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As a note on the appearance of platinum,rhodium or palladium in your silver it can be because the manufacturers are now producing silver items made to look like white gold, cost of metals, it is far from uncommon these days for items to be plated with any of the mentioned metals to give it that white appearance and palladium was used as a cheaper substitute for rhodium.
 
I cemented the silver from the dark yellow electrolyte this evening.

The silver cementing out appeared much draker than I am used to seeing.

The silver in the container to the right is from freshly digested sterling and 925 jewelry.

The container in the middle is the dark yellow electrolyte mixed with some dissolved sterling and 925 material.

Also, before I put the dark yellow solution into the container to cement out the silver, I did another stannous chloride test.

This time it turned a violet to purple color (see photo).

I am still studying Hoke on how to identify metals in solution.

I got my DMG today, but I have not had a chance to make some test solution. I did save about 2ml of the dark yellow electrolyte for later testing with the DMG.

Thanks - kadriver
 

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kadriver said:
Here is the last stannous chloride test that I did tonight from the dark yellow electrolyte.

The color is violet or purple - can this be gold?
No. What you're seeing is silver (photosensitive). It is unreasonable to expect gold in a nitrate solution. That doesn't happen.

The color reaction when you apply the drop of stannous chloride is the color to read.

You can confirm it's palladium with DMG---you'll get a distinct yellow precipitate. Where you have a lot of silver in solution along with palladium, it may pay to add a drop of HCl to the test before using DMG (test in a spot plate cavity). That will precipitate the silver as silver chloride. Test the resulting solution by dragging a drop from one cavity to another with a glass rod.

I highly recommend you get in the habit of testing with a spot plate. You are limited with cotton swabs. So much so that I NEVER used them. No need. They're a waste of resources and complicate the recovery of the miniscule amounts of values lost in testing (washed to the stock pot with ease from a spot plate).

Harold
 
I will order a spot plate today.

Also, I will make some DMG test solution and test the dark yellow silver nitrate electrolyte - then post the results.

I ended up mixing all the silver together and washing with boiling distilled water.

I am curious to see what will be left in the slimes of the anode basket after this batch of silver is put through the cell.

I added some nitric acid to the anode basket slimes from some earlier cell clean outs.

Using the process Harold posted, I am going to process these slimes and post what I recover from them.

This will be my first time processing anode basket slimes.

Thank you - kadriver
 
Here is a picture of the spot plate I just purchased on Ebay for $7.00 - I bought two of them.

It is made of glazed ceramic, the back is left unglazed.

It measures about 3.5 inches by 4.5 inches.

This should serve well to test solutions for dissolved metals.

kadriver
 

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I made up a batch of DMG test solution.

I put abour 1/2 gram in a small flask, added some distilled water and then boiled.

It all dissolved, then some crystals formed after it cooled a bit. I must filter out the crystals.

Before the crystals formed I was able to do the test on the dark yellow silver cell electrolyte.

I divided the amount I saved equally between two test tubes. Then added DMG solution to one. DMG test is on the left in the photo.

Does this test indicated a positive result for the presence of palladium? There was a light pricipitate in the solution - according to my Hoke, this is confirmation of palladium.

kadriver
 

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kadriver said:
Here is a picture of the spot plate I just purchased on Ebay for $7.00 - I bought two of them.
Well done! They will serve your needs perfectly.

In regards to your DMG test, if you introduced enough test solution, when the resulting material settles, the solution should be clear of color. The precipitant is canary yellow. Might not hurt to test with stannous chloride, too. If nothing else, it's a good exercise and learning experience.

Harold
 
This thread is excellent!

If it were not for several of the answers and tests as well as the natures of palladium and platinum metals in solutions I would have not bothered to retest some of my disgarded wastes.
This thread put me on a roll and certain of my disgarded wastes are dropping PM's right now.

Keep up the good work and questions/answers as they are very inspiring to further develope my skills.
Thank you kadriver for your informative process inquisitive nature show and tell and the answers that follow along from everyone.

John
 
Great reading! This thread needs to be bumped!

I'm also curious, kadriver, was it palladium in your electrolyte? Did the liquid in the test tube lose it's color when the precipitate settled? What other metals did you find in your slimes?

Maybe you wrote another thread about that... if I find one I'll add a link here.

Göran
 
I too am hungry for more info about how this all worked out. Please update this thread if you get the chance kadriver.
 
g_axelsson said:
Great reading! This thread needs to be bumped!

I'm also curious, kadriver, was it palladium in your electrolyte? Did the liquid in the test tube lose it's color when the precipitate settled? What other metals did you find in your slimes?

Maybe you wrote another thread about that... if I find one I'll add a link here.

Göran

The material in the electrolyte was palladium. It's been a while but I think I put the used electrolyte in a 4 liter beaker and added DMG that had been dissolved in boiling distilled water.

The DMG precipitated the palladium in the form of a bright yellow material that I was able to filter out easily via gravity filtration through a regular glass funnel using a #1 Whatman 185mm filter paper.

The color of the liquid was green going into the funnel (probably from the suspended yellow palladium precipitation), and the filtrate (liquid in the receiving container below the funnel) was a vivid blue color.

I rinsed the palladium precipitate with cold distilled water while it was still in the funnel to get out as much silver nitrate and copper nitrate as possible.

Then I removed the filter paper that contained the bright yellow precipitate and placed it on some paper towels.

I have a stack of these filters each with palladium precipitate and some day in the future I'm going to refine the palladium.

kadriver

Edited once to add a thread reference

Here is a post that has a video that shows how I removed the dissolved palladium from the silver cell electrolyte:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=50&t=19004&p=192260&hilit=Dissolved+Palladium+from+Electrolyte#p192260
 
If I remember correctly, this electrolyte turned green instead of the usual blue color. The blue is from dissolved copper.

In this particular case I had added some nitric acid to the cell because crystal growth (and consumption of silver shot in the anode basket) had slowed way down. I was trying to increase the silver nitrate concentration by adding nitric acid to dissolve some of the silver crystal that had formed in the cell electrolyte.

The next day after adding the acid I noticed that the electrolyte had turned green instead of the usual blue color that I was used to seeing.

I concluded that the nitric acid that I had added the day before had dissolved some palladium that was trapped in the anode basket. I do not know if this conclusion is correct or not, but I have recovered palladium from my silver cell slimes by dissolving the slimes in dilute nitric acid.

Small amounts of palladium dissolved in dilute nitric acid will produce a yellow colored solution. Copper dissolved in nitric will produce a blue colored solution.

If one mixes a blue solution with a yellow solution the result is a green solution.

Since that time I have never added nitric acid to my silver cell electrolyte again. To increase the concentration of the silver nitrate I dissolve some pure silver crystal that I keep in reserve, gently evaporate off some of the liquid, then add that solution to my silver cell electrolyte.

I think I read on the forum somewhere that there are specific pH ranges for silver cell electrolyte. If these ranges are maintained in the cell then the palladium won't dissolve from the anode basket.

But I think a small amount of palladium will get in the electrolyte no matter what precautions are taken.

kadriver
 
I do not know how this contamination got in there.

Here is the test I did with fresh stannous chloride solution this evening.

The four photos are a series of pictures about 2 seconds apart as I dropped the stannous chloride onto the sample of spent electrolye (the dark yellow liquid from my silver cell).

It obviously tested positive for something. I do not know what this test indicates. It turned a brown color very rapidly in about 5 seconds.

Then it stopped and remained as pictured.

The silver nitrate showed a very faint yellow color.

I tested this same silver nitrate solution two night ago and it was much darker that the test result from tonight.

I do not know what it is. I am hoping that the forum members can tell what it might be from looking at the photos.

This is all very exciting - like starting all over again.

I feel a bit overwhelmed because i am not certain what I should do next.

I probably need to study some more and take a break from it for a while.

The nice thing about it is that it will still be there for me tomorrow. It isn't going anywhere.

Thanks for looking

kadriver
How do you know when to replace your cell electrolyte? and how do you know what % of silver you have in your electrolyte?
 

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