This project is scary but intriguing. I cant imagine how much more difficult and thought out the process would be in a sealed fume hood. Looking forward to part 3.
Every time I watch one of your videos I’m silently impressed by the sheer competence you display with your basic laboratory skills. It’s wonderful to watch a master at work. 😊
Please be safe. I know you're very careful, so I'm only a little worried. You work so hard to provide us with this educational (and entertaining) content, thank you.
I've not been able to sleep and I've just been watching hours of your metal and gold refining and I love it so much!! I've always loved chemistry and hope I can try my hand at refining some day. Keep up the work
I want to say you are a good person not just because you share the process of refining but because you are conscientious of handling the toxic and treating it so it does not get poured into the sewer system and poison the environment. I'm not a tree hugger nor an environmentalist but I do care about how the environment should be cared for.
From my experience you actually don't need that much ammonium chloride. In order to precipitate hexachloroplatinic acid as ammonium hexachloroplatinate you actually only need a stoichiometric amount of ammonium chloride, so 2 mols per mol dissolved platinum. This will cause almost all the platinum to precipitate as ammonium hexachloroplatinate. A small amount will still remain in solution, since the solubility of that salt is 7g/L water at 15°C. Using saturated ammonium chloride solution would probably decrease it's solubility due to the common ion effect, so you'll get a tiny bit more precipitate. But instead I added ethanol to the solution (about 2 times it's volume) which crashed out practically all the ammonium hexachloroplatinate. There was no yellow color left in the solution and my yield was pretty much quantitative. I also added hydrazine sulfate to the filtrate which would reduce any hexachloroplatinate to metallic platinum and I saw nothing. For this method the solution should be relatively concentrated though, otherwise you'll waste a lot of ethanol. And nickel would make a light green color, and this procedure would have removed it. The extremely dark red color of the solution after dissolving the precipitate also indicates iridium. The only other platinum group metals that have such an intense color in solution are palladium and probably rhodium, and you've already ruled out palladium and it's also for sure not rhodium. Iridium is the only thing that makes sense to me, since it also said 90% Pt 10% Ir on the rings. Separating platinum from iridium seems like a very difficult task, maybe I can see if I could find some information about that.
Conner is here and I'm sharing your videos with all my good people hoping somebody will launch this with me. I want your job! Great service your doing.
Conner, I’m on the gold standard. You can go on it yourself. You don’t need to wait for someone to do it for you. Paper dollars are declining. Gold and silver are rising. Paper dollars can printed into existence. Gold and silver can’t be printed. The dollar is a Ponzi and it requires third-party validation. Gold and silver are real money and need no third-party validation, they stand on their. Which would you rather use to store your savings? And the best part: nobody knows you’ve got it, unless you tell them. If you need paper to pay bills or buy food, then sell a little of your metal.
Hey Sreetips, thanks for the great content. I watch all your videos and really appreciate the work you put into it. You have taught me and many others quite a bit. That's a difficult thing to do and you do it well. God bless you and your family!
You asking us to please understand your level of competency with refining certain metals int something u have to say we all watch and appreciate the job u do and seeing you learn as u go is an awesome watch the process and your ability to solve the issues calmly is amazing your always so full of information while being humble and honest with your viewers and for that I will always love watching the content
4:20 Cut the coffee filters to fit the bottom of the Buchner funnel. The edges will always lift, preventing a proper seal. HCL doesn't affect coffee filter paper, yet double the paper to prevent pin hole pull through.
I just listened to you about the 5 troy ounces you sold I believe what your saying I'm collecting some silver and gold but more copper brass and bronze and aluminum but working towards more silver and gold thank you for your knowledge your amazing
When I buy metals, I’m not expensing. Food is an expense, gasoline, clothes, light bill, water, almost everything else is an expense and i’ll never see another nickel of it ever again. Not so with precious metals. Precious metals are not an expense. When I buy metal, what i’m actually doing is trading paper, that’s declining, for metal, that’s rising. In my opinion (I’m not trying to give you financial advice) I can’t go wrong buying precious metals. Not as an investment, but rather as insurance against the declining paper dollars. Storing wealth in metal protects me from those who plunder the savers. They can’t print more gold and silver.
I Enjoy seeing you encounter something new, I’m not familiar at all with the iridium contamination but I suspect that is what is making your precipitate pink
I look forward to your next video I find your science projects fascinating, science was never my strong suit in school but as I get older you have brought some interest back, thank you for all your hard work. Happy New Year to you both.
To help improve your safety .... I was thinking you could build a removable Plate to cover the front of your fume hood with sand blasting type pass though gloves ... or you could chop up a HF sandblaster... Just 2 cents worth ... great job!!
Very interesting series, me Sreetips :) I'm avidly following how you manage the refinement of the (dangerous) Platinum metal... one thing I noticed is, how much effort it takes to refine a tiny amount of 10+ grams as compared to gold. Also, yes a stirbar is basically a neodymium magnet surrounded by a chemically neutral coating and those magnets can fail over time as they go through several heating/cooling cycles. The magnetic medium can't really take those repeated temperature swings without (slowly) losing their magnetivity... in other words, the more frequent you'll subject your magnetic stirbars to heating cycles the quicker you'll have to replace them Fun Fact: "cooking" something in a bath of hot water is also called "Au bain Marie" by the French :)
The leftovers could also contain ruthenium and cobalt since both are used to make platinum alloys for jewelry. Not sure if iridium is used more often. Iridium is rare. Also, most iridium salts/oxides are green or black. Cobalt nitrate is a possible when it comes to color. This salt is red/brown. Hard to see anything ruthenium in there because most of those oxides you would see in there are black unless you snuck in some fluorine. Cobalt is the cheapest. 😉
You’re welcome. It is quite the feat to plow through this refine. Gold is described as “God excrement” in an ancient tongue, it wouldn’t be incorrect to say platinum is “devil excrement”. Thank you Sir!👍👍🤟
15:00 I've looked up "cement" for a definition for the way you are using it, but I can't find any definition that makes sense. Do you mean "precipitate"? Or are you referring to a different chemical process? It's been a long time since I studied chemistry! Thanks!
Cementing is a term used in the refining community to describe the reaction of metals coming out of solution on another metal that’s more reactive than the metal being cemented. Silver is less reactive than copper. So if I put a piece of copper (more reactive) into a silver nitrate solution, the silver (being less reactive) will “cement” out on the copper as the copper goes into solution. Please see “Reactivity Series of Metals” for more on this.
@@sreetips Thank you for explaining the term! I will watch that series. Now I can also search for the term more effectively, too, for more information.
I hesitate to make any comment on the process because I don’t have any experience with PGMs and no recent experience with gold or silver. But I think you could probably start with considerably more of the solute medium ( distilled water or HCl). It seems that the medium frequently becomes saturated before the Nitric is consumed, stalling the reaction. At the end of each process, if the concentration needs to be increased, you could always evaporate. But in most cases you need to dilute, so it probably wouldn’t be a problem or increase the volume of your waste stream. Just a thought. I’m really enjoying watching this series. Happy New Year, Chief 🎉
Interesting suggestion Ed. I'm thinking that the limiting factor is more likely the surface area of the platinum. Platinum is the most ductile of all metals and is second only to gold in its malleability. My suggestion would be to run the metal strips through the sheet forming mill several times after heat treating it to reduce any work hardening.
@@roberthayward9299 it’s not actually heat treating. He’s just incinerating to remove any remaining organic contaminants. Saturation will stall the reaction with any metal. The solute can only hold so much and when it reaches that point, no amount of Nitric or surface area will make it continue. Adding more of the solute medium will, however, restart a stalled reaction. I know it doesn’t matter all that much when he is processing inquarted gold because of the concurrent silver refining, but other processes may benefit from increased solute medium.
@@CuttinEJ Sreetips has done exactly that on some of his gold refining videos. He added more HCl when the reaction stopped, rather than more HNO3. One of the dissolution steps (2nd? 3rd?) produced a lot of brown fumes when poured into the temporary stock pot. That is a sure sign that more non-HNO3 solute is needed.
I have learned so much from your videos and starting to LOL because your fails WILL SAVE ME A WHOLE LOT OF CUSSING when I refine. So a couple of questions. 1) Have you Acid washed beakers & flasks b4 use? 2) would De ionized water help the chemical process be more successful? My environmental Chemistry knowledge from back in 1995 which I haven't used since then....we used filtered DI water for EVERYTHING. ACID washed containers for the Chemistry that needed it. Also good Chemistry hygiene: NO OBJECTS IN CHEMICAL CONTAINERS! THE CHEMICALS CAN BE CONTAMINATED!!!! POUR CHEMICALS IN2 ANOTHER CONTAINER then scoop them out.😎. ASLO.....DO NOT PLACE ENTIRE PACK OF FILTER PAPER IN HOOD!!!!!!!! THEY MAY BE GETTING CONTAMINATED!!!!! I winched when you used your "dirty gloves" to grab filter paper, which the box was in hood, next to beaker that could have splashed fluid on filter box contaminating WHOLE BOX. WHAT WAS ON YOUR GLOVES WHEN YOU GRABBED THE FILTER PAPER? Please please please 🙏 leave filter box out of hood, do not let contaminated gloved hands touch stack of papers in the future. Use tweezers or pre assemble filter paper in funnel. I believe if you re establishe GOOD CHEMISTRY HYGIENE PRACTICES. ⚗️ OH L👀K the emoji has copper in it! Just want to end this by saying YOU ROCK AND ARE TICKLING MY BRAIN CELLS! 💖😎
1) no. 2) I use distilled water contaminants measured in parts per million. Except for chlorine, tap water is ppm also. Not enough to report in a PM assay. The other stuff, thanks for pointing it out.
So what and how do you wash all the Pyrex and corning ware that you us? Dishwasher or just use distilled water? Do the chemicals not screw with the GoPros or they always outside the fume hoot?
I watch a streamer that does a lot of fishing streams out of Australia and the salt water and air kills his cameras quick. Mainly the connections on the the battery packs. And happens faster than you think I can imagine that acid does it quicker.
How do you clean your beakers? Do you use soap and water? And where? You use so many chemicals, are you able to do them in a normal kitchen sink or do you have a special process?
If you have such clean wastes from this process it would be better to use zinc/aluminum to drop PGM, and filter than mixing it with copper - just my 3 cents. I use cotton wool pressed into plastic funnel to catch precious particles on wool. If there are basic metal in solution - they can be removed with formic precipitation [at least partially]. pH increase rate is key for this, and bromate hydrolysis too. I admire you spend so many hours on that.
Hello there , I refined 6 kg 14 carats. I added 60 ml of sulfuric acid to the king water. I had to buy 3630 gr has. 160 grams was missing. Does sulfuric acid damage gold? I would be very happy if you provide information.
We are thinking that we would like to attempt gold refining ourselves. I was wondering if you could tell me where you get your supplies. The beakers, glass acid bottles, pipettes, funnels, etc. I’ve found some stuff on Amazon, but as we all know, some of the quality of the things on there can be suspect, and if I’m going to be messing with acids and other scary chemicals I’d like to have stuff I know won’t fall apart at the first drop of chemicals in it.
First, get a fume hood. No way to do reactions safely without one. I buy all my glassware on eBay. I buy most of my chemicals from Ace Hardware, and eBay.
To all the people mentioning iridium, I'll go out on a limb here and say it's almost definitely not an iridium salt. Iridium hates to go into solution even in aqua regia and in fact that was how it was discovered in the early 1800s. It was the insoluble residue after dissolving platinum for ages. As it happens, that was probably a combination of both iridium and osmium but the scientist at the time correctly concluded it was a different metal from platinum. The amount of iridium metal was pretty small; only 10% of one ring which probably weighed say 3 grams maximum, so it would only be 300mg of metal and that would have been most of what was left after all the AR boils. When sreetips concentrated the dihydrogen hexachloroplatinate on the hot plate without the stir bar working, he would have put enough heat into that viscous liquid (approx 350 degrees C) to drive off a couple of chloride ions which bond with free H+ ions to form HCl and reduced the anion to the Pt(II) oxidation state... tetrachloroplatinate (2-) which is a weird one. Then the PtCl4 was in the hydrate form before the ammonium chloride was added, and thereafter the ammonium ions dissociated and formed ammonium tetrachloroplatinate salt which is the evil strawberry milkshake! :). Search online - the color looks exactly right. The fact it happened twice is pretty much confirmation that's what occurred but it won't matter - calcining is the right way to go, albeit turning a really valuable precursor for medical experiments into a slightly less valuable metal button.
After dissolving the metals he got a clear solution, so the iridium has to be in solution, where else should it have gone? And it's already apparent that iridium is going in solution while he was dissolving it due to the intensely dark red color the solution had, you couldn't even see through that. Hexachloroplatinic acid isn't that dark, it is orange and even a concentrated solution like 30% isn't that strongly colored. Iridium might be extremely resistant as a pure metal, but if it's 10% in an alloy it's a different story. You also have this with platinum, pure platinum isn't soluble in nitric acid, but if you dissolve an alloy of 95% palladium and 5% platinum in nitric acid all of it will go into solution.
@@alexanderkroboth3310 Agreed, it could well be - certainly makes some sense, but there was still some metal left undissolved after the 12 hours of multiple intense boils. Iridium ,if you can get it in solution, forms coordination complexes which from my (granted hazy) memory aren't overly understood and can display just about any colour depending on the structure. I remember this as my inorganic professor was a world expert in developing Pt and Ir complexes as anti-cancer treatments. I however was a lowly student so take my suggestion with a grain of Pt salt. Cheers and thanks for the reply.
@@AndyGraceMedia In that alloy the iridium was evenly mixed with the platinum, so if it would dissolve away all the platinum and leave the iridium behind you should end up with a powder or some spongy metal like how you have when dissolving the silver out of inquarted gold, but these were solid pieces of metal. And in Aqua regia, which is mostly HCl you'll have the hexachloroiridate complex, which has a dark red color. Anyway, thanks as well, have a nice day.
Love all your content! This platinum thing though... Seems nasty and difficult to work with. Don't want anything bad to happen to you. Take care with this stuff!
when did you add the sodium bromate because that step is what is supposed to seperate out the Pt from the Ir and it is done during the time that both are in solution (dark black). to seperate out the iridium while leaving the Pt behind in solution. pure chloroplatinic acid is dark red in color.
On your waste solutions, when it gets to the acidic iron solution, what do you do with that? Baking soda to neutralize it and down the drain? Do you have to take it to someone for disposal?
It is really strange for me. In like 95% of your videos you usually do almost the same stuff, but nevertheless I'm always waiting to see another one. :) So you know... a little dosage of something new is even more interesting no matter your experience. We all learn from your mistakes. Cheers!
The the magnetic stirrer wears out. Googling for "magnet experiments what happens when a magnet is heated" you will get the explanation: "When heated above 176° Fahrenheit (80° Celsius), magnets will quickly lose their magnetic properties. The magnet will become permanently demagnetized if exposed to these temperatures for a certain length of time or heated at a significantly higher temperature (Curie temperature)."
I have been curious for a while now but if you have all that cement silver and pure silver crystals, why do you use antique silverware and other utensil's to enquart gold? why not just use the cement silver or even the pure crystals?
Palladium will build up in the cement silver if it’s used over and over. Pure silver crystal has already been through the silver cell - like taking a step backwards.
У автора видео чётко выпал гексахлорпалладат аммония. То что диметилглиоксим не сработал, свидетельствует о том что палладий был в степени окисления +4 в то время как дмг работает только с 2 валентным палладием. Судя по цвету осадка красного, там больше 90% хлорпалладата аммония и возможно примесью платины. Иридия судя по цвету нет, так как если бы он был в растворе то с хлористый аммонием дал бы чёрные игольчатые кристаллы отлично различимые даже в такой каше.
I read that you can supposedly seperate pt from iridium by disolving the platinum from the mixed salts in dilute AR on gentle heat. It should leave metallic iridium behind. I'm not sure what exactly dilute means. Maybe you had some of it on the first run, just before you were going to filter it? I dunno. Good effort tho. You'll get it figured out, I'm sure.
No matter how careful, some of the Pt would get left behind with the iridium. And some of the iridium would follow the platinum and go in solution. That’s the nature of these six sister metals (platinum, palladium, rhodium, iridium, Osmium, ruthenium). They hate to be separated. They don’t cooperate. I’m afraid that I’m in deep water with this series. Maybe I should have left it alone.
I found that my magnetic stirs like that will lose their magnetivity when heated over a certain temperature. They make high temperature magnetic stirs which can handle a little more heat
Anyone planning on recovering and refining platinum from catalytic converters should really think twice about the amount of time chemicals and hazards.
What you mean is that industrial Zinc contains palladium, but there is no rate per kilogram, only how it is processed. As a lab man you are amazing but the metallurgical tricks are missing if you take the zinc for an estimated time in an induction furnace that reaches the stable temperature 1°C below . When the zinc boils, it begins to oxidize and becomes a metallic gas that can later be catalyzed in water and leaves palladium, platinum and rhodium as residues. For this reason, old zinc is so expensive due to the high content of platinum group metals in naval scrap yards there are thousands of buyers of this Zinc from ingots (Bota Mar).
Interesting it's pink when iridium hexachloride trihydrate is green/black. Through hexachloroplatinic acid is noted as reddish brown, it would have made sense for the iridium to have darkened rather than lightened the precipitate.
The other stir bar is too small for that beaker. The new one works, but you'd be guaranteed to keep the precipitate suspended the whole time if you had a stir bar that was 35mm or longer.
I know. But in my experience, I’ve seen many things happen that weren’t supposed to. And many thing that weren’t supposed to happen, happen. A 90/10 Pt/Ir alloy - everything dissolves in hot AR. Also, a 95/5, silver/Pt alloy - everything dissolves in hot nitric. I’ve seen hot hydrochloric dissolve small amounts of platinum. I’ve put gold in solution with boiling nitric. These hard and fast rules can all be broken. It’s an enigma.
On the other hand, if I tried to dissolve a piece of iridium in boiling aqua regia then nothing would happen. It would probably just sit there, looking back at you, unaffected. And that’s where the hot AR/Ir rule comes from.
@@sreetips That's one of the reasons that I love your channel. You do the experiments to determine what actually happens. I'll look around to see what I can learn.
Here is an excerpt from nvlpubs.nist.gov/nistpubs/ScientificPapers/nbsscientificpaper483vol19p325_A2b.pdf The authors formed an alloy of the Pt/Ir sample with Pb by fusion. They then dissolved away the lead using nitric and then aqua regia. The complete procedure is in the paper, which is from the 1920's. "In his researches on platinum-iridium alloys Deville discovered that when he dissolved in lead at a high temperature platinum alloyed with iridium, rhodium, palladium, iron, and copper he was able to effect a very distinct separation of the platinum metals. The lead formed alloys with all of the platinum, rhodium, palladium, and copper and with a very small proportion of the iron. The iridium, ruthenium, and iron formed a separate alloy containing no lead. Boiling dilute nitric acid removed the bulk of the lead, together with the palladium and copper and a small proportion of the platinum and rhodium. Digestion' of the residue with warm dilute aqua regia left insoluble only the alloy of iridium, ruthenium, and iron."
This operation is very dangerous, but it was a wonderful job, and I take my hat off to you for the efforts you made for your viewers.
This project is scary but intriguing. I cant imagine how much more difficult and thought out the process would be in a sealed fume hood.
Looking forward to part 3.
Every time I watch one of your videos I’m silently impressed by the sheer competence you display with your basic laboratory skills. It’s wonderful to watch a master at work. 😊
Please be safe. I know you're very careful, so I'm only a little worried. You work so hard to provide us with this educational (and entertaining) content, thank you.
I've not been able to sleep and I've just been watching hours of your metal and gold refining and I love it so much!! I've always loved chemistry and hope I can try my hand at refining some day. Keep up the work
Excellent, thank you.
I want to say you are a good person not just because you share the process of refining but because you are conscientious of handling the toxic and treating it so it does not get poured into the sewer system and poison the environment. I'm not a tree hugger nor an environmentalist but I do care about how the environment should be cared for.
Thanks for explaining the waste treatment some more, it's very much appreciated.
From my experience you actually don't need that much ammonium chloride. In order to precipitate hexachloroplatinic acid as ammonium hexachloroplatinate you actually only need a stoichiometric amount of ammonium chloride, so 2 mols per mol dissolved platinum. This will cause almost all the platinum to precipitate as ammonium hexachloroplatinate. A small amount will still remain in solution, since the solubility of that salt is 7g/L water at 15°C. Using saturated ammonium chloride solution would probably decrease it's solubility due to the common ion effect, so you'll get a tiny bit more precipitate. But instead I added ethanol to the solution (about 2 times it's volume) which crashed out practically all the ammonium hexachloroplatinate. There was no yellow color left in the solution and my yield was pretty much quantitative. I also added hydrazine sulfate to the filtrate which would reduce any hexachloroplatinate to metallic platinum and I saw nothing. For this method the solution should be relatively concentrated though, otherwise you'll waste a lot of ethanol.
And nickel would make a light green color, and this procedure would have removed it. The extremely dark red color of the solution after dissolving the precipitate also indicates iridium. The only other platinum group metals that have such an intense color in solution are palladium and probably rhodium, and you've already ruled out palladium and it's also for sure not rhodium. Iridium is the only thing that makes sense to me, since it also said 90% Pt 10% Ir on the rings. Separating platinum from iridium seems like a very difficult task, maybe I can see if I could find some information about that.
How can he test for iridium?
It’s all way over my head. This has turned my enjoyable hobby into real work. Thanks for the input.
@@GokouZWAR I don't know a qualitative test for Iridium, but by how it looks you can be quite sure it's Iridium. It also said that on the rings.
Conner is here and I'm sharing your videos with all my good people hoping somebody will launch this with me. I want your job! Great service your doing.
Bringing gold back to our economy
Conner, I’m on the gold standard. You can go on it yourself. You don’t need to wait for someone to do it for you. Paper dollars are declining. Gold and silver are rising. Paper dollars can printed into existence. Gold and silver can’t be printed. The dollar is a Ponzi and it requires third-party validation. Gold and silver are real money and need no third-party validation, they stand on their. Which would you rather use to store your savings? And the best part: nobody knows you’ve got it, unless you tell them. If you need paper to pay bills or buy food, then sell a little of your metal.
Hey Sreetips, thanks for the great content. I watch all your videos and really appreciate the work you put into it. You have taught me and many others quite a bit. That's a difficult thing to do and you do it well. God bless you and your family!
You asking us to please understand your level of competency with refining certain metals int something u have to say we all watch and appreciate the job u do and seeing you learn as u go is an awesome watch the process and your ability to solve the issues calmly is amazing your always so full of information while being humble and honest with your viewers and for that I will always love watching the content
I enjoy your channel and appreciate the wisdom you share. Thank you
You must truly enjoy refining to put yourself through this for us to watch. Thank you sreetips!
4:20 Cut the coffee filters to fit the bottom of the Buchner funnel.
The edges will always lift, preventing a proper seal.
HCL doesn't affect coffee filter paper, yet double the paper to prevent pin hole pull through.
I just listened to you about the 5 troy ounces you sold I believe what your saying I'm collecting some silver and gold but more copper brass and bronze and aluminum but working towards more silver and gold thank you for your knowledge your amazing
When I buy metals, I’m not expensing. Food is an expense, gasoline, clothes, light bill, water, almost everything else is an expense and i’ll never see another nickel of it ever again. Not so with precious metals. Precious metals are not an expense. When I buy metal, what i’m actually doing is trading paper, that’s declining, for metal, that’s rising. In my opinion (I’m not trying to give you financial advice) I can’t go wrong buying precious metals. Not as an investment, but rather as insurance against the declining paper dollars. Storing wealth in metal protects me from those who plunder the savers. They can’t print more gold and silver.
I Enjoy seeing you encounter something new, I’m not familiar at all with the iridium contamination but I suspect that is what is making your precipitate pink
Hello Mrs and Mr sreetips. You did the woork yust fine sir. I was supricing to how muth solids it was. Stay safe my friend. Great clip. Arne
What a difference in technique it takes to refine platinum and gold. Great videos so far and it's very interesting.
Makes me even more interested in platinum
Super cool seeing the drying out at the end.
This reaffirm that it's not worth it for a hobby refiner thank you for sharing this with us I have learned a lot from you six stars brother
Always intrigued on your process of what you do. Keeps me interested.
Really fascinating and I'm looking forward to seeing part 3. 👍
what a task. Love your drive Sir!
Also, great job and thanks. This series has been a nice surprise. I always enjoy watching your channel.
I look forward to your next video I find your science projects fascinating, science was never my strong suit in school but as I get older you have brought some interest back, thank you for all your hard work. Happy New Year to you both.
To help improve your safety .... I was thinking you could build a removable Plate to cover the front of your fume hood with sand blasting type pass though gloves ... or you could chop up a HF sandblaster... Just 2 cents worth ... great job!!
Very interesting series, me Sreetips :) I'm avidly following how you manage the refinement of the (dangerous) Platinum metal... one thing I noticed is, how much effort it takes to refine a tiny amount of 10+ grams as compared to gold. Also, yes a stirbar is basically a neodymium magnet surrounded by a chemically neutral coating and those magnets can fail over time as they go through several heating/cooling cycles. The magnetic medium can't really take those repeated temperature swings without (slowly) losing their magnetivity... in other words, the more frequent you'll subject your magnetic stirbars to heating cycles the quicker you'll have to replace them
Fun Fact: "cooking" something in a bath of hot water is also called "Au bain Marie" by the French :)
The leftovers could also contain ruthenium and cobalt since both are used to make platinum alloys for jewelry. Not sure if iridium is used more often. Iridium is rare. Also, most iridium salts/oxides are green or black.
Cobalt nitrate is a possible when it comes to color. This salt is red/brown.
Hard to see anything ruthenium in there because most of those oxides you would see in there are black unless you snuck in some fluorine.
Cobalt is the cheapest. 😉
im loving this series so much! thank you for explaining how dangerous is all this, i learn a lot from your videos
This appears to be 100x's more difficult than Au. Crazy... I enjoy watching
It’s grueling. I don’t know why I chose to do it. I’m in over my head.
You’re welcome. It is quite the feat to plow through this refine. Gold is described as “God excrement” in an ancient tongue, it wouldn’t be incorrect to say platinum is “devil excrement”. Thank you Sir!👍👍🤟
15:00 I've looked up "cement" for a definition for the way you are using it, but I can't find any definition that makes sense. Do you mean "precipitate"? Or are you referring to a different chemical process? It's been a long time since I studied chemistry! Thanks!
Cementing is a term used in the refining community to describe the reaction of metals coming out of solution on another metal that’s more reactive than the metal being cemented. Silver is less reactive than copper. So if I put a piece of copper (more reactive) into a silver nitrate solution, the silver (being less reactive) will “cement” out on the copper as the copper goes into solution. Please see “Reactivity Series of Metals” for more on this.
@@sreetips Thank you for explaining the term! I will watch that series. Now I can also search for the term more effectively, too, for more information.
I hesitate to make any comment on the process because I don’t have any experience with PGMs and no recent experience with gold or silver. But I think you could probably start with considerably more of the solute medium ( distilled water or HCl). It seems that the medium frequently becomes saturated before the Nitric is consumed, stalling the reaction. At the end of each process, if the concentration needs to be increased, you could always evaporate. But in most cases you need to dilute, so it probably wouldn’t be a problem or increase the volume of your waste stream. Just a thought. I’m really enjoying watching this series. Happy New Year, Chief 🎉
Interesting suggestion Ed. I'm thinking that the limiting factor is more likely the surface area of the platinum. Platinum is the most ductile of all metals and is second only to gold in its malleability. My suggestion would be to run the metal strips through the sheet forming mill several times after heat treating it to reduce any work hardening.
@@roberthayward9299 it’s not actually heat treating. He’s just incinerating to remove any remaining organic contaminants. Saturation will stall the reaction with any metal. The solute can only hold so much and when it reaches that point, no amount of Nitric or surface area will make it continue. Adding more of the solute medium will, however, restart a stalled reaction. I know it doesn’t matter all that much when he is processing inquarted gold because of the concurrent silver refining, but other processes may benefit from increased solute medium.
@@CuttinEJ Sreetips has done exactly that on some of his gold refining videos. He added more HCl when the reaction stopped, rather than more HNO3.
One of the dissolution steps (2nd? 3rd?) produced a lot of brown fumes when poured into the temporary stock pot. That is a sure sign that more non-HNO3 solute is needed.
This is the first I've seen this, amazing dude I can't to see the final video. Love what you do.
This is fascinating! I cannot wait to see part 3!
All these things you refine are fascinating. Thanks for the vlogs Yeshua Is The Way, The Truth and The life. Prayers for our world.
And thankfully so. I can’t imagine being stuck here forever. There’s an end to this madness called “life on earth.”
I have learned so much from your videos and starting to LOL because your fails WILL SAVE ME A WHOLE LOT OF CUSSING when I refine. So a couple of questions. 1) Have you Acid washed beakers & flasks b4 use? 2) would De ionized water help the chemical process be more successful? My environmental Chemistry knowledge from back in 1995 which I haven't used since then....we used filtered DI water for EVERYTHING. ACID washed containers for the Chemistry that needed it. Also good Chemistry hygiene: NO OBJECTS IN CHEMICAL CONTAINERS! THE CHEMICALS CAN BE CONTAMINATED!!!! POUR CHEMICALS IN2 ANOTHER CONTAINER then scoop them out.😎. ASLO.....DO NOT PLACE ENTIRE PACK OF FILTER PAPER IN HOOD!!!!!!!! THEY MAY BE GETTING CONTAMINATED!!!!! I winched when you used your "dirty gloves" to grab filter paper, which the box was in hood, next to beaker that could have splashed fluid on filter box contaminating WHOLE BOX. WHAT WAS ON YOUR GLOVES WHEN YOU GRABBED THE FILTER PAPER? Please please please 🙏 leave filter box out of hood, do not let contaminated gloved hands touch stack of papers in the future. Use tweezers or pre assemble filter paper in funnel. I believe if you re establishe GOOD CHEMISTRY HYGIENE PRACTICES. ⚗️ OH L👀K the emoji has copper in it! Just want to end this by saying YOU ROCK AND ARE TICKLING MY BRAIN CELLS! 💖😎
1) no. 2) I use distilled water contaminants measured in parts per million. Except for chlorine, tap water is ppm also. Not enough to report in a PM assay. The other stuff, thanks for pointing it out.
Thank you for doing this. So far this is making a platinum eagle look like a bargain at todays price.
This is a terrifying process. I don’t think I’d be messing with platinum much if I was doin this stuff.
You make pretty colours. Mad respect. Thank you.
How do you clean the "dishes"?
Have you considered leaving a glass rod in the beaker to control the splash from pouring?
Rinse with distilled water then scrub with alconox.
So what and how do you wash all the Pyrex and corning ware that you us? Dishwasher or just use distilled water? Do the chemicals not screw with the GoPros or they always outside the fume hoot?
The solutions are acidic and rinse right out with water. After a while, the GoPro will fail from those acid fumes.
I watch a streamer that does a lot of fishing streams out of Australia and the salt water and air kills his cameras quick. Mainly the connections on the the battery packs. And happens faster than you think I can imagine that acid does it quicker.
How do you clean your beakers? Do you use soap and water? And where? You use so many chemicals, are you able to do them in a normal kitchen sink or do you have a special process?
Acidic solutions rinse clean with water. Then I scrub with alconox and air dry.
the stir bars can get demagnetized over time, especially when they are heated, but that will take time.
If you have such clean wastes from this process it would be better to use zinc/aluminum to drop PGM, and filter than mixing it with copper - just my 3 cents. I use cotton wool pressed into plastic funnel to catch precious particles on wool.
If there are basic metal in solution - they can be removed with formic precipitation [at least partially]. pH increase rate is key for this, and bromate hydrolysis too.
I admire you spend so many hours on that.
A charmin plug. The copper in my stock pot is a “catch-all”
Hello there ,
I refined 6 kg 14 carats.
I added 60 ml of sulfuric acid to the king water.
I had to buy 3630 gr has.
160 grams was missing.
Does sulfuric acid damage gold?
I would be very happy if you provide information.
No, sulfuric should not damage the gold.
We are thinking that we would like to attempt gold refining ourselves. I was wondering if you could tell me where you get your supplies. The beakers, glass acid bottles, pipettes, funnels, etc. I’ve found some stuff on Amazon, but as we all know, some of the quality of the things on there can be suspect, and if I’m going to be messing with acids and other scary chemicals I’d like to have stuff I know won’t fall apart at the first drop of chemicals in it.
First, get a fume hood. No way to do reactions safely without one. I buy all my glassware on eBay. I buy most of my chemicals from Ace Hardware, and eBay.
@@sreetips thank you for replying. I’ll definitely check eBay. Didn’t even think about that.
To all the people mentioning iridium, I'll go out on a limb here and say it's almost definitely not an iridium salt. Iridium hates to go into solution even in aqua regia and in fact that was how it was discovered in the early 1800s. It was the insoluble residue after dissolving platinum for ages. As it happens, that was probably a combination of both iridium and osmium but the scientist at the time correctly concluded it was a different metal from platinum.
The amount of iridium metal was pretty small; only 10% of one ring which probably weighed say 3 grams maximum, so it would only be 300mg of metal and that would have been most of what was left after all the AR boils.
When sreetips concentrated the dihydrogen hexachloroplatinate on the hot plate without the stir bar working, he would have put enough heat into that viscous liquid (approx 350 degrees C) to drive off a couple of chloride ions which bond with free H+ ions to form HCl and reduced the anion to the Pt(II) oxidation state... tetrachloroplatinate (2-) which is a weird one. Then the PtCl4 was in the hydrate form before the ammonium chloride was added, and thereafter the ammonium ions dissociated and formed ammonium tetrachloroplatinate salt which is the evil strawberry milkshake! :). Search online - the color looks exactly right.
The fact it happened twice is pretty much confirmation that's what occurred but it won't matter - calcining is the right way to go, albeit turning a really valuable precursor for medical experiments into a slightly less valuable metal button.
After dissolving the metals he got a clear solution, so the iridium has to be in solution, where else should it have gone? And it's already apparent that iridium is going in solution while he was dissolving it due to the intensely dark red color the solution had, you couldn't even see through that. Hexachloroplatinic acid isn't that dark, it is orange and even a concentrated solution like 30% isn't that strongly colored. Iridium might be extremely resistant as a pure metal, but if it's 10% in an alloy it's a different story. You also have this with platinum, pure platinum isn't soluble in nitric acid, but if you dissolve an alloy of 95% palladium and 5% platinum in nitric acid all of it will go into solution.
@@alexanderkroboth3310 Agreed, it could well be - certainly makes some sense, but there was still some metal left undissolved after the 12 hours of multiple intense boils. Iridium ,if you can get it in solution, forms coordination complexes which from my (granted hazy) memory aren't overly understood and can display just about any colour depending on the structure. I remember this as my inorganic professor was a world expert in developing Pt and Ir complexes as anti-cancer treatments. I however was a lowly student so take my suggestion with a grain of Pt salt. Cheers and thanks for the reply.
@@AndyGraceMedia In that alloy the iridium was evenly mixed with the platinum, so if it would dissolve away all the platinum and leave the iridium behind you should end up with a powder or some spongy metal like how you have when dissolving the silver out of inquarted gold, but these were solid pieces of metal. And in Aqua regia, which is mostly HCl you'll have the hexachloroiridate complex, which has a dark red color. Anyway, thanks as well, have a nice day.
Love all your content!
This platinum thing though... Seems nasty and difficult to work with. Don't want anything bad to happen to you. Take care with this stuff!
Is there going to be a part 3 for a bar of platinum or is this considered complete?
I’m working on part three.
when did you add the sodium bromate because that step is what is supposed to seperate out the Pt from the Ir and it is done during the time that both are in solution (dark black). to seperate out the iridium while leaving the Pt behind in solution.
pure chloroplatinic acid is dark red in color.
I haven’t done it yet.
@@sreetips cant wait for part 3 then!!
You could probably remagnetize your stir bar by sticking it to one of your big neo magnets and leave it there till you need it 👌
On your waste solutions, when it gets to the acidic iron solution, what do you do with that? Baking soda to neutralize it and down the drain? Do you have to take it to someone for disposal?
Sodium hydroxide. Baking soda doesn’t have the punch.
@@sreetips Gotcha. Then it's safe to go down the drain?
Acid plus base make salt and water. Just make sure pH is right.
Excellent video once again thank you 😊 🙏
It's interesting how such a silvery metal is a dark, brownish orange in solution.
Fascinating stuff 🥹
Where does your fume hood exhaust to, is there a scrubber on it?
No scrubber, outdoors away from my work area.
Thanks again for sharing
Hi ich habe eine frage unwahr platin testing ging mit amonyumcloride oder ???
I’ve used ammonium chloride solution to precipitate pure platinum salt
It is really strange for me. In like 95% of your videos you usually do almost the same stuff, but nevertheless I'm always waiting to see another one. :) So you know... a little dosage of something new is even more interesting no matter your experience. We all learn from your mistakes. Cheers!
The the magnetic stirrer wears out.
Googling for "magnet experiments what happens when a magnet is heated" you will get the explanation:
"When heated above 176° Fahrenheit (80° Celsius), magnets will quickly lose their magnetic properties. The magnet will become permanently demagnetized if exposed to these temperatures for a certain length of time or heated at a significantly higher temperature (Curie temperature)."
I didn’t know that until this series. Thank you
How is this a bromate synthesis? I didn't see you use any bromate salts, only chlorides.
This a new (to me) process that I’ve never tried. Until now.
I have been curious for a while now but if you have all that cement silver and pure silver crystals, why do you use antique silverware and other utensil's to enquart gold? why not just use the cement silver or even the pure crystals?
Palladium will build up in the cement silver if it’s used over and over. Pure silver crystal has already been through the silver cell - like taking a step backwards.
У автора видео чётко выпал гексахлорпалладат аммония. То что диметилглиоксим не сработал, свидетельствует о том что палладий был в степени окисления +4 в то время как дмг работает только с 2 валентным палладием. Судя по цвету осадка красного, там больше 90% хлорпалладата аммония и возможно примесью платины. Иридия судя по цвету нет, так как если бы он был в растворе то с хлористый аммонием дал бы чёрные игольчатые кристаллы отлично различимые даже в такой каше.
It’s confusing, especially for a novice like myself.
Тебе надо было восстановить палладий до +2 тогда дмг сработал бы отлично. А платина осталась бы в растовре
I read that you can supposedly seperate pt from iridium by disolving the platinum from the mixed salts in dilute AR on gentle heat. It should leave metallic iridium behind. I'm not sure what exactly dilute means. Maybe you had some of it on the first run, just before you were going to filter it? I dunno. Good effort tho. You'll get it figured out, I'm sure.
No matter how careful, some of the Pt would get left behind with the iridium. And some of the iridium would follow the platinum and go in solution. That’s the nature of these six sister metals (platinum, palladium, rhodium, iridium, Osmium, ruthenium). They hate to be separated. They don’t cooperate. I’m afraid that I’m in deep water with this series. Maybe I should have left it alone.
Nice womble stacker well done sir
Like watching a mystery movie ;)
Thanks again
Wish you nothing but the best in 2023
What would the ammonium platinum salt look like if disolved in water? Would it look clear?
It would probably be very near the same color as the salt.
I found that my magnetic stirs like that will lose their magnetivity when heated over a certain temperature. They make high temperature magnetic stirs which can handle a little more heat
I had no idea
Anyone planning on recovering and refining platinum from catalytic converters should really think twice about the amount of time chemicals and hazards.
Do you use a the Patreon service or anything similar?
I don’t have patreon, sorry.
Nice work 🙏
Working late! Love the content.
I do hope you have a great night!
What you mean is that industrial Zinc contains palladium, but there is no rate per kilogram, only how it is processed.
As a lab man you are amazing but the metallurgical tricks are missing if you take the zinc for an estimated time in an induction furnace that reaches the stable temperature 1°C below . When the zinc boils, it begins to oxidize and becomes a metallic gas that can later be catalyzed in water and leaves palladium, platinum and rhodium as residues. For this reason, old zinc is so expensive due to the high content of platinum group metals in naval scrap yards there are thousands of buyers of this Zinc from ingots (Bota Mar).
Nice, I didn’t know that.
Is it possible to use hydrochloric and peroxide to put the precipitate in solution sreetips
Possibly
Great videos
Where did you use sodium bromate?
I chickens out. I didn’t use it. Platinum is best left to professional refiners.
Gooood morning from central Florida! Hope everyone has a great day!
Goooood morning!
Interesting it's pink when iridium hexachloride trihydrate is green/black. Through hexachloroplatinic acid is noted as reddish brown, it would have made sense for the iridium to have darkened rather than lightened the precipitate.
These metals are baffling to me. Completely out of my comfort zone here.
The other stir bar is too small for that beaker. The new one works, but you'd be guaranteed to keep the precipitate suspended the whole time if you had a stir bar that was 35mm or longer.
What happens if you drop that stannous solution in the beaker with the precious metal?
It will turn color
@sreetips will it ruin the batch or do you keep those test strips and refine later?
@@zacherysmith2667 If this is the same as his other refinings, he saves all test strips for processing later along with the filter papers.
I hope you're wearing level 6 gloves!
What does soyable mean?
Soluble means “dissolvable” like sugar is soluble in water.
Oh, oh this is IT! PART TWO, ...OH YEAH
Doesn't 40% HCl have 60% H2O which could dissolve the platinate ppt. ?
Yes
111👍's up sreetips thank you for sharing this video with us all
19:50 the solution is moving clockwise and the stir bar is moving counterclockwise. 🤔
Got to be an illusion.
It's a phenomenon called temporal aliasing. en.wikipedia.org/wiki/Wagon-wheel_effect
@emanuellandeholm5657 I thought it had something to do with the speed vs frame rate 🙄
@@laughinghyena001 Yeah, that's what it is.
It’s an optical illusion. The stir bar always turns clockwise looking down into the beaker.
Now we know why you don't make a practice of refining platinum. Seems like a lot of work and very dangerous.
Working with platinum looks like a pain in the ass
Understatement.
Cough cough...mass spectrometer ;) still waiting for that go fund me... I would donate towards it.
Make sure bucket isnt leaking, saw the pattern of it on the table, cant tell what liquid made it
Sometimes rain water is on the bucket. That’s why I set them on cardboard.
I precipitated palatin with NH4cl, why didn't I see a reaction?
That’s baffling. I don’t know why.
Can you help me how to dissolve metal rhodium? How can we combine acid?
I’ve heard that rhodium is soluble in hot sulfuric acid. But I’ve never tried to dissolve rhodium. It’s a mystery to me.
Hot concentrated sulfuric acid.
Can you help me with what chemical to precipitate rhodium?
This seems like it was a real pain. Though still interesting.
I’m stumped, my research shows iridium should not dissolve in aqua regia. It should have been left behind. It might not be Ir.
Iridium alloyed with platinum - everything dissolves.
Is pink not the colour of Rhodium?
It is
I wonder what makes it red this time.
Who knows what metals lurk in the alloys of men!?
Hi Sreetips. According to three independent sources that I found on the web, iridium is not solvable in boiling aqua regia
I know. But in my experience, I’ve seen many things happen that weren’t supposed to. And many thing that weren’t supposed to happen, happen. A 90/10 Pt/Ir alloy - everything dissolves in hot AR. Also, a 95/5, silver/Pt alloy - everything dissolves in hot nitric. I’ve seen hot hydrochloric dissolve small amounts of platinum. I’ve put gold in solution with boiling nitric. These hard and fast rules can all be broken. It’s an enigma.
On the other hand, if I tried to dissolve a piece of iridium in boiling aqua regia then nothing would happen. It would probably just sit there, looking back at you, unaffected. And that’s where the hot AR/Ir rule comes from.
@@sreetips That's one of the reasons that I love your channel. You do the experiments to determine what actually happens. I'll look around to see what I can learn.
Here is an excerpt from nvlpubs.nist.gov/nistpubs/ScientificPapers/nbsscientificpaper483vol19p325_A2b.pdf
The authors formed an alloy of the Pt/Ir sample with Pb by fusion. They then dissolved away the lead using nitric and then aqua regia. The complete procedure is in the paper, which is from the 1920's.
"In his researches on platinum-iridium alloys Deville discovered that when he dissolved in lead at a high temperature platinum
alloyed with iridium, rhodium, palladium, iron, and copper he was able to effect a very distinct separation of the platinum metals.
The lead formed alloys with all of the platinum, rhodium, palladium, and copper and with a very small proportion of the iron.
The iridium, ruthenium, and iron formed a separate alloy containing no lead. Boiling dilute nitric acid removed the bulk of the
lead, together with the palladium and copper and a small proportion of the platinum and rhodium. Digestion' of the residue with
warm dilute aqua regia left insoluble only the alloy of iridium, ruthenium, and iron."
Why does the pink color worry you my friend?
Platinum salt is yellow
Please be careful Sir. Thank You Sir. THE SARGE