Help with what process to use on my first project.

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Harold,

I think that, due to the fact that some people are sensitive to nickel, palladium is sometimes used as a migration barrier coating underneath the gold. It seems to be mainly used in Europe to meet their nickel-free restrictions on jewelry. See DECOREX in this link. This is a modern day thing. I knew it existed but didn't know much about it either until I looked it up.
http://www.enthone.com/decorative/index.aspx

DECOREX processes produce a white palladium electro-deposit that approaches the whiteness of bright rhodium at a fraction of the cost. DECOREX processes can also be used to create a barrier layer for nickel-free applications. The DECOREX system combines copper with white metal technology. DECOREX white palladium deposits offer a barrier layer to prevent metal migration to the surface. The alternative satisfies European nickel-free requirements. (Currently available in Europe and Asia only.)

For those interested in PM plating, the Enthone site has lots of info. Here's a good example in this link. Enthone also sells all the former Sel-Rex PM plating solutions. I worked for Sel-Rex in the late 60s, early 70s.
http://www.enthone.com/resources_detail.aspx?Page=precious.ascx

Chris
 
Thanks again Harold,

Yes it was copper, I am sure. Yes, I still read Hoke's book. I also watch LazerSteve's vid's. Yea I say I have unlimited patience, but I feel so close. So now on to better things. I used Ammonia Hydroxide. No blue at all. I rinsed a few times. In this picture it is still a little wet.
DSCF4570.JPG
Does this look normal? Do you think I am missing anything before I melt?
I do feel I have followed all steps correctly.
Thank you for your time again to anyone with help.
Robert
 
goldsilverpro said:
Harold,

I think that, due to the fact that some people are sensitive to nickel, palladium is sometimes used as a migration barrier coating underneath the gold. It seems to be mainly used in Europe to meet their nickel-free restrictions on jewelry. See DECOREX in this link. This is a modern day thing. I knew it existed but didn't know much about it either until I looked it up.

Thanks for that, Chris. One of the problems of having been away from refining for so long.

I can honestly say, in all my years of refining, I encountered white gold that was alloyed with palladium only once. It was very unusual to find any aside from the odd crown, or in dental gold.

I should have realized that there were changes in that one of my old customers, who calls occasionally, made reference to palladium being used frequently in modern jewelry.

At any rate, thanks for the news, Chris. I'll try to keep that in mind as I dispense my comments.

Harold
 
SureShot72 said:
Does this look normal? Do you think I am missing anything before I melt?
It looks quite good, although that may not manifest itself in a pure looking button (I expect it will). Note how the gold that is above the bottom has turned a nice, light tan color. That's a good indicator that you have achieved a high level of purity. My logic is that gold that is very pure is eager to agglomerate. You can abrade it with a porcelain spatula and have it turn a bright gold color for that reason. It clumps well when it's very clean, not so well when it is not.

The "acid" test is when you melt. Do not use a dirty dish. Properly season the dish, including heating slowly until it is dry, then raising the temperature to the point of glowing red. Sprinkle borax, sparingly, on the dish and continue heating until the dish has a full covering of borax, but it DOES NOT POOL. If you are more comfortable working with a cold dish, allow it to cool, then introduce your gold powder to the dish. You can do it hot if you prefer. Do NOT add borax to your gold. Apply a soft heat, so you don't blow the gold out of the dish. As it begins to melt, you can increase the flame, or move closer. When it is all molten, if it hasn't formed a common mass, swirl the gold in the dish, so it makes contact with all the prills, which should readily be absorbed by the molten mass.

When you remove heat, the button should remain bright---displaying a rather greenish color. If you see a rainbow effect that emanates from the center of the button and moves to the outside edge, you'll know that your gold is not pure. Pure gold will not form any kind of oxide, and will cool with a clear, shiny surface, often described by a coarse crystalline structure. It forms a deep pipe when it is very pure, and won't form much of one when it is not. If the surface of the button is not shiny, but has a rather soft matt appearance, it is contaminated, likely with traces of silver.

Good luck! Be certain to post a picture.

Harold
 
Thank you So Much Again Harold! This was my first and very exciting! I think I may of used a bit to much borax. There is a small piece stuck on top and the bottom has a thin coat. I started with a propane torch. I had to finish with Map gas cause I could not get it hot enough to melt. A small discoloration on the top. I hope it is just from the Map gas. I am very happy anyway. I think I will hold on to this one for a while, and maybe re-refine as I get better at this.
DSCF4575.JPG
DSCF4572.JPG
It weighs .25 troy. I am now still steaming down the rest of the liquid from this batch that would not drop. Do I need to add anything before SMB to help it precipitate?
Thanks again to everyone who commented on my first project.
Robert :p

Maybe in a few months everyone can help me with my palladium. I know I will need it. For now I have much more of this plated scrap to go through. :mrgreen:
 
SureShot72 said:
Thank you So Much Again Harold! This was my first and very exciting! I think I may of used a bit to much borax. There is a small piece stuck on top and the bottom has a thin coat.
If you don't mind dealing with borax after the button has solidified, you can sprinkle a trace on top of the button AFTER it has melted. If you have an adequate heat source, you can superheat the gold slightly, so it stays molten long enough for the borax to melt. Alternately, you can allow the button to freeze, then sprinkle a trace on the surface while it's still red hot. That will generally clean the surface of traces of discoloration. It does precious little in the way of improving quality of the gold---but it does look a little nicer. You can remove borax from a button by boiling the button in dilute sulfuric. If you have a heavy deposit, you can tap it lightly, using a small spoon, fracturing the deposit. The wash will remove traces without altering the surface.

I started with a propane torch. I had to finish with Map gas cause I could not get it hot enough to melt.
One of the harsh realities you'll come to understand is that you are wasting time with ANY torch that does not use oxygen. Even if you can achieve the melting point required, the time it takes wastes a huge amount of fuel, and you're drastically limited as to the volume you can melt. If you go beyond gold and silver, you won't achieve your goal at all---so you'd be well served to consider adding oxygen to your melting system.

A small discoloration on the top. I hope it is just from the Map gas.
Nope! Not from fuel. That's an indication of a minor amount of impurity in the gold. Probably a trace of copper (oxide). You will come to understand that it's not easy achieving 9995, although certainly possible. When you get down to high purity, you must use extreme care and practice very good hygiene in processing. Even the torch tip should be cleaned before melting pure.

I am very happy anyway. I think I will hold on to this one for a while, and maybe re-refine as I get better at this.
You should be happy! We all start somewhere. My first button was terrible as compared to yours---but it was very encouraging to get that far. I kept reading Hoke and finally conceded that her instructions were good---that I should stop trying to re-invent the wheel and go with what is known to work.

I am now still steaming down the rest of the liquid from this batch that would not drop. Do I need to add anything before SMB to help it precipitate?
The only reasons I can think of that would have prevented precipitation were to have used too little SMB, or that you had not eliminated all the free nitric. Evaporating isn't likely to achieve anything beneficial unless you evaporate to near dryness, then add HCl. That will help expel nitric.

Here's something I'd like you to try. Put your new gold button in with the solution you're evaporating, and add a little HCl. If you have an abundance of nitric present, it will be consumed by digesting some of the button. That's the way I dealt with nitric in all cases, for it was my choice to use slightly more than was required in many instances, to ensure that I had dissolved all of the values. That's particularly important when processing filings and polishing wastes.

The only thing you should do to a solution you are preparing to precipitate is to filter before precipitation. Beyond that, there's nothing required.

Harold
 
As a side note virtually all British 18k white is palladium bearing ranging from 8%-15% and most is finished with a rhodium plate to give it that bright white colour. There are a couple of nickel alloys allowed which pass the nickel release tests but are rarely used here. Imported white alloys have all sorts in them and some are like steel but few seem to have palladium content, I have even found yellow gold that's been plated before now.
9k is rarely alloyed with palladium but 14k can often have a palladium content especially if it's high quality.
 
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