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