Hi again folks,
I’m back so soon with another project because I’d been working on this one simultaneously as I did the “Unknown Contaminant” one you may have checked out.
A few years ago when I first started doing refining, I happened to purchase a very interesting old light bulb type of thing at a swap meet, I purchased it specifically because I thought it might contain precious metals and figured the $5 I paid for it was well worth the gamble.
Back when I got it, I did a little searching to figure out exactly what it was and any specifics about it, but didn’t find much, all I managed to establish was that the company who made it existed in the late 30’s and early 40’s and that this thing was some sort of heavy duty light bulb.
The thing is, at the time, I didn’t care a whole lot about what it was, I was more anxious to break it open and get to the contents, but now I’m regretting not having documented it before destroying it, in other words I have no image to show you, so all I can say is, it was about 2” in diameter, about 8” long, and made of clear glass with a lot of wires, meshes, and antenna like components inside.
What I salvaged from the bulb was: four wires of 1/16” diameter, two metal plates 1/64”x1/2”x2”, four rods of 1/32” diameter by 3/4” long, and a sort of mesh type of thing suspended between rods which I think was the filament. The four wires connected the two plates to the four rods, the means of joining being soldering, the filament was separate from these other parts and I don’t remember how it related to them.
Shown below are all the parts, except the filament, and some pieces of silver shot for color comparison.
Keep in mind that what’s shown is far from original condition, for one thing I cut the plates and rods off the ends of the wires, but more importantly, I’ve abused the hell out of this stuff in the few years since I first acquired the bulb. What you’re looking at are the pieces readied and sized to fit the mouth of the Erlenmeyer. The wires in particular have taken the most abuse, they’ve been repeatedly folded completely over and then straightened out again, they’ve been coiled up into tight spirals about the size of a nickel and straightened out again. What I’m getting at is how extremely malleable this stuff was, not malleable like a roll of solder you’d get from the hardware store, but malleable like you’d expect a platinum wire to feel like, and they never showed the slightest hint of ever wanting to break.
Besides all the folding, coiling, spiraling, and straightening of the wires, I also hammered one of them and there was no sign of cracking or splitting. I could’ve hammered until it was as thin as aluminum foil, but that wasn’t needed, I had seen enough, and the result is shown below in the next two images.
Seen also in the above two images are the results of another test I did with platinum in mind, the wire on the right was heated using a mapp gas torch, and the torch struggled, it would just get the wire to start to melt and that’s it. Obviously I never got the material to fully melt, not even enough to get the coils to stick together (I had it coiled up like a spring, with coils touching), for afterwards I pulled it apart and saw that the coils never adhered to one another.
The high melting point wasn’t the only platinum supportive conclusion that I arrived at with the melting test, the white light produced by the coil was intense. I learned the hard way that welders goggles should be worn when melting this stuff, I could see the white spots burned into my eyes, see them even in broad daylight, and it took till the next day before they went away. I never experienced anything like this before because I’ve never worked with PGM’s, I fear I may pay for this in the long run since my eyes are already hammered from doing similar stupid stuff in the past.
Besides the malleability, the high melting point, the intense light given off when heated, and some of the other indications such as the color of the metal in general and the color of the material after being heated, I also can add to this list that nitric had no effect whatsoever on it. Up until I did the nitric, palladium was still a contender, but supposedly palladium is attacked by nitric, thus platinum is still my number one candidate.
Something contrary to my platinum assumptions is that the parts are fairly attracted by a high quality, strong, neodymium magnet, the attraction is unmistakable. This lead me to think that there was a fair amount of nickel present, yet the nitric had no effect, so I don’t know what to think about this, the items are definitely not plated for the wires had been cut off and had exposed ends.
The weight of the salvaged parts was 17.98g, and here’s the solution after transferring from the erlenmeyer, at this point it’s been filtered, evaporated, and the nitric killed, at least I think it was killed as you will find out.
Two things about this solution, first it’s green, which I was expecting since I thought nickel might be involved, and second, I used an erlenmeyer because I was expecting it to be a long time on the stove, and sure enough it took twice as long to dissolve than the batch of gold I had started simultaneously. I thought this long in duration cook time was another promising aspect indicating platinum.
One thing deserving pointing out concerning the evaporation, there seemed to be way too much liquid still present, in other words I never got to the syrupy consistency I had wanted, unexpectedly and seemingly way to prematurely, the liquid suddenly turned into a mass of crystals. I added a good amount of hydrochloric, and a little water, and it took some effort to get the stubborn crystals to dissolve, but once they did, I then evaporated again as best I could before pulling it off the stove a little early in fear of getting the crystals back again. I don’t know what, if anything, these crystals might mean, maybe they are indicative of something gone wild like the girls I use to mess with, but I do know that I feel a little uncomfortable knowing I may not have killed the nitric.
Finally after all that setting of the stage, now I can get to my problem, that being the addition of ammonium chloride, it produced nothing, not even a wimpy little fizzle. The addition by the way, it was done to 5ml of solution, not done to the whole beaker full. I guess it’s possible that I never killed the nitric because of the crystal growth problem and thus the negative result I got from the ammonium chloride, so as I’m writing this now, I’ve got the solution back on the stove but this time taking it down at an excruciatingly slow rate, maybe this way I can get it to the syrup I didn’t achieve before, maybe this will make a difference when I go to try the ammonium chloride again.
In the mean time I did a test of the aqua regia, what you’re looking at is a few drops of it on a filter paper with a drop of stannous solution in the middle. Doing these stannous tests is something I definitely have no confidence or experience with, so what do you guys think?
After seeing no result with the ammonium chloride, I thought I’d try and see just what would precipitate, so I took the 5ml of the solution and sprinkled in a little SMB, and again nothing, I then put a length of copper wire, and again nothing, so I added a few drops of nitric and started getting a reaction. The addition of copper wire and nitric produced just a whisper of black fluffy residue, very light weight, but that’s it, so oh well, so much for messing around.
By the way, having never worked with platinum before, thus not with ammonium chloride either, is it normal that this stuff is hard to dissolve in water, and that it gets cold? I had to put it on the stove to get it to fully dissolve, which prompts me to ask this too, should I have added it to my aqua regia solution when both were about as hot as I could get them, was it a mistake to have done it at room temperature?
I must say, if the ammonium chloride had precipitated like I was expecting, you’d not be hearing from me right now, so besides comments about the stannous test results which I can hardly wait to hear, anything you can say about any of the other stuff I went over will be appreciated and given a lot of consideration.
I started off with 17.98g of material to dissolve, it all was completely dissolved, in fact there wasn’t even any residue that got filtered out when I transferred the contents from the erlenmeyer to the beaker, everything dissolved except the four rods, they remained intact.
Oooops, I’ve reached my limit of five images, to be continued..........
I’m back so soon with another project because I’d been working on this one simultaneously as I did the “Unknown Contaminant” one you may have checked out.
A few years ago when I first started doing refining, I happened to purchase a very interesting old light bulb type of thing at a swap meet, I purchased it specifically because I thought it might contain precious metals and figured the $5 I paid for it was well worth the gamble.
Back when I got it, I did a little searching to figure out exactly what it was and any specifics about it, but didn’t find much, all I managed to establish was that the company who made it existed in the late 30’s and early 40’s and that this thing was some sort of heavy duty light bulb.
The thing is, at the time, I didn’t care a whole lot about what it was, I was more anxious to break it open and get to the contents, but now I’m regretting not having documented it before destroying it, in other words I have no image to show you, so all I can say is, it was about 2” in diameter, about 8” long, and made of clear glass with a lot of wires, meshes, and antenna like components inside.
What I salvaged from the bulb was: four wires of 1/16” diameter, two metal plates 1/64”x1/2”x2”, four rods of 1/32” diameter by 3/4” long, and a sort of mesh type of thing suspended between rods which I think was the filament. The four wires connected the two plates to the four rods, the means of joining being soldering, the filament was separate from these other parts and I don’t remember how it related to them.
Shown below are all the parts, except the filament, and some pieces of silver shot for color comparison.
Keep in mind that what’s shown is far from original condition, for one thing I cut the plates and rods off the ends of the wires, but more importantly, I’ve abused the hell out of this stuff in the few years since I first acquired the bulb. What you’re looking at are the pieces readied and sized to fit the mouth of the Erlenmeyer. The wires in particular have taken the most abuse, they’ve been repeatedly folded completely over and then straightened out again, they’ve been coiled up into tight spirals about the size of a nickel and straightened out again. What I’m getting at is how extremely malleable this stuff was, not malleable like a roll of solder you’d get from the hardware store, but malleable like you’d expect a platinum wire to feel like, and they never showed the slightest hint of ever wanting to break.
Besides all the folding, coiling, spiraling, and straightening of the wires, I also hammered one of them and there was no sign of cracking or splitting. I could’ve hammered until it was as thin as aluminum foil, but that wasn’t needed, I had seen enough, and the result is shown below in the next two images.
Seen also in the above two images are the results of another test I did with platinum in mind, the wire on the right was heated using a mapp gas torch, and the torch struggled, it would just get the wire to start to melt and that’s it. Obviously I never got the material to fully melt, not even enough to get the coils to stick together (I had it coiled up like a spring, with coils touching), for afterwards I pulled it apart and saw that the coils never adhered to one another.
The high melting point wasn’t the only platinum supportive conclusion that I arrived at with the melting test, the white light produced by the coil was intense. I learned the hard way that welders goggles should be worn when melting this stuff, I could see the white spots burned into my eyes, see them even in broad daylight, and it took till the next day before they went away. I never experienced anything like this before because I’ve never worked with PGM’s, I fear I may pay for this in the long run since my eyes are already hammered from doing similar stupid stuff in the past.
Besides the malleability, the high melting point, the intense light given off when heated, and some of the other indications such as the color of the metal in general and the color of the material after being heated, I also can add to this list that nitric had no effect whatsoever on it. Up until I did the nitric, palladium was still a contender, but supposedly palladium is attacked by nitric, thus platinum is still my number one candidate.
Something contrary to my platinum assumptions is that the parts are fairly attracted by a high quality, strong, neodymium magnet, the attraction is unmistakable. This lead me to think that there was a fair amount of nickel present, yet the nitric had no effect, so I don’t know what to think about this, the items are definitely not plated for the wires had been cut off and had exposed ends.
The weight of the salvaged parts was 17.98g, and here’s the solution after transferring from the erlenmeyer, at this point it’s been filtered, evaporated, and the nitric killed, at least I think it was killed as you will find out.
Two things about this solution, first it’s green, which I was expecting since I thought nickel might be involved, and second, I used an erlenmeyer because I was expecting it to be a long time on the stove, and sure enough it took twice as long to dissolve than the batch of gold I had started simultaneously. I thought this long in duration cook time was another promising aspect indicating platinum.
One thing deserving pointing out concerning the evaporation, there seemed to be way too much liquid still present, in other words I never got to the syrupy consistency I had wanted, unexpectedly and seemingly way to prematurely, the liquid suddenly turned into a mass of crystals. I added a good amount of hydrochloric, and a little water, and it took some effort to get the stubborn crystals to dissolve, but once they did, I then evaporated again as best I could before pulling it off the stove a little early in fear of getting the crystals back again. I don’t know what, if anything, these crystals might mean, maybe they are indicative of something gone wild like the girls I use to mess with, but I do know that I feel a little uncomfortable knowing I may not have killed the nitric.
Finally after all that setting of the stage, now I can get to my problem, that being the addition of ammonium chloride, it produced nothing, not even a wimpy little fizzle. The addition by the way, it was done to 5ml of solution, not done to the whole beaker full. I guess it’s possible that I never killed the nitric because of the crystal growth problem and thus the negative result I got from the ammonium chloride, so as I’m writing this now, I’ve got the solution back on the stove but this time taking it down at an excruciatingly slow rate, maybe this way I can get it to the syrup I didn’t achieve before, maybe this will make a difference when I go to try the ammonium chloride again.
In the mean time I did a test of the aqua regia, what you’re looking at is a few drops of it on a filter paper with a drop of stannous solution in the middle. Doing these stannous tests is something I definitely have no confidence or experience with, so what do you guys think?
After seeing no result with the ammonium chloride, I thought I’d try and see just what would precipitate, so I took the 5ml of the solution and sprinkled in a little SMB, and again nothing, I then put a length of copper wire, and again nothing, so I added a few drops of nitric and started getting a reaction. The addition of copper wire and nitric produced just a whisper of black fluffy residue, very light weight, but that’s it, so oh well, so much for messing around.
By the way, having never worked with platinum before, thus not with ammonium chloride either, is it normal that this stuff is hard to dissolve in water, and that it gets cold? I had to put it on the stove to get it to fully dissolve, which prompts me to ask this too, should I have added it to my aqua regia solution when both were about as hot as I could get them, was it a mistake to have done it at room temperature?
I must say, if the ammonium chloride had precipitated like I was expecting, you’d not be hearing from me right now, so besides comments about the stannous test results which I can hardly wait to hear, anything you can say about any of the other stuff I went over will be appreciated and given a lot of consideration.
I started off with 17.98g of material to dissolve, it all was completely dissolved, in fact there wasn’t even any residue that got filtered out when I transferred the contents from the erlenmeyer to the beaker, everything dissolved except the four rods, they remained intact.
Oooops, I’ve reached my limit of five images, to be continued..........
