# Help with what process to use on my first project.



## SureShot72 (Jul 22, 2011)

First off, yes I have read "Refining Precious Metals Wastes by CM. Hoke" it stays on my desktop because it needs to be studied constantly.
I do not remember it all, but I do know the safety part by memory. So down to the question or questions.
I have a bunch of scrap. I do intend to process most myself. I recieved a few hundred pounds of Old Ma Bell telephone equipment. I have been clipping on and off for the past 5 years.
I would like it if someone maybe could help me identify some of it. For ex. some contacts I know are palladium, but after reading CM. Hoke, I think there may be platinum in there too. I think I will send this off to a pro. I have much gold. The first I wish to start with looks to be gold pins "I guess plated" over brass? I will attach some photo.
Photo #1 
Gold over brass? "When I break a pin in half or cut it looks to be gold solid. I know this cannot be. So what to use if it is gold over brass.
This would be my first project and need to know what process would fit it best.

Photo #2 
These are "as I was told" solid gold contacts. I think the gold is layered over palladium. I think the stems may be silver.

Last photo #3
I do not know. I aquired from a friend. I know the outside is a thin gold plate, but the inside has these really soft white wires?

I hope I am posting this in the right area.
I really just need a little identification info. Plz forgive my spelling and starting with #1 just let me know what chems to purchase. I do not want to buy too much.
Thanks anyone and everyone.
One last question. What type of situation should I use the "poll question" for?


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## Barren Realms 007 (Jul 22, 2011)

The plated items in your 1st and last photo I would run in a sulpuric acid cell. The middle photo I would seperate the contact point's and run them in HCL/peroxide.


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## SureShot72 (Jul 23, 2011)

When you say separate the contacts on the second photo, I hope you mean with some kind of chem process. I have about 500,000+ of these and they are just a little larger than a ball point on a pen. Could I use nitric acid to remove the base, and if I did would it destroy any silver or palladium that may be there?
I would like to point out that although I am completly new to this I have done a bit of homework.... Its just so much info and its depressing reading the "Hoke.pdf" and realizing that the prices for everything he is talking about was before I was born. LOL
I also have one other cry for help.
Before I started this venture with the acids, I tried the "Amalgamite 982" process or I guess as I read here "bismuth"
Well I built a furnace and it works too well I think. The "Amalgamite" soaked up a bunch of gold I had, but then when I tried to cupel it to leave the gold filtered out. The cupel got red hot but did not absorb the "Amalgacrap!" anyway here is a pic and if anyone know of how I may get my gold out with what acid or process... Please Help!


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## seawolf (Jul 23, 2011)

I agree use a sulphuric cell on the items in picture #1. On the items in picture #2 clip one or two of the stems from the contact drop them into a small test tube add a 50/50 mix of nitric acid and distilled water. When they are digested dilute to double with more distilled water then add a pinch of non-iodized salt if a cloud forms the stems contain silver. If the test is positive complete pins contacts and all can be digested the gold contacts should not be affected by the nitric acid. Filter then drop the silver with a heavy piece of copper. The contacts can then be refined with AR and tested for other PGMs then drop the gold and other PGMs.
Mark


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## nickvc (Jul 23, 2011)

seawolf said:


> I agree use a sulphuric cell on the items in picture #1. On the items in picture #2 clip one or two of the stems from the contact drop them into a small test tube add a 50/50 mix of nitric acid and distilled water. When they are digested dilute to double with more distilled water then add a pinch of non-iodized salt if a cloud forms the stems contain silver. If the test is positive complete pins contacts and all can be digested the gold contacts should not be affected by the nitric acid. Filter then drop the silver with a heavy piece of copper. The contacts can then be refined with AR and tested for other PGMs then drop the gold and other PGMs.
> Mark




The only fault I can see with this is if the points are Pd then they will dissolve with the silver in the nitric and if you then cement the solution you will have to put the silver through a cell to recover the Pd, another method to recover the Pd is to form the dreaded silver chloride by adding HCl , filter and wash the chloride well and then cement the Pd.


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## SureShot72 (Jul 23, 2011)

seawolf said:


> I agree use a sulphuric cell on the items in picture #1. On the items in picture #2 clip one or two of the stems from the contact drop them into a small test tube add a 50/50 mix of nitric acid and distilled water. When they are digested dilute to double with more distilled water then add a pinch of non-iodized salt if a cloud forms the stems contain silver. If the test is positive complete pins contacts and all can be digested the gold contacts should not be affected by the nitric acid. Filter then drop the silver with a heavy piece of copper. The contacts can then be refined with AR and tested for other PGMs then drop the gold and other PGMs.
> Mark



Thank you Mark, I understand. A little unsure what you define as a "Heavy piece of copper". Will research.
I will do so and reply with results sometime next week.

Side question: What acid or solution is most frequently used? This is so that I may bulk up on it, as I cannot afford to buy all at one time.


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## seawolf (Jul 23, 2011)

If you go to a scrap yard often you can buy a piece of copper strap that is 1/4 X 1 or larger for a few dollars a pound. Plumbing copper cut in half and flattened out will work also.
The type of acid depends on the process you decide to use AP, HCL and peroxide. If there is silver the Nitric and water works well. Testing is a must, when you know for sure what you have then decide on the method you want to use. If there is a chemical supplier in your area buy the proper acids to do the job. READ all of the msds info and work in a safe area and manner. A ton of gold is not worth your health or life or the people around you.
Mark


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## goldsilverpro (Jul 23, 2011)

SureShot72,

I haven't cupelled bismuth but I think it's about the same as working with lead. To cupel, you need a little air to be present on the surface to oxidize the bismuth. In general, the cupel doesn't absorb metals, just their oxides.


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## SureShot72 (Aug 20, 2011)

Well I am still on my first project and just trying not to mess up. I am really no good at math, but very good with commen sense and instructions that are not math.
So here is a pic of my first two batches.



Blue is just some pins here that I used Nitric on. My Nitric is a weak 35%


Should I use more nitric to desolve the rest or go to AR?
On the Blue, if it does have silver and I go to use copper pipe to drop.... Should I add more nitric, because it has sat around un covered for a week and I think it is dead.

As for the gold, I am just waiting for the nitric to dissapate from the AR so I can drop. Question on precipitation of gold from AR. Do I use Coopras or SMB?
Thank you all for your time..
Oh one last question about stannus. I have this from Shore.. Yea I know after I read enough, not to bother with them any more.


It does not seem to do anything. So I went to auto part store and purchased solder 95/5 tin. 
Using a razor I shaved some of the tin solder off into this solution. You can see it in there as the black bits. Is this normal for tin to do? Do you think I can make stannus with this solder as long as I stay away from the rosin core?

I am still reading as much as possible and following Hoke's book along with what I learn here. I think I am doing it right. I just take my time. Today I boiled down some Battery acid over 12 hours to concentrate. Then I will follow Lasersteve cold methed. I just do not think I will have the same ratio of ml. But I will try and post results.
Thank you all.


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## Geo (Aug 20, 2011)

the color looks good on your solutions.SMB will work for AR but you should look at some less expensive alternates for your processes besides nitric acid and AR such as AP and a stripping cell. no need to do anything to your tin solder other than cut a length and fold to fit in your container.


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## SureShot72 (Aug 20, 2011)

Geo,

You are right, its just that I am still new to this and do not know yet how AP differs. I have a Stripping cell and it works awsome. I just wanted to try nitric. Some of my Plated gold is very thick, like from Ma Bell back in the 50's or so. I also thought because what I did do in the cell left so many small bits untouched, I would just put in Nitric. That is when I noticed it turned blue. I am by no means an expert. I just know what I was told. Some of the gold plate has palladium or other behind it. 
I just found that my copper pipe is turning a black tint. No silver has percipitated to it. Any ideas?


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## Geo (Aug 20, 2011)

there are other metals that will tint solutions blue. leave the copper in for awhile and see what happens,if nothing cements then its not silver. by the way, did you put a small amount of the blue solution in a small glass container and add a pinch of salt? if it turns cloudy then you have silver in your solution.


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## SureShot72 (Aug 20, 2011)

OK well there is no silver there but, after one drop of the blue and one drop of the stannus that I talked about making before with the tin. "Keep in mind this solution never worked for me before"
This is the results.


So kink of a dark yellow brown. 
What do you think?
Stock Pot.


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## Geo (Aug 20, 2011)

brown is copper. by the way, stannous chloride does not store well and will go bad in a matter of weeks. the solution they sent may have set on a shelf for that long. when you make a batch make sure there is a piece of solder in the solution that doesn't dissolve, this means the acid is saturated and the piece of solid solder will keep it potent longer.


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## Barren Realms 007 (Aug 20, 2011)

Geo said:


> brown is copper. by the way, stannous chloride does not store well and will go bad in a matter of weeks. the solution they sent may have set on a shelf for that long. when you make a batch make sure there is a piece of solder in the solution that doesn't dissolve, this means the acid is saturated and the piece of solid solder will keep it potent longer.



If you follow the suggestions here on the forum it can last a long time. The batch I am using is probably 4-5 month's old and Trashmaster can vouch that it is still good because he was over here today and I did some test's with it.


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## SureShot72 (Aug 22, 2011)

Question before I percipitate my first batch of gold.
The Picture above of the yellow AR. I let this sit for a week. I do not know if that helps with the nitric.
I followed Hokes book and boiled down really low. It turned a brown dark blood red. Then cooled and added HCL 37% Still same color.
Is this normal? Letting sit overnight and want to try and drop today. Please advise.


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## Harold_V (Aug 22, 2011)

SureShot72 said:


> Question before I percipitate my first batch of gold.


Please note that the word is precipitate, not percipitate



> The Picture above of the yellow AR. I let this sit for a week. I do not know if that helps with the nitric.


It does not. Only evaporation of binding with urea will help---or use only that which is required to dissolve the values. Free nitric must be eliminated. 



> I followed Hokes book and boiled down really low.


I hope you don't mean that. One does NOT boil down---one evaporates. If you don't understand why, please go back to Hoke's book and read about evaporation. Don't stop until you understand what I'm talking about---and PLEASE do not post with terminology that alludes to boiling when evaporating. We already have more than enough trouble with readers that take that comment literally. 



> It turned a brown dark blood red. Then cooled and added HCL 37% Still same color.


Mistake! You do NOT let it cool---you apply the HCl while it is still hot. If, upon adding HCl when it is as dark as you claim, and it is hot, there is no evolution of brown fumes, fair chance you have eliminated the free nitric. 



> Is this normal? Letting sit overnight and want to try and drop today. Please advise.


Letting a solution sit serves no real purpose aside from allowing it to cool (to precipitate lead, or silver chloride) before filtering. 
If you feel you have eliminated free nitric, and have filtered the solution, go for it. If it fails to precipitate, you will then understand that your procedure was incorrect. 

I strongly advise you to go back to Hoke and read more. 

Harold


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## SureShot72 (Aug 22, 2011)

Thank you Harold.
So here is what I did next. I took this...


Added about 4 times the water. It turned golden yellow again. Same color as photo above, but also much more "mass" liquid.
Then used urea "slowly" till almost no fizz. Then SMB. It dropped. I am concerned it may be dirty. So I read an article, you had talked about washing with ammonia.
Can that be regular, like at the store?
Umm... Update. After the cloud had cleared the bottom had a fine brown or dark brown powder, but the liquid is not clear. Still yellow. I tried to drop some more but it will not. Stannus turn black as it did before the drop. Maybe I have to start over.?


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## Smack (Aug 22, 2011)

Filter off powder, re-heat your liquid to simmer off to about half it's volume, let cool and try smb drop again. Worked for me in the past.


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## Harold_V (Aug 23, 2011)

SureShot72 said:


> Geo,
> 
> You are right, its just that I am still new to this and do not know yet how AP differs. I have a Stripping cell and it works awsome. I just wanted to try nitric. Some of my Plated gold is very thick, like from Ma Bell back in the 50's or so. I also thought because what I did do in the cell left so many small bits untouched, I would just put in Nitric.


I have not read this thread to the end, so if my comments are redundant, please forgive me. 
In general, processing gold plated items with nitric acid won't be fruitful. It works, and works well, but is not economical. That might not be the case if you can purchase nitric for $4.00/ gallon, but few that refine at home can. It is available at that price with proper credentials and working conditions. 



> That is when I noticed it turned blue. I am by no means an expert. I just know what I was told. Some of the gold plate has palladium or other behind it.


It is highly doubtful you'd find palladium under gold. Nickel is typically used, which acts as a barrier to prevent gold migration. Gold, plated over silver or copper, will migrate to the point where it is no longer visible. Nickel prevents that from happening. 

The blue solution is most likely copper, although it may contain nickel as well. Both produce a blue solution in nitric. If you have a curiosity about the contents, test a drop of solution in a spot plate. Add a drop of ammonium hydroxide to the drop, which should turn deep blue. Then add a drop of DMG (dimethylglioxime). If you have nickel present, the drop will turn a vivid pink color. 

If you process materials that contain palladium, it will yield a solution that leans towards brown. If you process a serious amount of copper, with traces of palladium, you can expect the solution to have a green tint, growing ever more brown as the percentage of palladium in solution rises. You can determine the presence of palladium with stannous chloride, or even DMG. DMG introduced to a drop of palladium bearing solution will respond with a canary yellow precipitate. The test is very sensitive and will respond to miniscule traces of palladium. 



> I just found that my copper pipe is turning a black tint. No silver has percipitated to it. Any ideas?


Hard to say---but if you can collect a small amount of the black material, dissolve it in a drop of AR, then test with stannous chloride and DMG. Be certain to evaporate the solution to ensure you have eliminated traces of nitric that may not have been consumed. Color of the resulting solution alone will be somewhat of an indicator. If you see yellow through green and brown, you likely have something of value. What it is will be determined by testing. 
I tend to suggest readers explore Hoke's book, and I'm doing the same thing here. Keep reading until you understand everything she tells you. None of what I've discussed is not in print, in her book. When you can recite what you've read there, you will be, more or less, self sufficient in refining. The sole exception is silver, which she treats with contempt. You should assume a different view in that it becomes the carrier of platinum metals, especially if you use the inquartation process. 

Harold


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## goldsilverpro (Aug 23, 2011)

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


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## SureShot72 (Aug 23, 2011)

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.


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


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## Harold_V (Aug 24, 2011)

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


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## Harold_V (Aug 24, 2011)

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


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## SureShot72 (Aug 24, 2011)

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.




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  

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:


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## Harold_V (Aug 25, 2011)

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


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## nickvc (Aug 25, 2011)

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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