200 ml or so and just boil these boil these bags in nitric acid dilute nitric acid both of the beakers have been on now for about forty-five minutes you see the moment of build presenting solutions green looking that's an indication of little gets lady him out of there and this one over here has got a green tint to it as well we're gonna be harvesting some palladium at least out of these silver cell slimes I'm gonna give the the filters here quick stir [Music] I'm gonna add another dose of nitric acid here to the to the slides on this side been doing careful because that solutions hot and we don't want this thing bubbling up furiously still a lot of particulate matter down there black slimes now we're gonna get us a nice little reaction out of it pulled this one off the heat and as you can see there's about a inch deep thickness of blood on the bottom of that four liter people I'm quite sure what all that is but he came out of the filters it's a lot of material [Music] I don't know what to expect out of this so we'll just continue to hit it with the dilute nitric acid and see if I see what comes out of it [Music] both of the beakers have been on the heat now for about two and a half hours get a quick temperature reading on this one here and it's got that one up to 168 point five degrees and then on this one got up to 177 degrees now what I'm going to do is take this one off the heat it's still got quite a bit of material down to the bottom of it and I'm gonna take this one back here that's been boiling need the filters I pour this solution right in with this other rock this other mixture here and now get a good reaction noose if you've seen that this is real acidic so we've got to kind of be careful both solutions are real hot I had that real slow there okay I think that's about enough that might give this a stir make sure then we aren't gonna get a huge reaction here yeah it is gonna yeah pretty good when I go to stir it's better watch it there stuff's caked up on the bottom there but it hits that hot acid as I stir it it reacts pretty vigorously so I'm gonna have to watch how I add this acid don't want to add too much it'll boil it over you've got that pretty much that dose of acid from the filters pretty much reacted I'm gonna go ahead and add the rest of the a stop of the filters now and slow nice busy reaction here I'm gonna set that back on the heat put in about half a liter of still water and let that cook a little while longer to cook the rest of that acid out of those filters stir this up a little bit see what we get going here yeah I think I'm gonna go ahead and put this back on the heat just let just reacted we've got a piece of filter paper here go ahead stick the little bit of the solution from the big beaker there on my paper do a stannous chloride check right quick just see what kind of solution we got going on in there and it's like I've got a little bit of platinum there it's kind of an orange color and a brown color so there's some play them in there definitely got precious metals in there so I'm gonna get something out of it the filters have been boiling now for about a half an hour and just distilled water stir them up a little bit here she looks just like a little bit of a tent the green do it now what I'll do is go ahead and put down the main beaker and pour that water in here well let's give this a stir and put it back on the heat there let it react [Music] [Music] I'm going to add about 50 more email a concentrated nitric acid now and we'll just let this cook [Music] the solutions been on now for little over four hours and I've got a bunch of a solid material still tomorrow's because some adds more night solution here I'm gonna have another 200ml of still water we've got about a hundred ml of nitric acid left in here I'm gonna slowly add it to the beaker and see if we get the rest this stuff to go in solution I just have that - gas stop the mix down the down at the bottom contains all the party pretty vigorous match the freshly added nitric tends to suspend on top of the liquid in the beaker due to the different densities of the two fluids and the natural circulation causes it to mix and then creates this runaway reaction and that's what happens if you had the nitric acid to quickly I'm right at five and a half hours with this it's been on the high e that's at 214 degrees right now I've got some [Music] chicklet matter still down in there see that one just like Lisa silver still and what I'm gonna do is go ahead turn the heat off here let this cool down and then I'll siphon out the solution that I've got he got dissolved and go from there I've allowed the solution to cool overnight it's been settling overnight and so in that what I'm going to do is I've got a little tube in here filled it full of water put one end of the tube I clogged up the mine down here the other end into the solution just let my thumb off what solution - now we can have a look and see what's down inside of this beaker left over see we got plenty of solid dive pieces left in there looks like it's mostly silver this is stuff that was in the anode baskets from the silver cell left over that didn't dissolve when we disassembled the cell looks like it's mostly silver we'll go ahead and continue with hot dilute nitric acid treatments try to get everything here to go in solution I've completed the filtering operation here here's our filter it's got a little bit of residue on it so I'm ready take it out of the funnel here add it back into our main beaker I'll put this up on the heat now or me got 250 ml of distilled water I'll go ahead and add that [Music] now go yet at about this is ice-cold I just started this home they had about a hundred ml of button I can asked here [Music] just cover this up now [Music] and let this cook so we get the rest of those solids to go in solution the solutions been boiling now for about an hour after that that last nitric Edition and we got the temperature at 2:07 right now but if you looked at in here the bottom I can still see something this is a shower there are undissolved so I'm gonna have to add some more nitrogen you know let go and solution but ass slowly add another 50 ml of ah nitric acid to see if we get the rest of this sober too long to dissolve it's been about a half an hour since I added that last dosage of nitric acid gonna get a temperature reading here we've got that 217 degrees which is really hot and I had the remaining 20 or so ml of nitric acid here see we get the rest of that stuff to go in solution alright you got that 20 mm 20 ml and nitric in there go ahead and let this side let this go see we get the rest of that silver dissolved [Music] pair solutions been allowed to cool now it's below 100 that's at 82 degrees but what I'm gonna do is go ahead and filter it badly filter paper here try to get the solids out of the solution [Music] yeah and that nearly got everything out of the beaker here is some fine black sediment coming out I don't know what that's gonna be it didn't dissolve in the dilute nitric and I've got a bunch of got a whole bunch of silver left in here yet that I'm gonna have to try to hit with some more nitrate and get everything dissolved wanna heat add 250 ml water distilled water turn the heat on here medium over here I've got 50 ml concentrated nitric acid you can go ahead and add that 250 ml of distilled water in a beaker with the rest of the yeah silver good pour this in now I've got the heat set on medium go ahead and cover this up see if when you get the rest of that silver to dissolve and the filtrate in this looks real clear it's emerald green looking so I'm thinking there's gonna be some play diem in there up in the funnel here I've got this black liquid itself filtering out and the black solids I'm not sure what that's going to be maybe it'll be some precious metals we'll find out what you spot the region and just added that nitric acid DML to the remaining silver the big beaker there we'll go ahead let this dissolve and continue on with this process [Music] the solution is clear and green and the residue and the filter here I'm going to rinse all the rinses much the silver out of it as I can and then I'm going to put this filter aside and process it separate later on in this video [Music] just kept adding small doses of nitric acid and distilled water and I don't have any more particulate matter in there are no solids in there I'm gonna go ahead and pull it off it's got no fumes coming from it at all I'm just gonna go ahead and pull it off the heat now turn the heat off and let this cool down we'll do a filtering on it down here I've got the the solids that I filtered out of the the green liquid here I've rinsed those all down I'm going to go ahead and put this filter with those solids right in a separate beaker right here and I'm going to process those separately I've allowed this solution to cool it's down to ambient temperature right now which is down into the 50s probably easily it's down to forty three point five degrees so we've allowed that to cool down and I just want to review right quick where I am this is the main beaker to add this line this is the beaker that had the up filters in it and I'm going to save these filters put them over the filter storage and process them later these are the two acid nitric acid extractions that I'd saved in these up last back here and this is the residue from the gravity filtration that I did then I'm going to process that separately with the aqua regia and now I'm going to continue with the process right now I'm going to start this by pouring off some of the solution in this flask into the larger flask so we can make some room in here be able to filter this out now what I'll do is filter the solution out of this the main beaker everything's dissolved and they're all I have is some black residue in the bottom of the beaker a port through this filter paper and try to capture the the black powder in this filter [Music] at this point I've got all the silver dissolved and in solution these solutions are green this is probably going to contain this is going to contain some silver and probably some palladium and we're going to extract them play diem first out of this this big flask here has got the same solution dissolved with dilute nitric acid it's going to contain some silver lots of silver and then the green color of it tells me it's going to be full of palladium as well I'll show you how to extract that this filter here is going to have the solids that didn't dissolve in the nitric acid I'm not sure what's going to be in there but we're going to hit that with alkyl region up in this filter will also be some black solids and I'll take it out of this filter and add it to this container here and we'll process both of these with aqua regia the container here that was the main beaker everything is gone in the solution here except for a bring down the bottom there and then up a little piece so we've got everything in solution and what we'll do next is once we get this filtered I'll go ahead and prepare a solution of dimethyl Glocke scene or dmg and we'll extract the Palladium I've got the black solids filtered out of the solution now there's some black residue down there I'm gonna add it to this beaker over here with the other filter that had the black residue we're going to process this separately up to this point I've got the medals that will dissolve and dilute nitric acid in these two flasks in this beaker have two filters with metals that will not dissolve in dilute nitric acid and so we've got it separated to this point and so far what I wanted to point out is earlier I'd to the Stannis test and you notice that there was some platinum in solution indicated by the orange color of the Platinum test and some of you may be wondering how can he have platinum in solution if all he's done is treat the silver sauce limes with the live nitric acid Platinum and Gold will not dissolve in dilute nitric acid that's what's gonna probably be in here platinum with the gold palladium and silver both go into solution with hot glue nitric acid the question becomes how did palladium or how did platinum get in with the silver complain here there's one exception to the Platinum not dissolving I took an acid rule and it's this if platinum is alloy with silver 5% platinum and 95% silver when you put that alloy in the loop hot nitric acid both metals will go into solution totally it's an anomaly in refining I don't know what the chemistry behind it maybe some of you can make leave comments and tell us what's going on there I don't know what it is platinum by itself will not go into solution with just dilute nitric acid but it when it's alloy with silver at a ratio of 5% platinum and 95% silver when you put hot dilute nitric acid on that alloy both metals will go into solution that's why I've got a little bit of platinum in with my silver and palladium solutions okay before I go to a region with these filters what I'm gonna do is I've got a 150 ml of distilled water here and I'm going to add 250 ml of concentrated nitric acid to that to make a dilute solution solution of nitric acid that's 150 ml of distilled water and 50 ml of concentrated nitric acid now what I'm going to do is pour that in here with the filters and I'll put this on the heat let this let this cook for a while medium heat the reason I'm doing that is to make absolutely sure that I've got all the silver extracted from that before I go to aqua region the reason for that is aqua regia has hydrochloric acid if there's any silver in here the silver will hit the hydrochloric acid and immediately convert the silver chloride that causes filtering problems and problems with contamination of silver in with these metals so we're going to boil this and hide the loot nitric acid one more time to get make sure I got all the silver oddity while I have the filters up boiling in dilute nitric acid I've set up my hotplate stirrer here and I've got 150 ml of distilled water I'm going to drop in a little stir bar here turn that on and then what I'm gonna do is I'm gonna add some dimethyl bloxy more dmg dmg will dissolve in hot water so I'm gonna put some dmg in here and we're going to get some of this to dissolve and then prepare to precipitate out the Palladium idea on silver solutions [Music] [Music] now I'll transfer the silver and palladium solutions to this large 4 litre beaker it's been it's clean [Music] [Music] all right the dmg has been on here on the heat now stirring for about ten minutes it's at one hundred sixty six point five degrees the solution in the beaker here is ice-cold at forty four point five degrees but that shouldn't make any difference cool we're going to do here as I said earlier dmg is not very soluble in water but it will dissolve enough and hot water in order to be able to do this reaction I do here's slowly add the dmg while I stirred to pick that completely over some papers you see that yellow color it stopped right here that's the plate you know when I the solution has add the dmg it's gonna take a while for this to react it forms a bright yellow precipitate that is a palladium salt that can be extracted dump it out and then refined gonna leave the silver behind [Music] I've got the rest of the dmg dissolved 12 I can't and that hot still water go ahead add into the main beaker here careful not to pour the egg in with it the Palladium precipitate here is beginning to settle out and I've got the silver and the Palladium separated pretty good in that beaker now what I'm going to do I've got a big filter here that I put down into a Buchner funnel and I'm gonna go ahead and vacuum filter the silver solution and get the Palladium salt out of there [Music] I started this filtering operation and looked at the filtrate it's supposed to be blue but it's still green and I think what I've got is I've got some palladium still in solution so I'm gonna mix up some more dmg and after the big beaker here [Music] I mixed up another solution of a hundred and 50 ml of distilled water I've used about this a 30 gram bottle I've used about a third of it with this operation including the first mixture of a dmg and this one so I was probably about 10 grams that I've that I'll be putting into the into the a palladium solution told with this dose and the previous dose all right that dosage of dmg is up to about 165 degrees I'm gonna go ahead and slowly add it here while stirring we get the rest of the place into low come out of solution oh yeah there's some there's more in there I can see it taken out as I add this [Music] [Music] okay I got a total of about 10 grams of dmg in here dissolved in hot water hey the solution still looks green here go ahead and fill through this out now and then I'll deal with the PS solution once I get everything filtered out put this back right here now this is looking much better that's our solution with the Palladium salt in it we're filtering that out here's our solution looks blue which is what it should look like instead of green that'll be silver in solution with some copper in solution so we've we've effectively separated the silver and a copper in the palladium [Music] I've got all the solution filtered now all the Palladium salt has been rinsed down into the bottom of the filter there and what I'm doing is making sure I got clear water coming through here I do not want a bunch of silver in with my palladium salt because when I go and refine this palladium but if you use an aqua region and silver in there will form silver chloride and cause problems for me so I'm rinsing this out real good with some distilled water okay this class is full so I'm gonna trade out the flasks what a it's place here [Music] they keep rinsing this too like it all be the silver rinsed out of it rinse it real good so we can not and we put it in the outer region we don't get a bunch of silver chloride forming in the Ottoman region all righty now what I'm gonna do is I've got this palladium solved down to the bottom of the filter there it's been rinsed several times with the plenty of distilled water and I'm just going to put this whole filter right into a separate beaker here yes [Music] there we go up to this point I've got these medals separated out of the silver cell slimes back here I've got a bottle full of silver in solution here I've got the palladium extracted from that and a filter process that later on and over here I've got the black solids that didn't dissolve in the hot dilute nitric acid what I'm gonna do is I'm gonna go ahead and filter these out now I've had them on boiling in dilute nitric acid now for about I had him on boiling for several hours but I'm gonna go ahead and filter this off now and get the solids out of this liquid he's got a purplish black color to it I'm not sure what all is going to be in here but we'll find out and there's the mud that's left over we get that down into this filter and then we'll process this later alright now I'm going to take an get one drop of this solution coming out is filter on a piece of filter paper here and we're going to do a status test on this and see what kind of metals we've got possibly in solution and I don't have a whole lot of reaction near it's got a little brownish color to it probably just a touch more palladium in there but not very much [Music] here's our solids from the hot night with treatment I'm gonna go ahead and rinse these out now I've got the solids filtered out now there's quite a bit of stuff in there keep in mind there's two filter papers in there with it what I'm gonna do is I'm gonna add that to this beaker right here and then this material here this this is some silver nitrate with a little bit of palladium in it and what I'll probably end up doing without is just saving it I'll add some hydrochloric acid and precipitate out silver chloride and then filter out the silver chloride draw off the Palladium solution and put that in my stockpot there's not enough palladium in there to go chasing after here's all three of the separations that I was able to achieve from these silver cell slimes back here I've got about four liters full of a solution that's going to have silver in it here I have all the palladium that I extracted out of the silver solution I use dimethyl oxime or DM G to extract this material and here I have the solids from the dilute nitric acid treatments of the silver slimes the stuff that didn't dissolve in hot dilute nitric acid it's all been filtered out it's in the bottom of this beaker okay we're gonna start with the silver I'm gonna divide the silver up and these two four litre beakers evenly [Music] now I'm going to use hydrochloric acid convert to silver - silver chloride in both of these beakers [Music] [Music] yeah I've got both of these mixed up real well I've got all the silver to come out of solution with the hydrochloric acid [Music] we've got a tube full of water here with my thumb over one and put the other end in the solution I want to psych him and just siphon it off into this waste bucket here [Music] now I fill these back up with some hot tap water sperm and siphon each one again okay what we're gonna do now is use this little handheld blender it's got a little blade on it there I bought this for three bucks at the thrift store and we're going to convert the silver chloride using a lie I'm going to convert the silver chloride to silver oxide be a black colored material when we get done stick the handheld blender in here write it off start adding some my 40 micron side I'm adding a little bit of tap water here to help the reaction law [Music] now I'm gonna add some more more sodium hydroxide [Music] a little bit more tap water [Music] that's more sodium hydroxide [Music] yeah the next speaker here Keppel tap water to help the reaction but my blender in at some sodium hydroxide [Music] [Music] it took two pounds each of sodium hydroxide to convert these silver chloride jars to silver oxide to do the next part of the reaction I put them put the beaker down inside of a five-gallon bucket here now I'm going to add some sugar to the solution down there it's at 140 degrees right now you're gonna watch out adding this sugar you add too fast and you'll boil boil this solution it all over the place but I have a little bit more sugar now one of these times is gonna be the trick and that reaction will just take off up to 150° on the solution now give it a quick stir here and now we're getting the reaction there see the temperatures rapidly climbing it's up to 186 that goes 192 97 201 that wasn't too bad 2:14 it's gonna boil over my squeezing that put it in that bucket down there 215 degrees 220 okay I think the reaction is complete now as you can see there's our silver that'll be some nice pure silver once we get all that Lyon sugar rinsed off of it [Music] it's gonna go ahead and add some sugar now if this is a react he's only up to 160 a little more sugar here and this slope or that reaction really take off there it goes to 20 on the temperature see why I put in the bucket there I hadn't had it that bucket I'd have silver everywhere here I siphon the lye and sugar solution off of the silver and into a waste bucket because I'll be reclaiming the silver out of the bucket as well I rinsed the silver powder with hot tap water and then siphon off that into the waste bucket I've got all the silver out here I've rinsed it several times with some hot tap water and then I let it settle and then I'll get all this silver out and I'll melt that up into shot and I'll put that to my electrolytic silver cell judging by the amount that I've seen in the past that's gonna be just about one kilo or about thousand grams of silver between those two beakers next I'm going to turn my attention to this beaker here it has the the solids that did not dissolve in the hot dilute nitric acid treatments I'm going to begin this process of seeing what we got in there by adding some hydrochloric acid I'm going to put about I'll fill up to about the 200 ml level here I'm going to turn the heat up to about medium-low the beakers been on the heat now for about 15 minutes temperature in there is 152 degrees I'm gonna go ahead and add some nitric acid now about six ml or so [Music] I'm gonna give it a quick swirl here to stir it up [Music] already the solution has been on now for about two and a half hours temperatures at 170 what I'm gonna do now is go ahead I can see in there that it's got a ton of silver chloride in it down in the bottom I don't see that or not very well but what I'm gonna do now is go ahead and shut the heat off and just let this settle out the best way to get that silver chloride out of that solution is just to let it settle and cool down and then we'll draw off the the liquid on top and then just filter a little bit of the silver chloride I'll show you how to do that here in a minute the solution has been settling now for a couple hours I've got a piece of filter paper here get a little bit of the solution on it and put a piece of our drop of Stannis here and see what we got in solution there and that brown stain right there indicates we've got gold in the solution the solution is cool is down around 50 degrees and it's settled nicely it's got a bunch of us nothing builds up on a pilot there's water you recite this into a filter blast [Music] okay this solution here took less a minute to roll through that filter now what I'm going to do is I'm going to add the rest of the solution now that's got the silver chloride in it and it's gonna slow down significantly now I got most of the liquid through go ahead and pour this in now go to the solution off of that some requirements in this in this beaker here got all the gold filters out now what I'm gonna do is pour it into another beaker here and then we'll precipitate it with some sodium metabisulfite or SMD now I'll add some sodium metabisulfite or SMB and will precipitate the pure gold out of this solution now I'll let this settle will filter the gold out melted up into a button and getting healed okay normally I would let this settle overnight but I've been working on this for four days now and I want to go ahead and get this thing wrapped up this evening to get done the video posted so I'm just gonna go ahead and filter this [Music] you okay now I'm gonna transfer the gold what filter and everything over here to a melt dish and we'll go ahead and melt this into a button I'm going to pour a liberal amount of borax on to the filter here go ahead and store try it melt it up you you all right here's our little gold bead that we got out of the filters there here is our little gold bead that we recovered out of the silver cell slimes there go ahead and put on the scale see what how much it weighs here 1.1 grams 1.1 grams of pure gold is probably about 99% what I'll do is I'll throw this in with the next batch of carat scrap that I refine okay this will conclude the silver cell slimes video I was pleased with the result I was able to extract about about 1 kilo of pure silver I've got 1.1 grams pure gold and I extracted the Palladium here the video started to get pretty long it's over an hour long and so what all I have to do is refine this into metal in a separate video so that'll be coming up this is the this is the Palladium salt that I extracted out of the silver I've also got a an Alaskan placer gold video coming up I got some pieces of gold here in a little vial we're gonna try a new procedure on this I've got a bunch of watch batteries back here but I want to try to extract the silver out of of course I got my catalytic converter videos i getta get started on my stockpot and also the pure silver chess set so all that's coming up like to thank all my viewers thanks for tuning in or watching these videos it's important to me that that you learned something from these I read my comments daily and try to answer any questions that you might have concerning any of the procedures in these videos so that'll do it for this video thanks for watching and good night

Channel: sreetips

Views: 104,089

Keywords: Gold platinum refining filter anode basket

Id: m__zV793nC4

Length: 63min 53sec (3833 seconds)

Published: Sat Feb 03 2018