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The stannous chloride test uses 1. Transition metal character of noble metal - giving locally colored chlorides by highly concentrated SnCl2
2. Reductive ability of Sn++ resulting in metal powder + SnO2 powder, looking dark/black. Photos may deceive since it is a matter of principle, not exact return of the same color. However you can see them in Goldn'scrap publication about this subject.
Be aware that selenium and tellurium give red and black precipitates correspondingly, mercury grey by this test.
 
I totally agree with you assessment Kurt and thank you for you time and assistance, and the same to all others who have chimed in on this post. I needed to finally dispose of this stored mess but wanted to assure it wasn't containing something of value. I invested some time and some of my chemicals I have had stored for some time.
Thanks again Bill
And Truth does Matter
 
I'm back This is a new topic but is a further followup to my last post titled "Positive indication for Platinum with Stannous Chloride".
So what is new here is since I had pretty much determined that I had no values left in my solutions I thought I would at least try to drop any copper I had in this solution before I disposed of it. I proceeded to drop the copper by precipitating it out with iron and I did get a prec but not at all of what I was expecting. see pictured of what was dropped and a assay from my local coin/pawn shop when they put it in their new analyzer. They texted me the results as show below. I am still precipitating the remainder which I figure is about half of what I have already dropped, so I should end up with about a a pound of this. I have tried to melt a small batch but was only successful once I alloyed it with some silver. I guess I need to know since I am only familiar processing mostly silver and to a lesser gold, do I try to process this or sell it or send it somewhere and tale the cash.
IMG_1366.JPGIMG_1361.JPGIMG_1360.JPG IMG_0002.jpg
 
Iron doesn't just drop copper. It drops everything below it on the reactivity series.

The XRF numbers are nonsense. As much as I'd like to say "Sell it at those numbers!", that would be unethical.

I'll let others who are more knowledgeable about XRF help you interpret those results.

Dave
 
Thanks Dave I would not sell something like this on Ebay or to anyone that doesn't truly know what this means. I was thinking to a person/company that does nothing but refining PM's.
 
Sorry but have no tantalum capacitors!
But back to my thread I have 2 more pictures of the metal i melted with roughly 50% .999 silver. It took quite a bit more heat once the silver liquefied to finally get the sample metal to melt and mix together. As you can see it didn't pour very well and peaked at the end of the pour. Appears to have solidified before it had a chance to flow out. It definitely has a bronze color to it. I will try to get a XRF reading on it tomorrow or Monday.
I have been reading in other posts on XRF readings and how the readings can vary spuriously. What strikes me greatly is the XRF didn't show any copper. Another variable for this reading could be that the reading was taken from the bottom of the glass jar and that just so happens to be where the very finest particulates would form, (just a thought).IMG_1371.jpgIMG_1369.JPG
 
As part of an XRF's standard metals analysis package, copper is usually included. So it is possible that the XRF is a bit out of wack. Maybe just standardized/calibrated or only has software for precious metals.

You can test it by using a fine gold coin, .999 silver bar and a "pure" copper buss bar and see what each of the readings are.

Although it looks like the person that shot your sample is using a Niton series or similar, it could be that the XRF is not warning the user that it needs to be standardized, although nowadays most XRF's force the user to standardize.

Recently, I was messing around with an XRF and decided to sample some gold buttons I had and it showed that they were primarily Ti, Cu, Fe, and Ag. No Au whatsoever. Since the XRF didn't have software to read gold correctly, it spewed out a bunch of bull crap, figuratively, of course.
 
Attempting to melt anything with Cd in it is extremely dangerous and foolish. Please do some research before you hurt yourself . You have a toxic mess there.
 
Roger that. I really have no further need to melt this material without first separating the the PGM's from the rest if that is the advice I get from someone on the this board. If I am to attempt to refine this mess, I have no idea of my starting point, 1) drop the Ag first, then go after the Pd Rh and Ru. Or 2) separate the Pd, Rh, and Ru. The Ag, Cd, and Fe are of little concern to me other than the hazardous properties of the Cd. I am awaiting Steves video on refining PGM's and am studying Hoke's book on this subject chapter XII.
 
My sincere apologies for coming across like the Grinch however getting involved with Cadmium and PGMs either mutually exclusively or together without being involved in a super lab with all the mod cons for safety is beyond nuts.

Go play with Cyanide instead. It's a lot safer.

At least you know where you stand with it.

When you're coughing your bloody lungs out from permanent damage from one single Cadmium web or pissing red from Platinosis (both of which are irreversible) it's way too late.

Get real guys. Stop this crap off.
 
Just for the record and to assure everyone here, I am quite aware of the hazards of Cd. I am a 38 year retired Boeing employee in which we have for at least the past 15 years have had Cadmium awareness training with a recert every year on the dangers and hazards of Cadmium. As a QA inspector and certified for Cad plating repairs on acft skins I have great respect for not only Cd but training on the proper use and types of PPE. That said, I have no interest in proceeding with melting or unsafe handling of said materials without further knowledge of processing safely this material if at all possible, or getting information of a reputable refiner to send this to. In my search on this board larger refiners will not take the small amount that I have.
As for the button above, unfortunately was unaware of the XRF results prior to this melt, which was done with good to excellent ventilation. However I really do appreciate your concerns and reminders of necessary precautions with this and all manors of safe handling procedures, not just for me but for all concerned members and guests on this site.
Do you have a good reputable refiners name that I could send this too. So far all I have received from this post is cautions but no real advise of where to go from here with this material.
 
I found this place on the web to take or send this stuff to in NY. I have been wanting to visit the big apple so maybe I'll just get the wife, get on a plane and visit one of these places
https://www.mgsrefining.com/
http://www.generalrefining.com/
http://cjenvironmental.com/dallas/ Dallas this time of the year sound nice!
 
Lets get realistic here folks,

If this was cemented from a chloride solution there shouldn't be any silver.
If the solution contained that much palladium then the stannous test would have shown it clearly.
If this was cemented from a solution then there should have been a lot of rhodium plating solution.
If this was cemented with iron I would expect cadmium to stay in solution as it is so close to iron.

What was the source of your material?
How did you treat it? Was it a chloride solution or a nitrate?

I would say that the XRF is totally wrong so why believe in any of the numbers.

Göran
 
So at the beginning of this post I had ref to the previous post in which I described a chunk of metal I had got from a friend. We made a deal that I would refine the silver and gold from it and we would split it 50/50.
So I did just that and when all was said and done if I recall It came up about maybe 200g short of what I was suspecting. My thought was that was copper or what. I save all of the nitrate solution in a big bucket. This was in August 2011 from the date of these pictures attached. So if you go back to the post I started this one with you will see what I was saying and has many pictured of the solution and stannous chloride test performed.
Since my friend told me it was mostly silver i took it at that and went with that.
Since you want to get real let me tell you something about my self.
Im 63 years old, retired from the Boeing Co. and my duties when retired was team lead for Preflight/Delivery quality on the 787 program. My user name you will notice is truthmatters and this hold a lot of meaning in my life. So far most of the responses I have got from members on this board has been slams about my integrity and what I am trying to accomplish and feeling offended by your comments. So if you have no constructive comments to help guide me through this process keep them to yourself.
 

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truthmatters, while you may have had a long, distinguished career with Boeing, that doesn't translate to a knowledge of dealing with precious metals. You've come here asking for help, and people are trying to give it to you. It appears you don't like what your hearing, so you are taking offense at the replies, and telling the members here what they are and are not allowed to post. You need to lose that attitude immediately.

In your opining post in this thread, you said "So what is new here is since I had pretty much determined that I had no values left in my solutions I thought I would at least try to drop any copper I had in this solution before I disposed of it." Then you showed an XRF readout showing 15% silver, 12.94% palladium, 8.65% Rhodium, and 2.32% ruthenium. If you had determined there were no values, why would you believe that over a third of what you have are precious metals?

Göran has tried to succinctly give you some facts. If you think about what he's said, instead of rejecting it, you'll realize the XRF results are wrong. Silver doesn't exist to any appreciable degree in a chloride solution, so it's impossible that you have 15% silver. If there was 12.94% palladium, the stannous test would be very dark, not the faint brown you showed. I could go on, but I expect you'll feel I should keep my comments to myself as well.

Take a breath and realize that you don't have a jar full of precious metals. If people continue to offer you advice, understand that they are trying to help.

Dave
 
So in reference to my last post of which I posted pictures of what I believe to be where this Pd, Rh, and Ru as well as the Cd has come from. If you notice on the last picture there is a chunk that I cut off the corner. That chunk I gave back to the guy i got this from. I have just contacted him and he does in fact still have that chunk of this metal. He is going to bring it by in the next couple day and we will take it and have a XRF test done on it. I feel this to be of great evidence one way or the other since it is the only thing I can think of where it may have come from. And BTW if indeed there is any values left in this my original deal with him still stands, he is entitles to half less any cost to get it refined. He reminded me that his father was in the refining business, I'll try to get more on that later to see if we can determine what mine it may be from.
I have also take 2 more samples and the one previously posted and had them sampled again, here are the results.
IMG_1374.JPGIMG_1377.JPGIMG_1375.JPGIMG_1378.JPGIMG_1372.JPG
 
Hi Dave I am a bit frustrated in that I came here to get some idea of what to do with this discovered values ie: refine, sell, or send it to somewhere to have it refined. All the advise has been what not to do with it. If this was your metal in a jar that all the evidence that is shown by the XRF readings what you do with it. Dispose of or look to try to confirm one way or another if there is of any values in it. I agree I am no chemist and I do not know much about what is being said about there should be no Ag in these samples but if that is the case and these results are erroneous then should I assume that there is no Cd also. All I am trying to do is find out do I have 0$ value or $3000.+ value. My only point in giving my back ground is that I am not some 25 yo moving recklessly into some endeavor for which I know nothing about. Back when I was refining this back in 2011 I was a member of this post and if I recall my member ID was WCT0415, so I am not just shooting from the hip. I learned a great deal from back then, which is why I saved all this solution. This has been in the corner of my shop for nearly 7 years and one of the last things I processed was this chunk of silver metal. What was in solution from my many refining tasks have sat there for all this time. I took 2 1/4 full buckets of what was left over from silver refining, first 1/4 bucket from previous silver drops and the second from this chunk of metal mixed them together since no one would give me any guidance, let them settle poured off the liquid from the heavy settlement. I started by inserting a copper bar onto and nothing dropped. So that is when I thought as long as there is nothing of value there I would at least drop the copper from this solution and dispose of the solution. I am pretty good friends of the coin shop down the road so I thought I would see what quality of copper I had dropped. I never expected to see anything but Cu from test. All my refining and testing was done with a wind tunnel of sorts that I did all my previous refining in, it is quite safe. My frustration is I know no more now than I did when I first started this post or the first post except that I have three jars of metal containing metals of value mixed with hazardious Cd. But what do I do with it? Can anyone give me an answer please.
 
Nice picture of you irradiating a sample you are holding in your hand.

Did you read the manual?


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When using a niton, first of all realize that you are pointing an X-ray beam. While the heavy metal will stop a good portion of the radiation, it's still a safety hazard.

The niton does not have enough elements in its database to form a reasonable assay in either precious metal mode or alloy Id mode. This metal would need to be analyzed on a much more advanced machine. Desktop edxrf with expert analyst or wdxrf, still with a good analyst.

Gravimetric analysis will be necessary either way.


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