Welcoem to posts!!
in the future - u will be able to do some more stuff here,,,!! like pat catgirl- i mean um yeah... for now u can only see others's posts :c
Method for refining DMG precipitated palladium
If you want 992 parts per thousand palladium (industry standard for pure palladium) then, in a fume hood, dissolve the DMG Pd salt in AR, do this in a large beaker because it could boil over on you very easily. Once dissolved, denoxx by evaporation, then rehydrate with HCl and filter out any silver chloride. Reduce to metallic Pd with zinc. Remove any excess zinc with dilute hcl. Then rinse with hot water until neutral pH. Dry the metallic black metal - thereās probably platinum in there with the Pd because DMG will drop platinum along with the palladium. Get a weight on the dry mixed black pgm powders. Dissolve the mixed black pgm powder (in a fume hood) using hot HCl and hydrogen peroxide. This will avoid having any excess nitric. Once the metals are dissolved completely, adjust the liquid by evaporation to achieve a concentration of 20ml per gram of metal. If you had 100g of mixed black pgm, then you want a solution that is 20ml per gram of metal or 2000ml for 100g of metal in solution. Filter it again to remove any solids, careful not to add too much rinse liquid to throw the concentration off. Now prepare a saturated solution of ammonium chloride. Add the ammonium chloride to the dissolved metals. Any platinum in solution (if any) should come down as a fine yellow powder. Add more ammonium chloride to completely infuse the remaining solution that has your Pd in it with ammonium chloride. Excess ammonium chloride is necessary for the next reaction to get your palladium. Filter out the platinum salt and save it. Donāt rinse with water or else it will try to go back in solution, use ammonium chloride water to rinse the platinum salt. Donāt rinse it into the palladium solution, take the funnel off the palladium solution and put it on a separate container to avoid getting any platinum in your palladium solution. Then use the ammonium chloride water (distilled water with ammonium chloride dissolved in it) to rinse the yellow platinum salt. Save the platinum salt (if any) for further refining later. Now, in a fume hood, set up a chlorine gas generator. Bubble chlorine gas into the ammonium chloride infused palladium solution. The reaction happens quickly, turning the solution to a brick-red palladium salt that is soluble in ammonia. If the solution is still dark, add some more saturated ammonium chloride water so that the chlorine sparge gets all the palladium to convert to the ammonia-soluble, brick-red, Pd salt. When the chlorine reaction is complete, filter out the brick-red palladium salt, collect it in a filter. Next, place the filtered brick-red palladium salt, filter and all, into a clean beaker and add some ammonia. Iāve used ten percent grocery store ammonia, but 30% reagent grade works faster and creates less waste. Add stirring and gentle heat and the brick-red palladium salt will dissolve in the ammonia. Next, filter out any solids and collect the clear palladium/ammonia liquid. Transfer the liquid to a clean beaker and add hydrochloric acid until you see a bright yellow precipitate form. This is your pure palladium salt. Collect the bright yellow salt in a filter paper, get it as dry as you can to avoid spattering during the next step. Then burn the yellow salt in a fused quartz dish or a Corning ware dish until all the yellow color is gone and your left with a gray ash. Go slow because the yellow salt can melt and youāll lose some of your metal. If you see the yellow salt turning black, smoking and melting then turn the heat down and heat it slowly. This gray ash is your pure palladium sponge. Put it in a crucible and melt into a button. First time will be the most difficult. If your careful at each step, your palladium should be very pure.
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Some have asked about submerging our gold filled or gold plated items in aqua regia to strip off the gold then quickly removing once all the gold is off. Here is a paragraph from āRefining Precious Metal Wastesā by C.M. Hoke (available as a free download all over the internet) that kind of describes why itās not a good technique to use to recover the gold from that type of material.
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A Word About Rhodium
Hello and āthank youā to all my subscribers. If not for you, my channel wouldnāt exist. I realize that refining precious metals is a very narrow category with a limited audience. But I am truly thankful for the success that has been granted to me, through you! I know that I have rhodium, but I have no idea how to even detect it - yet. Iāll just keep saving filters and solutions, like I already do, until I figure out how to detect, recover and refine RHODIUM. People who know how to detect and recover rhodium are not eager to share their secrets with the masses. There is no go-to place to learn the process of getting rhodium. Itās shrouded in secrecy. But I guarantee, I will figure it out. Iāve pretty much got this far through trial and error, and much help from professional refiners on the goldrefiningforum.com. So why not trial-and-error my way to rhodium? Thereās one key ingredient in becoming successful at anything in life: an intense desire to succeed! Thanks to you ALL, donāt cut corners, and stay safe!
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BEHOLD: The power of gold
A brief story: yesterday I bought some scraps of karat gold from an elderly woman. Her late husband didnāt pay real estate taxes for several years on their house. It was sold, unknowingly, at a tax sale auction for a few thousand dollars. She had received notice that she would be evicted if a payment was not received soon. She was packing her things to move out. She was distraught. Not sleeping. No savings and no way to pay the debt. An estate sale friend of hers (and ours), knew that we bought gold. So she (our mutual friend) arranged a meeting at her home. She (the lady about to lose her home) brought some bits and pieces of karat gold. I weighed it up and offered her two grand - 80% of spot. Her jaw dropped and tears began running down her face. She took the money, hugged me, and thanked me profusely. āNow I can finally sleep tonight for a changeā, is what she was saying. Behold, the power of gold! PS - she got more gold jewelry that she can sell to pay off the debt completely and save her home. It was a joy to be part of that - plus i made a little profit. What a ride. The point of the story is that she had the capital to relieve her suffering sitting right under her nose. And that she was stunned that the currency had lost that much purchasing power. She had an 1854 one dollar gold coin that contained $67 worth of gold. I told her to take it to a coin dealer and didnāt buy it because it probably had more numismatic value than the gold it contained - $67 fake paper dollars for a one dollar gold piece.
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Here is one of my first posts on the goldrefiningforum.com back in Oct 2010. I became interested in refining and accidentally stumbled on this forum. Notice how I am asking these guys about refining gold plated scrap with aqua regia - sound familiar?
One experienced refiner, Nick, told me to stop because trying to refine the tiny micro bit of gold plated from this material would NOT WORK.
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A WORD ABOUT TIN PASTE (meta-stannic acid)
Tin that dissolves in nitric acid forms a thick paste that will bind metals and cause loss of metals. It usually comes from repairs done to fine jewelry with soft solder. Soft solder is an alloy of tin and lead. The tin paste, or meta stannic acid, is the consistency of elmers glue and will clog filter papers making filtering impossible. Iāve encountered it while refining gold filled material. Itās a whitish jelly that traps metal foils and makes their recovery difficult. To remedy I used hot sulfuric acid to try to dissolve the tin paste. Itās slow, and silver will also dissolve, but it is a way to rid your gold foils of the troublesome compound. I had to do several sulfuric acid boils to get rid of it completely. I boiled the foils in hot concentrated sulfuric acid, allowed it to cool, poured it off, and boiled again. Each time the amount of the paste decreased.
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A WORD ABOUT REFINING PLATINUM GROUP METALS
For a trained chemist not familiar with separating the six sister metals in the platinum group, a clean separation is not possible (even the refiner well experienced with PGMs a clean separation is difficult). For the non chemist - forget it. These metals are so much alike that they follow each other through the refining process. Palladium is soluble in nitric, platinum is not. This would lead one to conclude that a simple nitric boil will remove all the palladium from a Pd Pt mix. But not so. Even after full nitric boil for hours, there will still be some palladium left in the platinum and some of the platinum will be in the palladium. The only process that I know of to give a clean separation of platinum from the others is a bromate hydrolysis, developed by Raleigh Gilcrest. Impure platinum sponge is dissolved then a saturated sodium bromate solution is injected slowly. The bromate forms metal hydroxides of other PGMs, if present. Platinum, not forming a hydroxide, is left in the mother liquor, and can then be isolated and precipitated making very high purity platinum sponge. Nitric wonāt dissolve gold, yet Iāve seen gold in solution with just nitric boils. Platinum wonāt be affected by HCl yet Iāve seen platinum go into solution in hot hydrochloric acid. Also, platinum will dissolve completely in hot dilute nitric acid if it is alloyed with 95% silver.
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FIVE PART 25 TROY OUNCE BAR SERIES
This series was fraught with problems. I had to redo the end screen because I left my pistol on the table and had on the wrong hat in the end screen. Iāve corrected the video and reposted it. Sorry for the confusion.
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A WORD ABOUT UREA
I get many viewers asking me why I donāt add urea to the gold solution before I precipitate with SMB. I guess years ago, folks added urea to try to kill the excess nitric in their gold solutions. I did it when I first started refining back in 2010. But then Butcher, on the goldrefiningforum.com, used stoichiometry to show me that it doesnāt even work. The nitric, according to his equation, remained after the urea was added. The pros on the forum just donāt use it. Instead, they taught me to use incremental nitric dosing; adding small doses of nitric until the all the gold dissolves. If done properly there wonāt be any excess nitric to remove. But if I do over-shoot with nitric additions then I remedy the excess nitric by adding a few extra spoons of SMB. Premixing aqua regia three to one, or four to one just isnāt done any more. But if we do add too much nitric and we want to get it out of the gold solution then we add sulfamic acid, not urea. Premixing aqua regia and adding urea are two antiquated refining techniques that are not used by modern refiners. Even Hokeās book never once even mentions urea. She used the classic reduction to a syrup and rehydration with hydrochloric to rid the chloroauric acid solution of excess nitric. Just think of it, it only took me 230ml of nitric to dissolve 23 Troy ounces of gold completely. If I had pre-mixed the aqua regia three to one or even four to one, then Iād still be out in my shop right now trying to precipitate that gold!
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TWENTY FIVE OUNCE BAR IS COMING
Patience. Did you see all the junk that got filtered out in part four? Refining this much gold takes a long time. And it takes a toll on the refiner. Iāve been up till 4am two nights in a row refining, shooting and editing the video. I was up until 3am Friday morning and then had to take Mrs sreetips to estate sales early that morning. Iāve only gotten about 18 hours sleep in the last four days. It wipes me out. Iāve been in bed for two days trying to recover. Nothing worse than going out in my shop half baked and worn out. Cause me to take short cuts and possibly ruin the series. I took Friday and Saturday off. Had to. I should be fresh as a daisy by Sunday and Iāll get that bar posted Sunday night or early Monday morning.
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Demonstrations of precious metals refining techniques that I have developed since starting back in September of 2010. It began as a hobby and still is to this day for the most part. I am just an advanced beginner. I enjoy making these videos. I wish videos like these were available back when I first started. Please enjoy and be safe! I will try to answer any questions that you have about any of these processes. I enjoy helping people!
Any references to using or making illegal drugs will be promptly deleted.
Please refrain from using offensive language in the comment section. I would request that a suitable environment be maintained for people of all ages to view and learn about precious metals refining.