# Here is one for the experts here



## truthmatters (Feb 10, 2018)

It has been about 2 years since I have done any refining and from that time I was just refining gold and silver. I was given in trade a very large chunk of silver metal from some melt of his grandfathers, It weighed 3.7 lbs and looked to be mostly silver. I refined the silver and gold from this piece and put all the solution into a very large bucket and stored it away.
I have since pulled it back out and and have noticed it has evaporated quite a bit with some very interesting results. I have separated it into 4 different containers all of which test positive for Platinum using a fresh batch of Stannis Chloride with a distinct yellow color. I have attached some pictures of what I have here with the hopes that I may get some help starting to further refine this lot. I have just ordered the video -Fundamentals of Platinum and Palladium DVD- Video Guide to Processing Catalytics and Other Pt and Pd scrap- to assist in this endeavor but thinking my starting point will not be covered ie: uncertain state of this solution. My hopes is that many of you with knowledge with PG have seen this before and know what stage this is in and to avoid any mistakes and help get me started.


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## truthmatters (Feb 11, 2018)

Here is the last photo since it would only let me insert 5


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## nickvc (Feb 11, 2018)

I’m far from an expert on PGMs but if that were mine I would add some Hcl and heat gently, allow to cool filter it, if there is any gold it will be here, and then use copper to cement any values from the solution, I’m always a little wary around PGMs and their salts they are very nasty and toxic so make sure you wear gloves and do any reactions within your hood.
If after cementing any values you have a decent volume then perhaps go further into refining them but in my opinion unless you have a large volume leave them as PGM blacks and keep until you have a large amount to make the risk worth the return or send them to someone used to dealing with them safely.


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## snoman701 (Feb 11, 2018)

nickvc said:


> I’m far from an expert on PGMs but if that were mine I would add some Hcl and heat gently, allow to cool filter it, if there is any gold it will be here, and then use copper to cement any values from the solution, I’m always a little wary around PGMs and their salts they are very nasty and toxic so make sure you wear gloves and do any reactions within your hood.
> If after cementing any values you have a decent volume then perhaps go further into refining them but in my opinion unless you have a large volume leave them as PGM blacks and keep until you have a large amount to make the risk worth the return or send them to someone used to dealing with them safely.



Nick,

Will the pgms completely precipitate? Your post is identical to my feelings about the PGM's...I don't want them. But, since they are there, I do want to collect them prior to my waste treatment.

-Jacob


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## FrugalRefiner (Feb 11, 2018)

If you use sufficient agitation, yes the cementation will be complete. I think 4metals made a post about a method he uses. In simple terms, he uses a piece of PVC pipe with a piece of copper hanging inside and an air bubbler at the bottom. The air bubbler draws the solution in at the bottom of the PVC pipe, causes it to flow over the copper, and then exit at the top.

Found it in Fuzz Button Interconnects, need some advice.

Dave


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## nickvc (Feb 11, 2018)

With the addition of an air pump yes they will all cement but it can take time it also helps to clean the copper off a few times to make sure there is copper available to cement the PGMs.


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## truthmatters (Feb 11, 2018)

Thank you for your inputs. I do have a magnetic stirrer and about a half pound of copper dust that I have dropped with steel from other solution that I had. I will give your suggestions a go and see what I have. Will do this with a small amount first just to see what drops. Will keep you posted as to the results. I think I will mix all of these solution together and take my first run at this from that batch, that way if successful it is just a matter of repeating the same process for the rest.
Thanks again Bill


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## snoman701 (Feb 11, 2018)

Thanks Guys...I'll build it later today if I can get out of the driveway! Winter is really kicking my butt this year!


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## Lino1406 (Feb 11, 2018)

A reminder: The stannous chloride test indeed starts with red/orange/yelow but continues with dark/black if noble metal is present


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## Shark (Feb 11, 2018)

FrugalRefiner said:


> If you use sufficient agitation, yes the cementation will be complete. I think 4metals made a post about a method he uses. In simple terms, he uses a piece of PVC pipe with a piece of copper hanging inside and an air bubbler at the bottom. The air bubbler draws the solution in at the bottom of the PVC pipe, causes it to flow over the copper, and then exit at the top.
> 
> Found it in Fuzz Button Interconnects, need some advice.
> 
> Dave




I use these pumps a fair bit. They operate by bubbling air in from the bottom, up into a small container that is divided by a slot for filter use (or a copper sheet). I have switched to these for my copper cells as they don't splatter droplets everywhere like the regular air pumps do. The down side is I have only found them in a smallish size, the larger sizes operate from a submerged pump and I haven't tried them. Plus they are a lot quieter to operate.

http://www.tetra-fish.com/products/filtration/whisper-internal-power-filter.aspx#thumbCarousel

Edited for clarity


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## truthmatters (Feb 11, 2018)

So i just performed per your suggestion my first 500 ml solution with 80ml of HCL, heated it and from a prior post (If all else fails, clean a short piece of copper wire with fine abrasive cloth, so it's nice and shiny, then dip it in the solution. If there's any values present, you should see them form on the surface. If, however, there is no reaction, or if the copper simply dissolves, leaving behind an etched surface, it's pretty safe to assume that you have recovered all the values.) and sure enough values were indeed present. They appear to be under 15x magnification some shinny metallic values present. Started my next 500ml batch while the first is filtering. Will post more when i have more information.
Bill


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## kurtak (Feb 12, 2018)

truthmatters said:


> I have separated it into 4 different containers all of which test positive for Platinum using a fresh batch of Stannis Chloride with a distinct yellow color.



You need to show a pic of the stannous test (on the end of a Q-tip or on a piece of paper towel or filter paper) because "yellow" is NOT the color for a Pt positive test --- "orange" is the positive for Pt

Showing a bunch of pictures of the solution along with crystals that have formed from evaporation &/or other sediments does no good in helping to determine the presence of PMs in the solution - so - if you are going to ask about a stannous test - then show pic(s) of the stannous test

I say this because as much as a stannous test can/will show positive for PMs does not mean getting a "color" change is a positive for PMs --- there are other (base) metals that will show a color change but are not positive for PMs --- this is known as a "false" positive

The stannous color test for PMs are as follows

Au = purple (which can be so purple it looks black)
Pt = orange (can show up as a false positive if molybdenum is present - but no Pt - the hue's are different)
Pd = green (this is a deep forest green & like Au can be near black - also - Pd will often start out with a Pt orange but "quickly' turn green)

Other "common" colors that show up - but are "false" positives

Brown &/or yellow - which can show up in different hue's - also green but this is usually a light lime green rather then the darker green of Pd

The point being that not all color change with a stannous test mean a positive for PMs - sometimes they are "false" positives --- I (highly) recommend doing the acquaintance experiments suggested in Hokes book in order to better understand what you are looking at in the colors of a PM stannous test & those of (base metal) false positives

In my opinion - the pictures of your solutions are much to bright a blue to have any PGMs in them - even a small amount of PGMs in solution will tend to tint a blue (copper) solution towards green 

Green does NOT mean PGMs are present - other (base) metals can make a solution green - green only indicates that PGMs "might" be present 

The forth picture down from the top - which does have a green color to it is clearly the result of iron from the iron oxide sediment that has not fully settled out of the solution - the other pics that are clear blue are clear blue because the iron has settled out & in my opinion because they are a bright clear blue tells me they have little or no PGMs in them (which may - or - may not be true)

So again - what you need to do is show pics of the stannous test --- & NOT pics of the solutions 

Kurt


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## truthmatters (Feb 12, 2018)

Thank you Kurt I will get some pictures or my Stannis Chloride results. So after heating 1/3 of my solution in HCL I did a Stannis test and the results were somewhat different. Just as soon as I put a drop on it, it immediately turned brown and slowly faded back to yellow. I will post some pictures of this test at my earliest opportunity. My process was 500ml solution to 160ml HCL and heated on Med low for 4 hours. Inserted clean copper bar for about 5 minuted showing a grey color with something adhering and under magnification of 15x some shinny granules. 
Bill


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## FrugalRefiner (Feb 12, 2018)

I hate to be picky, but it' stannous chloride, not stannis chloride. I'll change the title of this thread so it shows up when people do a search for stannous.

Dave


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## truthmatters (Feb 12, 2018)

Thanks Dave


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## truthmatters (Feb 12, 2018)

Results of Stannous Chloride as mentioned by Kurt. I have attached 3 pictures one before SC and 2 post


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## Lino1406 (Feb 12, 2018)

While positive stannous chloride test is essential, but not a proof at this point one needs additional test - not stannous chloride test


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## g_axelsson (Feb 13, 2018)

This looks more brown than orange to me. Did you use SMB to precipitate the gold?

Göran


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## anachronism (Feb 13, 2018)

Lino1406 said:


> A reminder: The stannous chloride test indeed starts with red/orange/yelow but continues with dark/black if noble metal is present



I wasn't aware of this Lino, I always thought that colour tending to a black was gold. Could you share some pictures please? 

Jon


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## kurtak (Feb 13, 2018)

anachronism said:


> Lino1406 said:
> 
> 
> > A reminder: The stannous chloride test indeed starts with red/orange/yelow but continues with dark/black if noble metal is present
> ...



Jon

Just like a stannous test for gold - how dark the test (for PGMs) shows up depends on how dilute &/or how concentrated the solution is when testing

Au - when a solution with gold is dilute &/or has little gold in it the stannous test will report as very evident purple - if the solution has a high concentration of Au &/or is not dilute the stannous test will "appear" black - but its actually a "very" deep purple - or - black with a purple hue to it - if you do the test on a piece of paper the purple is more evident & more so at the outer edges

Pd - again depending on concentration - Pd - at "first" will give an indication of Pt orange - but will then (in relatively short time) shift to green - this green is generally a deep forest green - & again if the concentration is high enough - like Au that green will "appear" black - but will actually have a green hue to it

The purple or green hue of a test that "appears" to be black - depends some what on the lighting & again if you do the test on a piece of paper (rather then on say a Q-tip or solution in a spot plate) the purple or green will be more evident especially at the edges of the spot on the test paper

I have not done a lot of Pt - but when I have - it have always come out with a clear & evident orange - how deep/dark of an orange again depends on concentration (it can lean toward a red/orange) --- as a side note - one thing I have noticed with Pt stannous test - which I usually do with Q-tips - a day or two after they have dried out they will tend to turn blackish with a reddish orange hue 

As a general note to anyone refining PMs - I "highly" recommend DOING (not just reading about) the acquaintance experiments suggested in Hokes book so that you "in fact" become "acquainted" with the "true" colors of a PM test --- reading about the colors purple green or orange can mean just about anything in "the minds eye" & unless you have a true visual of the colors you are trying to identify - you can find yourself chasing your tail to find PMs (that don't exist) - because - "false" positives do show up - & you find yourself saying - well the book said purple or green or orange & that test "kinda" looks purple or green or orange --- colors you see in your minds eye from reading - & colors identified from a true visual can be & often are two different things

truthmatters --- based on the pics of the stannous test - it is my opinion your test is a false positive - I would not chase my tail on that test - at best there "might" be a "trace" of PMs there - so - at best I would put the solution(s) to the stock pot with copper & an air bubbler NO HEAT - heat can & will "force" non PM (base) metals out --- but I would NOT chase these solutions in hopes &/or expectation of getting anymore PMs outs 

Kurt


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## Lino1406 (Feb 13, 2018)

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.


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## truthmatters (Feb 13, 2018)

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


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## truthmatters (Feb 17, 2018)

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.


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## FrugalRefiner (Feb 17, 2018)

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


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## truthmatters (Feb 17, 2018)

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.


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## etack (Feb 17, 2018)

never mind reread the post.    

Eric


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## truthmatters (Feb 17, 2018)

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).


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## geedigity (Feb 18, 2018)

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.


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## jonn (Feb 18, 2018)

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.


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## truthmatters (Feb 18, 2018)

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.


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## anachronism (Feb 18, 2018)

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.


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## truthmatters (Feb 18, 2018)

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.


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## truthmatters (Feb 19, 2018)

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!


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## g_axelsson (Feb 19, 2018)

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


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## truthmatters (Feb 19, 2018)

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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## FrugalRefiner (Feb 19, 2018)

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


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## truthmatters (Feb 19, 2018)

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.


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## truthmatters (Feb 19, 2018)

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.


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## snoman701 (Feb 19, 2018)

Nice picture of you irradiating a sample you are holding in your hand.

Did you read the manual? 


Sent from my iPhone using Tapatalk


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## snoman701 (Feb 19, 2018)

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. 


Sent from my iPhone using Tapatalk


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## truthmatters (Feb 19, 2018)

Hi snowman FYI, I am the one taking the picture, not the one holding the equipment or the sample. but the next time I go over to the shop I will let them know they are doing just what you are talking about


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## FrugalRefiner (Feb 19, 2018)

truthmatters said:


> All I am trying to do is find out do I have 0$ value or $3000.+ value.


And I've been trying to answer that as diplomatically as I can. You have $0.00. You previously precipitated the silver and gold from your solutions. You tested your remaining solution with stannous and the result was negative. As I said in my first reply, iron precipitates everything below it on the reactivity series. That can include Cadmium, Cobalt, Nickel, Tin, Lead, Tungsten, Antimony, Arsenic, Bismuth, and Copper.

I have never seen anyone try to take an XRF reading through a glass jar, especially while holding it in their hand. :shock: 

Again, I'm not trying to be a jerk. I am trying to respectfully tell you the XRF readings are meaningless and that you have a jar of base metals.

Dave


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## snoman701 (Feb 19, 2018)

Just a thought here...I know that the SOP here is to poo poo any XRF results from a powder, and I too question the results enough that I wouldn't expect it to be accurate, but it is possible for it to be.

I would PM Lou and ask him if he'd be willing to buy it based upon his ICP analysis if it's Pd.


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## truthmatters (Feb 19, 2018)

Dave Thanks for your straight forward reply. What you are saying makes a lot of sense and I respect the knowledge of all on this site. However for me to be assured of what you are saying, i will go ahead and do a XRF test on the sample of the silver alloy pictured above, if neg for PGM's off it goes to the hazmat dump, pos it will get sent to confirm or reject the XRF results to one of the refining companies and will update you all.
In either case I thank you for putting up with my ignorance and spending your time trying to educate me.


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## g_axelsson (Feb 19, 2018)

You can't take an xrf reading through glass if that was how it was done.

I don't care if you are a backyard scientist in high school or a 63 year old Boeing employee, I was only discussing the results of the xrf. It just didn't make sense to me.

So... what you should do with your metals. One of the most basic reactions of silver is silver nitrate and chloride forming a white precipitate of silver chloride.

Dissolve some of your "copper" powder, then add salt or HCl. Did it form a white precipitate? Then you have either silver, lead or mercury.
No white precipitate? Then you don't have silver in solution. Period!

That is the truth. And if that matters that is the first test you can do.

Ok, I'm done, I rather spend some time watching youtube videos than giving advice to those who don't want to listen.

Göran


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## geedigity (Feb 19, 2018)

Snoman, I thought I saw the same thing.....holding a sample in ones hands while testing it with a XRF!! Sorry, safety first truthmatters. *This is exactly what you do not do when using XRF.*

I have posted this before, but there is a free online training course offered by Niton/Thermofisher. http://www.thermofisher.com/us/en/home/industrial/spectroscopy-elemental-isotope-analysis/portable-analysis-material-id/xrf-radiation-safety-training.html As you will see, even if you are not the operator of the XRF, you could be receiving a significant dose of X-rays just by watching. The training is free!!

Back to my first post in this thread. Did you check the XRF (not holding sample in your hand and testing) using a copper buss bar, .999 Ag bar? Those are two items you either probably have or could easily get. If your readings are not what you would expect, I really doubt the readings of the unknown material mean anything at all. Since even getting results you expect with known purity metal does not mean the result of an unknown will be known, except maybe if you had the geochem mode on that machine and ran the sample for two minutes.


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## Palladium (Feb 19, 2018)

With all this dickering i could have done run it and had the answers! :lol: :lol: :lol: 
Xrf..... Yeah...........!!!! It's not as point and click straight forward as they would like you to believe!
That's why years ago i coined the term ( What comes out the beaker, comes out the beaker!)
Test are great, but physical metal tells the tell!


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## truthmatters (Feb 20, 2018)

PM sent, hope this is alright with you


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## Palladium (Feb 20, 2018)

To me?


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## truthmatters (Feb 20, 2018)

Yes to all involved in this post


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## truthmatters (Feb 20, 2018)

To Palladium
Somehow you got dropped off the to list. resent


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## g_axelsson (Feb 20, 2018)

That is why I don't like discussions in PM with more than one person.

.. and the fact that we now have split the discussion about the liquid and cemented metal powder over two threads and one pm chain. In the reply I wrote I hadn't included Palladium, so I'm going to post my reply here too.

In reply to a long pm from truthmatters...


> I would rather see this discussion being done in the open, if people are bored they just skip a thread.
> 
> One way science works is to put up theories and then test it. If it fails the test then try to find a better theory that matches the results better. If one aspect of a theory can be proven false then the whole theory is questionable.
> 
> ...



I also wrote


> By the way truthmatter, I have nothing against you. I don't know you and until the contrary is proven I'm quite sure we would have a good time, trading life stories over a couple cold beers.
> 
> ... it is that XRF-reading I'm attacking. :wink:
> 
> Göran



I will not comment any more via PM, it sucks. I might be part of a discussion here if I feel I have something to contribute.

Göran


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## FrugalRefiner (Feb 20, 2018)

I agree with Göran that I'd prefer to continue these discussions on the open forum instead of PM. I also agree that the discussion has been confusing, in part because there was a separate thread about a stannous test which has become part of the discussion here, so I've merged the threads.

truthmatters, I hope you have a jar full of money there, but logic tells me otherwise. On the other hand, we have a member who seems to have found an electronic component that contains almost 20% by weight of gold. The numbers don't seem to make sense, but we will see.

As Ralph says, what comes out the beaker, comes out the beaker!

Dave


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## truthmatters (Feb 20, 2018)

You wrote 


> Dissolve the copper powder in nitric acid. Any rhodium should remain as solid and any silver would end up in solution. Add HCl and it would precipitate silver chloride.
> My prediction is that since you cemented this on iron from a solution where all gold has been removed. (negative stannous test) the metal should be easily dissolved in nitric acid and not precipitate when you add HCl.



I will perform the test you have outlined first thing tomorrow. Is this the formula I should use: 3/1 water/nitric and observe reaction and see what goes into solution. Any thing that does not dissolve, decant and add HCL and observe any silver chloride that may or may not drop?

Thanks Bill


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## truthmatters (Feb 20, 2018)

Oh and Dave as a matter of fact I do have a jar full of money "nickels"


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## truthmatters (Feb 21, 2018)

6 hours into my putting the 250 gr sample into solution.
1) Initial reaction vigorous with 300Ml H2O and 100Ml nitric, action considerably slowed within .5hrs (start-1hr)
2) Added another 50Ml nitric pace picked up and with in an hour approx 60% has gone into solution (1hr - 3hr)
3) Action nearly stopped until stirred. but would nearly stop. Added 50Ml nitric, action picked up. (3 - 3.5hr) 
4) Added 50Ml nitric and put on low heat. Approx 90% metal in solution, the remainder is being very slow to go into solution. Consistent stirring needed to keep action moving. (3.5 - 4hr)
5) Have been adding 25Ml at about 1 hr intervals on low heat to keep action going along. At this point 5 hours into process the last remaining seem to be very stubborn to go into solution and am hesitant to keep adding more nitric until i get some clearity as to how far to go.
Im thinking about decanting what solution I have and starting with anew with what I am having a problem getting to go into solution. Anyway I did take some stannous chloride samples 1 hour apart, what's your thoughts.
Bill


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## truthmatters (Feb 21, 2018)

6 pm and no more action in solution. Put away for the night, will pick up again in the morning by decanting solution off and try to drop any AG from solution and will start with a 50/50 H2O nitric solution with what is remaining solids.


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## anachronism (Feb 22, 2018)

Do you have any white precipitant from the AR process or is it as per the last picture? 

With the 19% reading of silver I would expect a lot of silver chloride if it was correct. That would be my personal judgement standard on the viability of this particular XRF reading. 

If there's not a boatload of silver chloride then the signs are not good.


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## Slochteren (Feb 22, 2018)

Maybe i missed it but if you only added Nitric there should be no gold in your solution, you dissolved all base metals and silver. I would put a drop off hcl in the filtered solution to see if it makes a white cloud off silver chloride to see if there is any silver dissolved. Adding HCL to the remaining solids would create AR with the remaining nitric in it, or adding a litle bit nitric to see if the solids dissolve.

Paul

edit for spelling


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## anachronism (Feb 22, 2018)

Yes Slochteren I misread and thought he had dissolved in AR. 

You're quite correct the next step is to take some of the Nitric solution and put a drop of HCl into it and see if it precipitates out the Silver Chloride. If it doesn't then the rest of my original post applies.


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## truthmatters (Feb 22, 2018)

Ok as of 6 am no further action from the remaining metal settled at the bottom. I poured off this solution and added 250ml HCL, no silver chloride dropped out. I took remaining solids added 200ml H2O with 200ml nitric action picked up again but only mild reaction, but with agitation helped it along. By 9am had completely stopped so added 75ml more nitric to get it going again. This last little bit is being very stubborn to get into solution. Question is this because it may be getting coated over somehow and requiring the nearly constant agitation and adding this much more nitric. With the amount I started with my initial 50/50 water nitric should have put this into solution if it was representative of the material i started with. So far I am assured that there was no Ag in metal sample but still attempting to get last of metal to completely dissolve into solution with difficulty.


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## anachronism (Feb 22, 2018)

If you didn't get any silver Chloride then that shows that the XRF report of silver was wrong. I would respectfully suggest that it's therefore likely that the rest of the XRF report was just as wrong. 

That given I would test your solution with DMG and see if you get a result from that but at this stage it isn't looking positive.

Jon

Edit: As an aside I use an XRF myself as part of my business and one made by the same manufacturer as the one of which you showed pictures. The comments on here about these reports having the potential to be wildly wrong are correct. 

For some reason Rhodium "pops up" on readings with appalling regularity where there is no Rh present.


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## g_axelsson (Feb 22, 2018)

Hehe, by "taking a sample" I meant a few gram, not 250. That's a lot sized sample.  

The reason we take small samples are that we can tell if there is silver in a metal powder from a 5g sample faster than processing a 250g and with less chemicals used and less waste that needs to be treated in the end.

At least it is quite clear that there are no huge amount of silver (or led or mercury) in your material. You still have an undissolved part. Can you filter off and clean the remaining solids after it stops reacting with the acid. Then take a picture of it and let us have a look.

For the remaining undissolved solids I would start by adding (not much more than covering it) a bit of nitric acid (about 30% concentration, 67% concentrated nitric acid reacts slower than diluted acid). If there is a reaction or if the acid changes color then it still reacts with the nitric acid and more patience is needed.

When the sample doesn't react with nitric acid I would then add some HCl (add double the volume already in the beaker), this would create aqua regia and dissolve any remaining palladium, platinum or gold. Add it slowly as the reaction could get quite vigorous and create a boil-over. 
If there is any precious metals in it a stannous test should reveal it. By the way, have you tested your stannous so it hasn't gone bad? 

Göran


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## truthmatters (Feb 22, 2018)

Hi Göran
My Stannous chloride is about 10 days old. The tin I used was from tin fishing weights but have since ordered some along with the DVD on PGM refining, still haven't received them in the mail. I could make up a new batch of stannous chloride if not in the mail today.
When it stops I will proceed as you have described. I am seeing a minute white substance forming in the bottom. Will get picture if possible.


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## anachronism (Feb 22, 2018)

Ten days old is nothing - it'll be fine.


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## snoman701 (Feb 22, 2018)

Why not just add copper to the nitrate solution? If you get a precipitate, you can expect it to be a PGM, as you've already shown there is no silver in there. Given how concentrated the nitrate solution is, if it's there, it should cement.


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## truthmatters (Feb 22, 2018)

I set the beaker from this morning on a glass shelf and took pictures of the grayish material settled in the bottom. You can still see a small amount of the base metal and the bottom is now covered with this gray matter.


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## galenrog (Feb 22, 2018)

I’be been following this thread with some interest since it started. I noticed something that I have a question about. Truthmatters stated that he makes his Stannous Chloride with tin fishing weights. Since tin fishing weights I am familiar with are a bismuth/tin alloy, typically about 55/45, would bismuth have any affect on test results? Or are the fishing weight used pure tin?


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## truthmatters (Feb 22, 2018)

All base metal has now gone into solution and this is whats left.


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## truthmatters (Feb 22, 2018)

So my conclusion is this, as interesting as it was and for the knowledge I have pickup it has been priceless. As for what came out of the beaker regardless of what it happens to be, the cost of time and materials can in no way equal up to what value it may hold. Good and valuable lesson for myself and anyone else that may travel down this lonely road. To all who put up with me through the many days of this process, I thank you for your help and understanding. Your knowledge of these processes in unequaled to non other and a great resource for anyone wishing to dip their toes into refining PM's. I am looking forward to getting back to doing more refining again one day soon. 
BTW any ideas of what I have in the test tube so I can label it for future use or does it go to the hazmat recycle?

Thank Bill


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## nickvc (Feb 23, 2018)

I’d suggest to pour off the solution and then dissolve in AR and then test with stannous or if you have had enough of this project put it all in your stockpot.


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## g_axelsson (Feb 23, 2018)

nickvc said:


> I’d suggest to pour off the solution and then dissolve in AR and then test with stannous or if you have had enough of this project put it all in your stockpot.


I second that, a test-tube with AR is a decent sized sample. It will tell everything about the possibility of precious metals with a stannous test.

As for the gray remnants, only small amounts of tin in a nitric solution could make quite a large volume of pale gray tin hydroxides. That is my guess on what it is.

It's been a bumpy ride this thread, but in the end we managed to get together and examine the material in a logical and scientific way. We all wish we have more gold than we do, but to be able to look beyond personal wishes and find the truth is a gain by it self, no matter what comes out of the beaker in the end.

I hope I didn't treat you too harsh, truthmatters.  

Göran


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## truthmatters (Feb 23, 2018)

Added AR and the gray substance went into solution, stannous test was neg for any PM
Thanks again
Bill


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