WIZZARD
Well-known member
I'm a new member. When reading posts I've looked at as many as possible to resolve my questions, however I have not found a direct answer to my problem. The normal Au reagents, FeSo4, SmB, Oxalic, SO2, drop brown mud, however Pd is suspected to confound the brown drop, because there is lot of it. The starting matrix is not secondary reduced metal scrap.
My solution of Pt/Pd/Ir/Rh/Ru/Au ( little Fe trace Ni Cu,trace Sn, Pb, Ag, Zr, lots of si ) placed into solution with AR using H2O2 as oxidizer, no nitric. Most of these NM are not reduced metal, is the reason they go into solution with modified AR. I use NaOH and sometimes NH3 to raise the pH to 4.5-5.5 to get a brown drop. I know 15% of the starting matrix is NM; 3.3% Au, 6.15% Pt, 2.55% Pd, 3% Rh and 2.55% Ir/Ru/trace Ag. Fe and other base metals in the matrix are hit with pre acid to get rid of them and rinsed well, before using AR. HCL not used as pre treatment as the particle sizes of NM are below 1 micron and this known to place some NM in solution. Inquarting with silver works, however that is another question, another 10 steps, electrochemical Mubuis cells and a lot of time.
Question; As NaOH or NH3 is added to the filtered yellow/orange pH 1 solution a brown drop forms @ 4.5pH, darker brown color at 5.5pH, allowing this to settle over night the solution's pH is close to 6, the color now very dark amber. The brown mud filtered, rinsed with H2O dried with low heat, and when ignited 800F in a stainless steel dish, a gold metal with gray metal to reddish powder residue is visible under the scope. The brown drop is suspected to be 60% Au / 40% Pd brown powder and will not melt at 2115F. Normal reagents for Au seam not to work as the brown drop of Au/Pd may also have a conflicting element locked to their atoms?
I've use NH4Cl to drop the PM as a first stage and get test book orange, to red PM salts. When igniting the salts I notice brown fumes coming from a velvet brown ignition mass toward the end of the ignition, mixed with PM sponge. AuCl is my guess, when oxalic acid added causes a brown residue to form at 900F and the residue is very golden with whitish gray PM looking metal. Remember no nitric was use.
The reason to drop by pH first is to separate Au/Pd first as dealing with the PM solution is easier without the Au.
How to part the Au/Pd brown mud is the question. The brown mud is a hydroxide of Au/Pd, thus is very soluble in weak acid. Got suggestions? Breaking atomic bonds of inner shell electrons must a trick in someone's pocket?
I'm hoping someone has been there done this and has a answer not requiring the involvement capitol investment.
WIZZARD, FNG...FORUM NEW GUY
My solution of Pt/Pd/Ir/Rh/Ru/Au ( little Fe trace Ni Cu,trace Sn, Pb, Ag, Zr, lots of si ) placed into solution with AR using H2O2 as oxidizer, no nitric. Most of these NM are not reduced metal, is the reason they go into solution with modified AR. I use NaOH and sometimes NH3 to raise the pH to 4.5-5.5 to get a brown drop. I know 15% of the starting matrix is NM; 3.3% Au, 6.15% Pt, 2.55% Pd, 3% Rh and 2.55% Ir/Ru/trace Ag. Fe and other base metals in the matrix are hit with pre acid to get rid of them and rinsed well, before using AR. HCL not used as pre treatment as the particle sizes of NM are below 1 micron and this known to place some NM in solution. Inquarting with silver works, however that is another question, another 10 steps, electrochemical Mubuis cells and a lot of time.
Question; As NaOH or NH3 is added to the filtered yellow/orange pH 1 solution a brown drop forms @ 4.5pH, darker brown color at 5.5pH, allowing this to settle over night the solution's pH is close to 6, the color now very dark amber. The brown mud filtered, rinsed with H2O dried with low heat, and when ignited 800F in a stainless steel dish, a gold metal with gray metal to reddish powder residue is visible under the scope. The brown drop is suspected to be 60% Au / 40% Pd brown powder and will not melt at 2115F. Normal reagents for Au seam not to work as the brown drop of Au/Pd may also have a conflicting element locked to their atoms?
I've use NH4Cl to drop the PM as a first stage and get test book orange, to red PM salts. When igniting the salts I notice brown fumes coming from a velvet brown ignition mass toward the end of the ignition, mixed with PM sponge. AuCl is my guess, when oxalic acid added causes a brown residue to form at 900F and the residue is very golden with whitish gray PM looking metal. Remember no nitric was use.
The reason to drop by pH first is to separate Au/Pd first as dealing with the PM solution is easier without the Au.
How to part the Au/Pd brown mud is the question. The brown mud is a hydroxide of Au/Pd, thus is very soluble in weak acid. Got suggestions? Breaking atomic bonds of inner shell electrons must a trick in someone's pocket?
I'm hoping someone has been there done this and has a answer not requiring the involvement capitol investment.
WIZZARD, FNG...FORUM NEW GUY