Here is one for the experts here

[truthmatters]

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.

 

[truthmatters]

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

 

[nickvc]

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.

 

[snoman701]

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

 

[FrugalRefiner]

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

 

[nickvc]

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.

 

[truthmatters]

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

 

[snoman701]

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

 

[Lino1406]

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

 

[Shark]

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

 

[truthmatters]

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

 

[kurtak]

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

 

[truthmatters]

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

 

[FrugalRefiner]

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

 

[truthmatters]

Thanks Dave

 

[truthmatters]

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

 

[Lino1406]

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

 

[g_axelsson]

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

Göran

 

[anachronism]

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

 

[kurtak]

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

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