Palladium Refining Complete Process - VIDEO

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kadriver
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Palladium Refining Complete Process - VIDEO

Postby kadriver » April 17th, 2018, 2:11 pm

Here is my latest attempt to refine my collection of palladium derived from silver nitrate solutions with dimethylgloxime (DMG). I experience a runaway reaction that spews hot AR solution out of the top the beaker!

Part 1 of 2:
https://youtu.be/XTVJcOUl8bE

Part 2 of 2:
https://youtu.be/IE23cbEoWAU


Thank you
kadriver (sreetips)
edited once to include link to part 2
Last edited by kadriver on April 19th, 2018, 5:29 pm, edited 1 time in total.
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Re: Palladium Refining Complete Process - VIDEO

Postby g_axelsson » April 17th, 2018, 4:39 pm

Nice video and a dramatic foam over. :D

Two comments...
1. You could do something about the foam over, removing the watch glass would have cooled the top down and made it less severe, you wouldn't have had that fountain of foam shooting out. The dryer air also helps popping the bubbles in the foam when it dries out.
The other thing you can do when having a boil over is to use a spray bottle with water, it cools the surface of the foam and decrease the surface tension so the big bubbles easily breaks and the volume goes down.
2. 40 volume of hydrogen peroxide isn't the same as 40%. It's more like 12% strength. http://goldrefiningwiki.com/mediawiki/i ... n_peroxide

Thanks for the video, eagerly waiting for the sequel to find out who the killer is.

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Re: Palladium Refining Complete Process - VIDEO

Postby kadriver » April 18th, 2018, 12:44 am

g_axelsson wrote:Nice video and a dramatic foam over. :D

Two comments...
1. You could do something about the foam over, removing the watch glass would have cooled the top down and made it less severe, you wouldn't have had that fountain of foam shooting out. The dryer air also helps popping the bubbles in the foam when it dries out.
The other thing you can do when having a boil over is to use a spray bottle with water, it cools the surface of the foam and decrease the surface tension so the big bubbles easily breaks and the volume goes down.
2. 40 volume of hydrogen peroxide isn't the same as 40%. It's more like 12% strength. http://goldrefiningwiki.com/mediawiki/i ... n_peroxide

Thanks for the video, eagerly waiting for the sequel to find out who the killer is.

Göran


I was going to yank the cover off but I decided in an instant to just let it go and make sure to get it filmed as it blew. I was kind of ticked when it happened, but after viewing the video I realized that it made an incredible example what not to do and that it should be kept in the video. I could have edited the entire sequence out and no one would have known that it even happened.

I've evaporated the Pd solution down to 150ml and added the ammonium chloride. There was Pt in with the Pd. I almost gasped when the platinum started to precipitate out when I added the ammonium chloride. Coming from DMG i firgured that there would be zero platinum. I've got the Pt filtered out and I'm ready to gas the Pd solution with chlorine to get the ammonia soluble Pd precipitate. It should be calcined and the video ready to post by tomorrow evening.
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Re: Palladium Refining Complete Process - VIDEO

Postby Palladium » April 18th, 2018, 12:54 am

Bigger beakers are your friend! 2,000 ml would have been perfect!
Occasionally i beak out the big guns and use my 4,000 ml beakers.
The paper residues or pulp help keep the bubbles suppressed and allows the head to build pressure. Sort of like paper wadding in a shot gun shell!

When i have a boil over if nothing gets outside the containment vessel i use water to wash the beaker of into the catch vessel. Then i wash the catch vessel back into the beaker. Then i evaporate the excess water if needed to resume processing. What happens is the water flashes off from the solution on the outside of the beaker and on the catch vessel. This will cause metal salts to adhere to the surfaces that can't be just wiped off. Water will put them back into solution and remove the majority from the surface better than just wiping it. All that paper just adds more to your processing. In the end you're going to have to use excess water to wash all the solution from all that filter pulp anyway.

I still have the occasional boil over myself! :D
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Re: Palladium Refining Complete Process - VIDEO

Postby kadriver » April 18th, 2018, 1:34 am

Palladium wrote:Bigger beakers are your friend! 2,000 ml would have been perfect!
Occasionally i beak out the big guns and use my 4,000 ml beakers.
The paper residues or pulp help keep the bubbles suppressed and allows the head to build pressure. Sort of like paper wadding in a shot gun shell!

When i have a boil over if nothing gets outside the containment vessel i use water to wash the beaker of into the catch vessel. Then i wash the catch vessel back into the beaker. Then i evaporate the excess water if needed to resume processing. What happens is the water flashes off from the solution on the outside of the beaker and on the catch vessel. This will cause metal salts to adhere to the surfaces that can't be just wiped off. Water will put them back into solution and remove the majority from the surface better than just wiping it. All that paper just adds more to your processing. In the end you're going to have to use excess water to wash all the solution from all that filter pulp anyway.

I still have the occasional boil over myself! :D


The first thing that popped into my mind when I was watching it rise up: "I should have used a bigger beaker"

I used hydrochloric acid to rinse the inside of the beaker, could have used it on the outside as well. That's a good suggestion for my next boil over.
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Re: Palladium Refining Complete Process - VIDEO

Postby rickzeien » April 18th, 2018, 9:40 am

Thank you for posting your videos. I am just beginning to process some e escrap. I have nitric acid but will not use it until my fume hood is installed.

For now I process foils in an outdoor environment. I have a box fan that I use on low to blow any fumes away from me. (No close neighbors or anybody in the vicinity)

I use the same respirator that you do. What cartridge or cartridge(s) do you use?

Again thanks for the informative videos and post.

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Re: Palladium Refining Complete Process - VIDEO

Postby rickzeien » April 18th, 2018, 9:54 am

I just purchased a fume hood. It is a Labconco 47 inch wide. Very simular to yours.

It did not come with a base cabinet or a bottom. What do you use for your base cabinet and what is that shelf made of.

Thanks.

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Re: Palladium Refining Complete Process - VIDEO

Postby kadriver » April 19th, 2018, 3:00 pm

rickzeien wrote:Thank you for posting your videos. I am just beginning to process some e escrap. I have nitric acid but will not use it until my fume hood is installed.

For now I process foils in an outdoor environment. I have a box fan that I use on low to blow any fumes away from me. (No close neighbors or anybody in the vicinity)

I use the same respirator that you do. What cartridge or cartridge(s) do you use?

Again thanks for the informative videos and post.


the filters are P95 3M
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Re: Palladium Refining Complete Process - VIDEO

Postby kadriver » April 19th, 2018, 3:01 pm

rickzeien wrote:I just purchased a fume hood. It is a Labconco 47 inch wide. Very simular to yours.

It did not come with a base cabinet or a bottom. What do you use for your base cabinet and what is that shelf made of.

Thanks.


i built a table into the wall with firm braces to hold the weight.
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Re: Palladium Refining Complete Process - VIDEO

Postby kadriver » April 19th, 2018, 3:03 pm

OK, here is part two of the video:

https://youtu.be/IE23cbEoWAU

kadriver
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Re: Palladium Refining Complete Process - VIDEO

Postby rickzeien » April 19th, 2018, 3:03 pm

Thanks for the info.

Sent from my LG-H872 using Tapatalk

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Re: Palladium Refining Complete Process - VIDEO

Postby cuchugold » April 21st, 2018, 6:02 am

"Coming from DMG i firgured that there would be zero platinum."

I also learned the hard way. To get pure palladium with DMG you must get rid of the gold and platinum first. The good news is that if you have a little palladium contaminating Pt or Au solutions, DMG will scavenge the palladium out, along with some gold and platinum.
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Re: Palladium Refining Complete Process - VIDEO

Postby anachronism » April 22nd, 2018, 8:42 am

Palladium wrote:Bigger beakers are your friend! 2,000 ml would have been perfect!
Occasionally i beak out the big guns and use my 4,000 ml beakers.


2 litre and 3 litre tall form beakers rock. A litre of liquor in a 3 litre tall form has a serious problem trying to boil over. I'd seriously recommend using those, or the 2 litres ones for smaller quantities. I've not had one boil over since I started using them. I tend to to use 5 litre with no more than 2.5 litres of liquor for batch jobs and the same applies- you have to work REALLY hard or do something incredibly dumbass to get them to boil over.

Regards

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Re: Palladium Refining Complete Process - VIDEO

Postby cuchugold » April 23rd, 2018, 6:51 am

That ammonia / HCL cycle in video 2 was really nice to watch. Gorgeous colors. :G
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