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jeneje

Well-known member
Joined
Jan 23, 2011
Messages
1,176
Location
Knoxville Tennessee
Hey guys, i will try to explain this, a few months back i had some fixer, i added lye to it and i thought it did nothing. So i put it in my shed under some other things and i found it today and there were black sludge in the bottom - a bunch of sludge. So i took a spoon and scooped out a little bit on the spoon end and put into a test jar i have(small baby food jar) added water to it and then added 1ML of HNO3. I got a reaction on contact, as it begain to react i noticed that on top what looked like silver forming, as the reaction slowed there were silver flakes everywhere. The solution turned a light to medium brown color.
My question is - is this silver and is it safe to do this.
Thanks
Ken
Well no reply yet, so i took a pic to add.
 

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Test for silver by adding a drop of salt dissolved in water. If you have silver it will form white silver chloride cloud in the liquid.
 
Filter out your sludge - force dry - incinerate (or oxidize roast in SS pan on burner) treat with warm HCL to remove base metal oxides - if there is silver you will get some AgCL - treat with NaOH to convert AgCL - wash - force dry - treat with nitric - test for silver - if you still have solids after nitric - treat with AR - test for other PMs

Kurt
 
kurt said:
Filter out your sludge - force dry - incinerate (or oxidize roast in SS pan on burner) treat with warm HCL to remove base metal oxides - if there is silver you will get some AgCL - treat with NaOH to convert AgCL - wash - force dry - treat with nitric - test for silver - if you still have solids after nitric - treat with AR - test for other PMs

Kurt
Kurt thanks for your responce, What i got here is somewhat a challange for me. I have attached some pics to help explain. The fixer i was processing came from infared film, I added NaOH and it droped the silver oxides and then i started to process the oxides with HNO3 and i Got a yellow solution. I tested it with DMG and behold it dropped yellow salt in my test tube. OK now i have Pd mixed with my silver. Now to the question How do i seperate the two, It is above my knowedge and help here would be appreicated.
Thanks
Ken
 

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http://www.goldnscrap.com/index.php?option=com_content&view=article&id=62:recovering-palladium-and-silver-from-monolithic-ceramic-capacitors&catid=38:eek:thers&Itemid=50
 
Ken – I may not be the best person to help you here. For one thing the only fixer material I have worked with was an already recovered dried sulfide from regular photo processing & you say yours was a “solution” from infrared film & I have no idea what the make up of that solution is.

GSP or some of the other more experienced members may be of more help here.

Was your starting point a fixer solution – or something in a dry form already recovered from fixer – or the film its self?

Did you do any testing on the solution to start with? (stannous to determine PMs in general – HCL spot test for Ag – DMG for Pd)

Did you test the solution after adding the NaOH?

Was the original solution a nitric solution to which you added NaOH – or – was the nitric a treatment something you did after recovery from the original solution?

Why did you use NaOH as a precip reagent instead of cementing &/or instead of other precip reagents? (like HCL &/or DMG etc. that precip more selectively)

The reason I ask is that NaOH will precip a whole host of base metals as well as PMs

What makes you think the last pic in your post is - "This is the pd that dropped out on it own." (you need a reagent to get a selective drop)


Another words we need more info here.

Please post what it was you had to start with & what you did to the point of getting a sludge from the addition of the NaOH

Kurt
 
kurt said:
Ken – I may not be the best person to help you here. For one thing the only fixer material I have worked with was an already recovered dried sulfide from regular photo processing & you say yours was a “solution” from infrared film & I have no idea what the make up of that solution is.

GSP or some of the other more experienced members may be of more help here.

Was your starting point a fixer solution – or something in a dry form already recovered from fixer – or the film its self?

Did you do any testing on the solution to start with? (stannous to determine PMs in general – HCL spot test for Ag – DMG for Pd)

Did you test the solution after adding the NaOH?

Was the original solution a nitric solution to which you added NaOH – or – was the nitric a treatment something you did after recovery from the original solution?

Why did you use NaOH as a precip reagent instead of cementing &/or instead of other precip reagents? (like HCL &/or DMG etc. that precip more selectively)

The reason I ask is that NaOH will precip a whole host of base metals as well as PMs

What makes you think the last pic in your post is - "This is the pd that dropped out on it own." (you need a reagent to get a selective drop)


Another words we need more info here.

Please post what it was you had to start with & what you did to the point of getting a sludge from the addition of the NaOH

Kurt
Hey Kurt, thanks for the reply. I will try to answer your question here.

Was your starting point a fixer solution – or something in a dry form already recovered from fixer – or the film its self? It was Kodak, here is the MSDS for it containing the make-up. fixerhttp://msds.kodak.com/ehswww/external/result/report.jsp?P_LANGU=E&P_SYS=8&P_SSN=284&P_REP=00000000000000000338&P_RES=212

Did you do any testing on the solution to start with? (stannous to determine PMs in general – HCL spot test for Ag – DMG for Pd) The only test I did was with salt to check for agcl it tested positive. In the beginning.

Did you test the solution after adding the NaOH? No, Not in the beginning, I waited for the drop, it dropped out as a black fine powder.

Was the original solution a nitric solution to which you added NaOH – or – was the nitric a treatment something you did after recovery from the original solution? After the black sludge dropped out NaOH, I filter it - I rinsed the sludge into a container added water and then began to add HNO3 at 2-3-ml at a time from my dropper.

Why did you use NaOH as a precip reagent instead of cementing &/or instead of other precip reagents? (like HCL &/or DMG etc. that precip more selectively) This is a great question and the answer is a lack of knowledge on my part.

What makes you think the last pic in your post is - "This is the pd that dropped out on it own." (you need a reagent to get a selective drop) When the solution I filtered off started to change color to a yellow I tested it with DMG, I added some solution to a test tube and added a few drops of DMG and it dropped out yellow salt in the bottom. The longer it set the deeper the color became. After 24 hours the bottom was covered with the yellow paste/salt.

At this point, i'm not sure how to proceed so i put posted here hoping for help with it.
Thanks
Kurt

Ken
 
Ken - for some reason the link you provided is not working for me so I am still a bit in the dark.

Kurt
 
kurt said:
Ken - for some reason the link you provided is not working for me so I am still a bit in the dark.

Kurt
Hey Kurt, the website is kodak.com go to the second tab(Global Sustainability) and it will load an adobe file. The first one on the list is the correct MSDS for the fixer.
Thanks Kurt
Ken
ps by the way i just filtered of my rinse water and tested with stannous and got a yellow test result, odd. I also went to sammual site on mLcc to read up and looking at his stannous results mine match for pt. Something is wrong with what im doing i know it. Just can't put my finger on it yet, but will figure it out...lol got to its brothering me know.
Also pulled out the Bible on the issue, C.M. Hoke
 
Kurt here is the test pic from the solution the one in the middle is DMG befor rinse, the one to the right is stannous after rinse.
Ken
 

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