Palladium Recovery From Silver Cell Slimes Pt2

hello YouTube well channel ensuite tips and today what I'm going to attempt to do is refine the the Palladium that we extracted from the silver cell slimes of God hearing this beaker it's been sitting there since ever since I did that last video and I've also got some other palladium precipitate from some previous reactions that I did with dimethyl Block C or dmg and I recovered this out of some silver that I dissolved and from some of my electrolyte out of my silver cell so what we're going to do today is we're going to dissolve this in aqua region at first and then we're going to extract the palladium black powdered metal with some strips of pure zinc and I'm gonna do that right now for you in a previous video I used dimethyl block scene to precipitate the Palladium salt I poured it through a filter paper to collect the precipitate it's a yellow fluffy precipitate that forms when the Palladium mixes with the dime X dimethyl glycine then I took the filter and the precipitate and put it in a beaker okay in this video I'm gonna start out by adding the other filters that have some dried dimethyl block seem precipitated palladium salt in them to the main beaker and what I want to do here is get everything into one beaker so that I can dissolve everything in aqua region here's one of the filters I open it up to show you what the yellow precipitate looks like it's dried in a powdered form here I've got this in a fume hood this powdered salt is not good to breathe it's extremely important to not breathe this stuff [Music] next I put some hydrochloric acid into the beaker with the filters I fill it up to about the 300 ml level with hydrochloric acid [Music] here you can see the level is at 300 now I'll give it a quick swirl to try to mix everything up and then I'll put it on the hot plate and turn the hot plate up to medium after a minute or so you can see the solutions turning green and then after about a half an hour this is what it looks like after it's been boiling for about a half an hour before I go any further what I want to do is put a drop of my palladium standard test solution on a piece of filter paper here and I'm gonna test the potency of my stannous chloride it's a stannous chloride I'm gonna drop it out on here and you see I get that brown stain that means that my stannous chloride solution is good to go I made this palladium standard test solution by dissolving 1/10 of one gram of palladium in some dilute nitric acid and then I topped it off to 100ml so I got 100 milligrams or 1/10 of one gram in 100 ml of solution and that'll give me a standard test solution that I can judge how much up lady UNS going into solution with my experiment over here what I'm gonna do now is go ahead and dip the piece of filter paper into the experiment get a little on the end of it add some Stannis quartz we've got radium going into solution which is hydrochloric acid and it looks like I do just hydrochloric acids put some of that palladium in solution not what I'm gonna do is go ahead and start adding some nitric acid here this is a three ml pipette filled up to this level right here that's just over three ml at night Rick I'm gonna go ahead and just start dripping it in you want to add it too fast you can see we get a nice bubbling reaction there only got about a half ml in there for one like that so it's a careful add these reagents very slowly or you could get a boil over and have some problems I'm just gonna go ahead and wait on that like the Solutions been on boiling now for about a half an hour on medium heat I turned the heat down the temperature reading here on and I got 195 point five degrees inside that I've turned the heat down I'm gonna go ahead and try to add a little bit of more of this nitric acid now see what kind of reaction we get on that a little slow I got about another half ml in there and you can see it's highly reactive so we got to add that stuff very slowly in order to prevent having a boil over solution is down to 178 now go ahead and try to add some more nitric irritants if we can get it done get all in there all right that's better and tried about another one one half ml here [Music] so far I've got 4.5 ml and nitric acid in there okay this segment of video I it's been about the three four minutes since I added that last dose of night picking all of a sudden I experienced a runaway reaction I haven't added any more nitric acid I just wanted to get in close with the camera I seen it was gonna go over so I tried to set the camera down to try to do something I realized there was nothing I could do so I just picked the camera back up and filmed the old before disaster they had a too much nitrogen added it too quickly all right you get to see the mishaps and the air is here so what I'm gonna do is I'm gonna kill the power to the hot plate there let this cool down and clean it up and continue the experiment all right I'm gonna use a piece of paper towel here to try to stop up the overspill there put it in this other beaker okay this is seven years worth of experience working against me I got a false sense of security when I lowered the temperature and I put that first one and a half ml of nitrogen it didn't react very vigorously so but the second one and a Half Men melon nitrogen and then four minutes later I experienced that what a reaction this is due to my lack of experience with refining palladium I did not expect that runaway reaction and I got a big mess to clean up here so we'll do it and continue on all right I've allowed the solution to cool down now it's down to 84 degrees my lack of experience in refining palladium is what caused this mishap I've only done it a couple times and that's what caused this problem I do now is try to like remnants off of here what a mess I'm gonna try to quite the outside of the big graph here this stuff is highly toxic it's not quite as bad as platinum but it does cause problems in any Anya so I want to try to avoid that real careful here I'm just gonna try to pour this back into the beaker probably a mistake probably should pour this in the other jar I think there's some silver chloride it's gonna form in this container but was that the deal with it [Music] [Music] back on the heat keep going all right it's been back on the heat now for about 20 minutes it's up to 150 degrees or so what I'm gonna do is I'm going to use some hydrochloric acid and a pipette and rinse down the bits of the Lady of salt is clinging to the side of the beaker inside there [Music] now I'm gonna go ahead and start adding some more nitric acid see we can get everything to go in solution here this time I'm I'm gonna add it real slow it's about a half of a half of the melt I'm just gonna let that react you you [Music] over the last half-hour I went from 4.5 ml of nitric which some of that was lost when the overflow happened but I've added one for 4.5 to 11 which is what six and a half more ml over the last a half hour so go ahead and get a temperature reading now [Music] and we've got one hundred and seventy seven point five degrees Fahrenheit I think most of the palladium has dissolved now I'm going to just let this cook for a while the amount of night think that I've got in there and I keep going it till I see all those Olo specks that is all we'll check the bottom of the beakers who have got everything in solution then we'll proceed from there it's been about a half an hour since I added the last dose of nitric just let it sit I'm going to get another temperature reading here and we still have 175 or so I've got about 1 and 1/2 ml and nitric here we'll go ahead and add this to the beaker slowly we got about a half of it in there good night it's only been about a minute or so since I added that last dose I'm gonna add the rest of this a total 1.5 ml at 12.5 ml at night for kidding here I'm gonna give it a put a swirl and stir it up I want to check the take the bottom down here and see what kinda don't we got left see there's still some stuff that had dissolved yet so I'll just keep going with the nitric acid additions until I get all that to go into solution I've got another 1.5 ml of nitric acid I'm gonna go ahead and add it now it's been about an hour since I restarted the experiment what I'm gonna do is let this acid react until all the fumes go away and I'll check the bottom of the beaker to see how much is left to dissolve and if I have to on that score nitric acid did everything go into solution the Palladium solution has been on boiling now for about two hours since that last segment of video I've cranked the heat up and I added four more ml of concentrated nitric acid for a total of 18 we get a hit temperature reading here [Music] as you can see I got it up to 216 degrees Fahrenheit go ahead and turn the heat off and look up underneath the beaker here and see what all else has to go in the solution as you can see there's just a little bit out looks like silver chloride in the bottom of the beaker there all the plating has been dissolved now so I'm gonna go ahead and take it off the heat and let it cool off so we can filter it out this palladium precipitate was derived from from silver solutions so there's no way of getting around having a little bit of silver chloride in there with the lady 'm so what I'm gonna do here is I'm going to cool it down in an ice bath to get that silver chloride come out of sweetheart yeah come out of solution so that I can filter it out temperatures down to 106 [Music] you you solutions been in the ice bath for about 20 minutes now get the temperature down to 52 degrees [Music] I've got my filtering rig here cold so we keep everything cold got everything refrigerated had this water in the freezer so everything's nice and cold so when we go to filter this out won't heat it back up [Music] you you okay while I'm waiting for the the solution to filter out there I've got a box of zinc that I bought here this is pure zinc sheets at some place in Ohio I can't remember what the name of it is but I found them online and this is a they make stuff by the zinc and this is 99.9% pure zinc and these are just remnants of pieces that were left over after they got done with their projects it's 50 pounds of it and I think I paid $85 for it it'll last me for a lifetime so what I'm going to do is I'm going to cut this into some strips and then we'll use this to precipitate the clean palladium out of that solution [Music] I've completed the filtering operation here go ahead and take the funnel off now and move this up onto the syllabi phew mud here now what we'll do is transfer the solution into this large 2-liter beaker [Music] I will say it's got some residue and I'm not gonna add that to the main batch I'll probably add that to my stockpot here I have the pieces of zinc's that that I prepared earlier what I'm going to do is I'm going to go ahead and put this zinc metal into the palladium solution I twisted them so they don't set flat on the bottom and what will happen is the Palladium solution will react with the zinc and cause the zinc metal to dissolve but as it dissolves it will cement out the pure palladium metal as a black powder the two metals trade places during this chemical reaction the zinc goes into solution the Palladium comes out of solution as a black powder and when we get done what we'll have here is a green solution with some black powder in it hopefully that's what I'm expecting this is called cementing out the palladium onto the zinc as you can see here the that black residue on top of the phone there is an actual caladium metal a black powder that comes out of the solution as the zinc dissolves and goes into solution I'm going to add the rest of the zinc to it now the reaction is exothermic and this is heating up a little bit when I add the rest of the zinc in you you I went and chopped up smaller pieces of zinc here what I'm gonna do is go ahead and add these slowly and keep cementing out the lady Amon this zinc until it won't do it anymore until I don't get any kind of reaction what I'm expecting to happen here is for the solution to turn green and have the black powder the Palladium settle to the bottom of the beaker there I've got a lot of acid and chew up with these zinc pieces you [Music] you you [Applause] you the zinc reaction is progressing nicely I'm gonna go ahead and test this solution see if we got any uh palladium left and solution with some stannous chloride and you can see by that test nah we'll be cold the solution is taken on a greenish tint just like I expected and you can see the black powder building up on the bottom of the beaker there's the black powder that's our palladium down there as I stated earlier I'm gonna go ahead and just add this a little bit of palladium solution that's left in this flask down into my stock pot here it has residue in it and I did not want to add that to the main solution contaminate legged this beaker here here's our nice pretty zinc lady in metal it's a black powder and the zinc is still reacting in there he's turned a little slight green color I've got one more piece of zinc I'm gonna put in there a large one instead of dropping and hand us finish the a Senora I'll be able to pick that out what's all the acids digest about 12 hours into this process now the solution is turned back from a green color back to a burgundy color but I can see my metal down there it's I'll help three high down here I'm gonna go ahead that small pieces as a beer the reaction okay the book calls for a little bit of hydrochloric acid to be added if the reaction stalls I've got some zinc in there I'm gonna add just a little bit of hydrochloric acid here that little uh you actually pieces of zinc a little bit more hydrochloric acid really cleaned it up nicely I see the little pile of black-metal down on the bottom of the beaker there in a minute what I'll do is pick those pieces of sink out great off the liquid get our black lady of metal powder I'm gonna start drawing off some of the liquid out of the main beaker here with this pipette you that black powder is our Palladium against water on this right quick the link the acid and that whatever residual acid harcourt acids in there go ahead and dissolve the rest of the sink out of it I'm gonna add about 250 ml of distilled water right here's our first extraction of black lady empower already added some distilled water I'm gonna put in just a touch of hydrochloric acid - just a little bit here maybe just a few ml maybe five ten ml it's and what that'll do is that will dissolve off any residual pieces of zinc that's in the Palladium black powder I've got some distilled water and some hydrochloric acid in there with the powder the black palladium powder and I can still see just a few tiny pieces of zinc that's reacting in there I want to get all that out of there and what I'm looking for is for that fizzing action to completely cease and when that happens I go ahead and drain off the solution and rinse the black lady in powder real good with some fresh water I don't see any more bubbles coming up out of my metal here so I'm gonna conclude that all the zinc has been dissolved out of there I'm gonna go ahead and pour off my solution now into this container making sure my black powder stays in the main beaker here I'm gonna rinse the powder little bit of hydrochloric acid or that off into this container I've got some distilled water here that I heated up in the microwave I'm going to add about 250 ml and give it a quick rinse with that pull that off into this beaker here notice how that settles quickly do another quick rinse for this monster water [Applause] here is our black lady in powder who's gonna put some water on it put the lid on and then when I come back out tomorrow morning we'll continue the process the next step in the process here is to get a weight on our palladium powder that we have and to do that what I'm going to do is weigh this beaker and then write write on it what the weight is it's 115 point 2 grams so one one five point two grams one one five point two this next morning and what we want to do here is I'm gonna pour this water off and I'm gonna rinse the black powder out a couple more times I want to make sure all the zinc is out of that before I go to the next step actually what I'm gonna do is go ahead and transfer it into this little beaker right here the one that we just got the weight on here's our black powder the Palladium in the water in our little beaker here what I'm going to do is I'm gonna pour this rinse water off and give it a couple more rinses with some distilled water and the reason I'm doing this I want to make sure all the zinc is out of there before I go to the next step okay here's our black palladium powder that's been rinsed real well to make sure all the zinc is out of it this is the beaker it was in if you notice there's a little ring of black around it what I'll end up doing is probably put some aqua region in there just a little bit and there's all that and then add that to my stock pot here's our rinse water that we just rinsed the blacks off with the black powder and there's still a little bit of black powder that got poured over in the rinse I'll drain this water off and I'll save that put that in my stock pot as well and then back here I have the wastewater from the from earlier in the video it's got a big old piece of zinc in it and notice how black it is it's black as ink and I just wanted to show how we get this to clear up we just add little hydrochloric acid to it not much and what will happen is that will tend to make that colloidal suspension come out of solution and settle on the bottom and then once that happens what I'll do is get the blacks off the bottom of this beaker add it to my spot stockpot as well now back to our main beaker here this is our black powder I've got the weight of the beaker on the black on but the way through the beaker written right on the side of it and I'm gonna go ahead and evaporate this water off now to get as much of water off as I can and dry it to up and outer I'm gonna use a small pipe bed here and try to get as much this liquid off as I can before I start that evaporation process alright here's our black fellating powder that I've gotten a beaker here go ahead and put it on the heat now and turn the heat up to low and just let that slowly evaporate off until it's uh completely dry you you all right our palladium black powder is bone dry on the heat now here it is in our beaker and what I'm going to do is I've got the scale turned on down here we're gonna set the beak around here with the powder in it and measure how much powder we got okay we got one 15.2 on the beaker and one 22.7 with everything so that means we've got about seven point five grams of palladium powder in our beaker one twenty two point seven seven minus two is five twelve minus five is seven so we got seven seven point five so palladium black powder and our beaker here okay the next step in the process is we're gonna dissolve this palladium now that I know how much mass I have seven point five grams of palladium powder I want to create a solution where all this is in solution that is about 20 ml per gram in other words I've got seven point five grams so I want a solution that's going to be about 150 ml I had about a hundred ml of hydrochloric acid we're gonna put the mixture the Palladium in the hydrochloric acid here want some heat and I'm gonna start adding some hydrogen peroxide here I've got some 40% hydrogen peroxide that I bought at Sally's a beauty supply I guess they use it to bleach hair and this dissolved the Palladium I won't have to worry about any nitrate compounds being in there because we're not going to use aqua reagent to dissolve it we're going to be using the hydrogen peroxide and hydrochloric acid I've got the heat set on medium we'll go ahead and get a temperature I just set it on there it's only been on there for about two or three minutes it's up 250° which is about 60 to see I turn the heat down to about medium-low I'm gonna go ahead and add a little bit more how to do the rock side now give it a quick swirl with the mix things up [Music] I'm gonna add one more quick dose of hydrogen peroxide here I'm just gonna let that let that simmer for a while I had the solution on the heat here low heat for about half an hour [Music] you've got it at 133 degrees Fahrenheit fifty-six degrees centigrade they have one more shot of 40% hydrogen peroxide here the solutions been on there now for about an hour I've added about four doses of hydrogen peroxide where 58.4 see 137 degrees Fahrenheit at the 8.4 see what I'm gonna do now I'm gonna go ahead and pull this off and pour it into this beaker pour off the solution that we have dissolved into this beaker you can still see that there's plenty of black powder that has not dissolved yet so we'll put it back on the heat and continue with dissolving this black powder with how did your peroxide and hydrochloric acid that's hydrochloric acid for the planean powder and that last dose I added was not a hundred ml I said it was a 100 ml but it was only about 50 and that's what I'm gonna put in here right now another 50 ml or so [Music] Donaghy I'm gonna notch the heat up just a touch here go ahead and start adding some more hydrogen peroxide see if I can get all this stuff to go in solution quite a bit there they left to dissolve all right I had a three-shot so hydrogen peroxide that's about one and a half ml each there's some tiny bubbles forming inside the solution there after I did that last time three doses of hydrogen peroxide to eat up a little bit too so we going into the reaction I think the stuffs gonna go a little bit better with a little bit more heat okay the solution is heated up a little bit more now I've got that sixty two point six C 144 degrees Farenheit what I'm gonna do is go ahead and add another one and a half ml of but part of jumper oxide here and watch what the reaction does higher heat seems get a little bit better reaction there we've been about three or four minutes since that last addition I got another one and a half ml here and but the hierarchy that seems to be dissolving much quicker puts a little tick marks here for the number of doses one and a half and mental doses that I'm adding [Music] after Marisa put that last bit of hydrogen peroxide in and put 20 doses and what I'm gonna do now is go ahead and pour this off and see how much more power we got to go to dissolve getting down there but we still get quite a bit to go I'll just put this back on the heat with some more hydrogen peroxide hydrochloric acid and we'll just continue this process to meet all this time plenty of powder to go into solution kev allowed the solution to heat back up before i started adding the hydrogen peroxide we're at 176 degrees fahrenheit 79 to be centigrade we'll go ahead and add this one in slowly because it's a little hotter than it was before see what happens here you you it's been about five minutes since that wrapped 20 dose succession of hydrogen peroxide additions what we're going to do now is go ahead and pour this off see how much more black powder we have to dissolve and it's getting down there we've got less than 50% left to go there puts more hydrochloric acid in dissolving with the hydrogen peroxide I went ahead put the beaker that I'm pouring the solutions off into on the heat there so I can start evaporating that down to I need to get it down to 150 ml which will satisfy the 20 ml per gram concentration requirement that I'm looking forward to be able to precipitate the ammonium ammonia soluble lady and precipitate you I got 20 doses in this little beaker here where the powder was so I'm just gonna pull the lid off of that and let it go ahead and evaporate too it shouldn't be but just a little bit of powder left in the bottom of that will be both of the solutions have been on the eat now for about an hour I'm down here go ahead and pour this one off into the larger beaker see we got the powder left at the bottom of this little beeper it still needs to be dissolved while we got it all yet as you can see there we've got just a touch a little bit of powder in there he dissolves still so I have to add a little bit hydrochloric acid get that last one fit to go into solution we don't have much powder left in the beaker here so I'm just splash it a little bit of hydrochloric acid put it back on the heat and go ahead and add some more hydrogen peroxide to get this last little bit to go in solution and then we'll be done with that part of it [Music] I'm watching it dissolve right before my eyes to go to in solution yet and yes it has nothing left to dissolve so that's complete we got to do is evaporate these solutions down so then I have 150 ml [Music] before I go to the next step of the process now I'll add this last little bit of palladium solution that's been dissolved in hydrochloric acid and hydrogen peroxide to the main solution and then we'll evaporate this down to 150 ml concentration okay YouTube viewers this is going to conclude part 1 of the palladium refining video the video is already one hour long so I'm gonna have to make this a two-part video once I get that solution evaporating down to 150 ml what I'll be doing is adding some I'm William chloride to see if there's any platinum in there precipitate the Platinum out and then once I get the Platinum if any filtered out of that solution I'll be bubbling chlorine gas through it to try to make some ammonia soluble palladium salt and then what I'll do is I'll take that ammonium or ammonia soluble salt and dissolve it in ammonia filter it and then reify it with some hydrochloric acid to make some really pretty canary bright yellow hexa claw pallid eight it's a really pretty salt of palladium and then we just put that in a in a fused quartz dish and cal sign it into pure palladium sponge I've got the other video is still coming out I got my stockpot video to do I've got the catalytic converters the catalytic converter beads those are all coming out this is like oh this one here this plugin video is a practice run for those this I got to get up to speed with all these platinum group metals refining procedures before I can dive into those and come out with them some good results so I'd like to thank all my viewers and my subscribers thank you so much for sticking with me during these lean times when not cranking out too many videos I'm coming up on like thirty-eight thousand subscribers and that's just awesome you know you guys are really supporting me I like to answer questions if you have questions please leave those in the comment section and I try to get to those every day and look at those and answer those as best as I can so well this will conclude part one of the video tomorrow I'm going to continue on with part two and hopefully by that by the end of that part two I'll have you some nice pure palladium metal to show for the effort so thanks for watching oh I forgot one other thing my sweet wife Theresa Lynn hello Teresa she reminded me and made me promise to put this little clip in about our finances if you'd like to support me it costs money to run this shop and to buy the materials and they're all the chemicals and the glassware and the equipment and the material to refine and so if you could you could support me by going to my eBay website my eBay store my eBay user name is baffle Asst that's B a F e L o u s Mathis and I've got some really nice gold and silver items on my store in my store for sale these are some really nice gemstone original authentic gemstone rings and other things and they're like one-third of the retail price what you pay in a jewelry store and they're just sitting there people I don't know what's going on with the with the buy the jewelry I guess some people are holding back on doing stuff like that but instead of going to the jewelry store and spending $1000 you can come to my store and buy it for 300 so if you could go take a look at my based or Ballas be AF e Oh us and you could support me by buying a few of the items on there or just one whatever whatever whatever lose you so appreciate you for letting me put that message out there thanks for watching

Channel: sreetips

Views: 100,545

Keywords: hydrogen peroxide palladate precious metals refine

Id: XTVJcOUl8bE

Length: 63min 37sec (3817 seconds)

Published: Tue Apr 17 2018