Macgiver
Member
lazersteve said:
Hey LSteve,
Can you direct me to some good instructions on using zink and HCl to convert my 3 pounds of Ir salts? Not looking forward to all the smoke and time involved calcining.
Thank you mucho.
CW
Calcining colored PGM powders.
- Thread starter Quirkzunc
- Start date
Help Support Gold Refining Forum:
Hey LSteve,
Can you direct me to some good instructions on using zink and HCl to convert my 3 pounds of Ir salts? Not looking forward to all the smoke and time involved calcining.
Thank you mucho.
CW
Macgiver
Member
Thank you.
adam_mizer
Well-known member
- Joined
- Nov 4, 2010
- Messages
- 176
For the zinc, I use the shavings and it took quite some time.
Was trying to think of a way to make those shavings into powder.
I had in a large coffee pot 7 cups of the hcl/cl and PGM.
It took 90 shavings of zinc, over an estimated 1.5hr maybe less?? time to drop the PGM's.
About 5 shavings plus at a time because the foam it creates from reaction was indication of how much zinc can react at one time (depends on the size of your shavings).
Has anyone ever tried putting zinc metal shavings into a coffee bean grinder to try to make powder?
The zinc in powder form will react much quicker.
John
Was trying to think of a way to make those shavings into powder.
I had in a large coffee pot 7 cups of the hcl/cl and PGM.
It took 90 shavings of zinc, over an estimated 1.5hr maybe less?? time to drop the PGM's.
About 5 shavings plus at a time because the foam it creates from reaction was indication of how much zinc can react at one time (depends on the size of your shavings).
Has anyone ever tried putting zinc metal shavings into a coffee bean grinder to try to make powder?
The zinc in powder form will react much quicker.
John
Iridium cannot be reduced quantitatively with zinc. You need to use magnesium or hydrazine or hydrogen.
John,
If you are getting large amounts of foaming when usng zinc turnings check to see if your ammonium chloride is the 'treated' or 'untreated' variety.
A few quick tests to check:
1) Add NH4Cl to water in a test tube and shake. A sudsy, foamy layer on top means you most likely have treated powder.
2) Does the NH4Cl flow freely like table salt? If yes you most likely have treated powder. Untreated powder clumps into chunks over time, but breaks apart easily.
3) When you precipitate your PGMs do they float on on top in a froth or sink like a rock? Treated NH4Cl will produce a PGM salt that floats.
4) Does your vacuum filtered colored PGM salt look porus and spongy or tightly packed and smooth? Treated NH4Cl produces the fluffy spongy stuff.
If you have the treated stuff ditch it for some untreated NH4Cl and your foaming issues will be greatly reduced.
On the subject of the size of the zinc:
The fine mesh zinc reacts way too quickly and produces a collodial suspension of PGM metal. It's hard to settle, filter, and rinse from filters. Most zinc powder has Cab-O-Sil (SiO2) added as a shipping stabilizer. This junk fouls up your filters and prevents complete dissolution of the resulting PGMs.
Zinc turnings are like small cornets (curled up sheets of zinc) with a consistent thickness and several layers of turns. These are ideal for reducing PGM salts and solutions.
Shavings are simply flakes or chips of zinc. The smaller the surface area of the zinc, the faster it dissolves and the more the solution foams due the the evolution of hydrogen gas. This is why turnings are preferred, they produce a gray/black heavy spongy mass of easily rinsed and filtered PGM metal.
One other key aspect of the use of zinc turnings as a reducing agent for PGM salts is the concentration of the muriatic acid. If your solution is over 10% acid you will dissolve the zinc way too fast and the solution will boil due to the large amount of heat and gas evolved. Start with a 5% solution and add zinc and acid only after the intial reaction ceases. Your reaction should be a steady fizzing not a violent foam over. The use of this methodology produces a good quality easy to handle product.
The only other variation I have witnessed in the results come from the use of different the purity of the feedstock of colored powder. Dirty feedstocks result in a finely divided darker colored (black) powder.
Steve
If you are getting large amounts of foaming when usng zinc turnings check to see if your ammonium chloride is the 'treated' or 'untreated' variety.
A few quick tests to check:
1) Add NH4Cl to water in a test tube and shake. A sudsy, foamy layer on top means you most likely have treated powder.
2) Does the NH4Cl flow freely like table salt? If yes you most likely have treated powder. Untreated powder clumps into chunks over time, but breaks apart easily.
3) When you precipitate your PGMs do they float on on top in a froth or sink like a rock? Treated NH4Cl will produce a PGM salt that floats.
4) Does your vacuum filtered colored PGM salt look porus and spongy or tightly packed and smooth? Treated NH4Cl produces the fluffy spongy stuff.
If you have the treated stuff ditch it for some untreated NH4Cl and your foaming issues will be greatly reduced.
On the subject of the size of the zinc:
The fine mesh zinc reacts way too quickly and produces a collodial suspension of PGM metal. It's hard to settle, filter, and rinse from filters. Most zinc powder has Cab-O-Sil (SiO2) added as a shipping stabilizer. This junk fouls up your filters and prevents complete dissolution of the resulting PGMs.
Zinc turnings are like small cornets (curled up sheets of zinc) with a consistent thickness and several layers of turns. These are ideal for reducing PGM salts and solutions.
Shavings are simply flakes or chips of zinc. The smaller the surface area of the zinc, the faster it dissolves and the more the solution foams due the the evolution of hydrogen gas. This is why turnings are preferred, they produce a gray/black heavy spongy mass of easily rinsed and filtered PGM metal.
One other key aspect of the use of zinc turnings as a reducing agent for PGM salts is the concentration of the muriatic acid. If your solution is over 10% acid you will dissolve the zinc way too fast and the solution will boil due to the large amount of heat and gas evolved. Start with a 5% solution and add zinc and acid only after the intial reaction ceases. Your reaction should be a steady fizzing not a violent foam over. The use of this methodology produces a good quality easy to handle product.
The only other variation I have witnessed in the results come from the use of different the purity of the feedstock of colored powder. Dirty feedstocks result in a finely divided darker colored (black) powder.
Steve
adam_mizer
Well-known member
- Joined
- Nov 4, 2010
- Messages
- 176
Steve,
I did this per your video.
First stage, HCl/Cl, filtered from any debree's.
Addition of Na2CO3 until a light layer of white dropped on bottom.
Addition of zinc turnings until all PGM's have dropped out.
Accumulation on bottom but a lot of black in solution. Filter is catching all the powder.
Filtered solution is very light light green and clear.
All this appeared like the DVD.
Only diference was zinc turnings verses powdered zinc.
I inserted as much zinc as I could deal with the reaction making hydrogen and the foam created.
After all settled is when I filtered the solution.
Now have to watch DVD again and check the next steps.
Before I proceed to these next steps I have over a gallon and half of solution to add soda ash/zinc. Turning take a long time.
Oh Yeah! One question what bothered me was after the first initial filter from maybe carbon and debree's I got a bunch of a light blue powder. Any ideas on this light blue powder?
I did this per your video.
First stage, HCl/Cl, filtered from any debree's.
Addition of Na2CO3 until a light layer of white dropped on bottom.
Addition of zinc turnings until all PGM's have dropped out.
Accumulation on bottom but a lot of black in solution. Filter is catching all the powder.
Filtered solution is very light light green and clear.
All this appeared like the DVD.
Only diference was zinc turnings verses powdered zinc.
I inserted as much zinc as I could deal with the reaction making hydrogen and the foam created.
After all settled is when I filtered the solution.
Now have to watch DVD again and check the next steps.
Before I proceed to these next steps I have over a gallon and half of solution to add soda ash/zinc. Turning take a long time.
Oh Yeah! One question what bothered me was after the first initial filter from maybe carbon and debree's I got a bunch of a light blue powder. Any ideas on this light blue powder?
The primary topic of this thread is calcining PGM powders so I was under the assumption that you were working with the colored powders when using your zinc.
After filming the DVD I have made numerous posts on the subject of zincing out the leach solution. Search the forum for these posts. I have modified the way that I do this myself since filming the DVD. The key difference is that I don't use soda ash any longer. Instead I use a diluted muriatic acid in the leach reaction.
The foaming should be reduced if you eliminate the use of soda ash in the reaction. The blue powder is likely a base metal hydroxide formed by the soda ash and contaminating metals.
Where did you get your zinc from?
Steve
After filming the DVD I have made numerous posts on the subject of zincing out the leach solution. Search the forum for these posts. I have modified the way that I do this myself since filming the DVD. The key difference is that I don't use soda ash any longer. Instead I use a diluted muriatic acid in the leach reaction.
The foaming should be reduced if you eliminate the use of soda ash in the reaction. The blue powder is likely a base metal hydroxide formed by the soda ash and contaminating metals.
Where did you get your zinc from?
Steve
adam_mizer
Well-known member
- Joined
- Nov 4, 2010
- Messages
- 176
Yes its off topic!
Ran a second batch it was much quicker this time. Foam settled very fast. Less soda ash was used.
Main bulk of powders settled much faster.
The light blue powders filtered from HCl/Cl were maybe a coating the manufacturer puts on the outside of a honeycomb. They dried a tan color in the filters.
The turnings were purchased from you.
I imagine all is going along as indicated, its very foreign to understand whats going on for the first time.
Will store all powders, until ready for calcining.
Maybe there are some posts for modified methods not using soda ash, as you suggest the diluted Hcl.
Also these few posts maybe deleted/removed from this topic. No harm done I hope.
Ran a second batch it was much quicker this time. Foam settled very fast. Less soda ash was used.
Main bulk of powders settled much faster.
The light blue powders filtered from HCl/Cl were maybe a coating the manufacturer puts on the outside of a honeycomb. They dried a tan color in the filters.
The turnings were purchased from you.
I imagine all is going along as indicated, its very foreign to understand whats going on for the first time.
Will store all powders, until ready for calcining.
Maybe there are some posts for modified methods not using soda ash, as you suggest the diluted Hcl.
Also these few posts maybe deleted/removed from this topic. No harm done I hope.
