Lightspeed
Well-known member
Hi all,
help is needed from experienced members please. My assay result shows I have some trace elements which I am struggling to quantify in my assay report.
This assay is on crystal silver from stainless steel silver cell runs.
Loose description of my process:
1:Clean glassware with Bar keepers friend, triple rinse with distilled water.
2igest clean scrap in 50/50 nitric &/DW(source is small amount of jewellery, sterling pre decimal junk silver coins, hallmarked sterling in various forms mostly antique)
3:Filter; either vacuum or gravity
4recipitate with clean 110 grade copper slab
5:Rinse,rinse,rinse,rinse, you get the picture,test samples separately for Ag nitrate & ammonia Cu test etc and rinse, rinse, rinse etc
6:Vacuum filter rinse
7ry
8:Melt in Morgan salamander clay graphite crucible, no flux in LPG fired furnace
9:Shot into iced tap water
10:Rinse shot and dry on hotplate
Electrolytic cell
1: Electrolyte composition; Silver crystal from previous run or silver shot, electrolyte test for palladium with DMG. Electrolyte colour is either colourless or slight tint of yellow. Electrolyte is heated down to nil active nitric on remaining silver digest. Ag concentration of 200g pl minimum x 4L
2:Vacuum filter electrolyte with Whatman No 5 paper twice through same paper.
3:Clean inside of 300series SS bowl and rinse with DW x3
4:Rinse all cell running equipment in contact with electrolyte several times in DW, Muslin filter in dilute nitric and DW wash and x3 rinse
5:RUN cell 4-5 Amp @3-4V
(note** at worst electrolyte condition after 2 kilo run is slightly tinted greenish, certainly not enough colour to indicate possible co deposition issues)
Crystal
1:Harvest and rinse, you know the drill, rinse and rinse and rinse, test sample for silver nitrate with hcl and rinse as needed, dry crystal and store or re-run according to needs.
Well as a rough in you get the picture, I may have missed a few small details but that's pretty much me for silver runs.
So obviously I need help with my contaminants, and where and at what steps and points where i must apply extra work, or extra processes, i already spend a small fortune on rinsing alone, and I don't know where I am getting Calcium and Potassium from. I am obviously still learning from all my experiences to this point and have a way to go yet.
My DW is not homemade and is store bought deionization process, I do not get Ag chloride from its use at any stage.
There is much room for improvement with my process management, I hope the ones who shoot for 4N silver can help.
By the way, this Ag shoots 99.99 on two bullion dealers handheld XRF's, its not good enough for me 99.95 is not where its at for me, I need 4N, because its my goal and my standard I set for myself.
My results are listed below from 2 separate samples to the right of BATCH-00 corresponding to the elements and listed in ppb.
edit due to formatting.
help is needed from experienced members please. My assay result shows I have some trace elements which I am struggling to quantify in my assay report.
This assay is on crystal silver from stainless steel silver cell runs.
Loose description of my process:
1:Clean glassware with Bar keepers friend, triple rinse with distilled water.
2igest clean scrap in 50/50 nitric &/DW(source is small amount of jewellery, sterling pre decimal junk silver coins, hallmarked sterling in various forms mostly antique)
3:Filter; either vacuum or gravity
4recipitate with clean 110 grade copper slab
5:Rinse,rinse,rinse,rinse, you get the picture,test samples separately for Ag nitrate & ammonia Cu test etc and rinse, rinse, rinse etc
6:Vacuum filter rinse
7ry
8:Melt in Morgan salamander clay graphite crucible, no flux in LPG fired furnace
9:Shot into iced tap water
10:Rinse shot and dry on hotplate
Electrolytic cell
1: Electrolyte composition; Silver crystal from previous run or silver shot, electrolyte test for palladium with DMG. Electrolyte colour is either colourless or slight tint of yellow. Electrolyte is heated down to nil active nitric on remaining silver digest. Ag concentration of 200g pl minimum x 4L
2:Vacuum filter electrolyte with Whatman No 5 paper twice through same paper.
3:Clean inside of 300series SS bowl and rinse with DW x3
4:Rinse all cell running equipment in contact with electrolyte several times in DW, Muslin filter in dilute nitric and DW wash and x3 rinse
5:RUN cell 4-5 Amp @3-4V
(note** at worst electrolyte condition after 2 kilo run is slightly tinted greenish, certainly not enough colour to indicate possible co deposition issues)
Crystal
1:Harvest and rinse, you know the drill, rinse and rinse and rinse, test sample for silver nitrate with hcl and rinse as needed, dry crystal and store or re-run according to needs.
Well as a rough in you get the picture, I may have missed a few small details but that's pretty much me for silver runs.
So obviously I need help with my contaminants, and where and at what steps and points where i must apply extra work, or extra processes, i already spend a small fortune on rinsing alone, and I don't know where I am getting Calcium and Potassium from. I am obviously still learning from all my experiences to this point and have a way to go yet.
My DW is not homemade and is store bought deionization process, I do not get Ag chloride from its use at any stage.
There is much room for improvement with my process management, I hope the ones who shoot for 4N silver can help.
By the way, this Ag shoots 99.99 on two bullion dealers handheld XRF's, its not good enough for me 99.95 is not where its at for me, I need 4N, because its my goal and my standard I set for myself.
My results are listed below from 2 separate samples to the right of BATCH-00 corresponding to the elements and listed in ppb.
edit due to formatting.