jaun
Well-known member
I have taken some pictures of my precipitation of Pd with Calcium Hypochlorite (Pool chlorine granules). Here’s what I did:
I dissolved some Pd pins and contact points from telkom scrap in nitric. The solution turned red-brown to almost black, evaporated to syrup, add HCL, repeated 3 times till no more brown fumes. With the final syrup I added HCL till 1L, no water, so it was very concentrated.
I then added 30g ammonium chloride and the solution turned brick orange. I heated to below boiling and added the Calcium Hypochlorite (small amounts at a time lots of stirring). As you can see in the picture, the red powder floats on top like a thick milkshake and some sink to the bottom.
I then filtered the solution and was left with a clear light green solution (see pictures). I tested with stannous and it turned clear and later a faint grey, no Pd!! (I tested before I started the precipitation and it was positive, orange then tuned green).
I then took some of the red powder and reduced to metallic form by cementation, adding 50% HCL and 50% water, and adding an iron nail. Hoke states it her book- page 160. I left it for a few hours, stirring occasionally. The solution turned clear with a grey precipitate, mine turned to Pd flakes (see pictures) I washed it with HCL and lots of water.
The final picture shows some of the Pd (flakes) I have reduced from the red powder, in nitric acid (just to test if it is Pd) Note the orange brown colour Pd makes in nitric.
I’m going to melt it and send it for assay. I’ll let you know what the results are.
I hope you can follow the pictures to the writing, I am writing this before posting the pictures. PS: English is my second language, so it took a long time to write this.
:lol:
I dissolved some Pd pins and contact points from telkom scrap in nitric. The solution turned red-brown to almost black, evaporated to syrup, add HCL, repeated 3 times till no more brown fumes. With the final syrup I added HCL till 1L, no water, so it was very concentrated.
I then added 30g ammonium chloride and the solution turned brick orange. I heated to below boiling and added the Calcium Hypochlorite (small amounts at a time lots of stirring). As you can see in the picture, the red powder floats on top like a thick milkshake and some sink to the bottom.
I then filtered the solution and was left with a clear light green solution (see pictures). I tested with stannous and it turned clear and later a faint grey, no Pd!! (I tested before I started the precipitation and it was positive, orange then tuned green).
I then took some of the red powder and reduced to metallic form by cementation, adding 50% HCL and 50% water, and adding an iron nail. Hoke states it her book- page 160. I left it for a few hours, stirring occasionally. The solution turned clear with a grey precipitate, mine turned to Pd flakes (see pictures) I washed it with HCL and lots of water.
The final picture shows some of the Pd (flakes) I have reduced from the red powder, in nitric acid (just to test if it is Pd) Note the orange brown colour Pd makes in nitric.
I’m going to melt it and send it for assay. I’ll let you know what the results are.
I hope you can follow the pictures to the writing, I am writing this before posting the pictures. PS: English is my second language, so it took a long time to write this.
:lol:
