Help with what process to use on my first project.

[SureShot72]

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?

 

[Barren Realms 007]

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.

 

[SureShot72]

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!

 

[seawolf]

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

 

[nickvc]

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.

 

[SureShot72]

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.

 

[seawolf]

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

 

[goldsilverpro]

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.

 

[SureShot72]

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.

 

[Geo]

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.

 

[SureShot72]

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?

 

[Geo]

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.

 

[SureShot72]

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.

 

[Geo]

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.

 

[Barren Realms 007]

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.

 

[SureShot72]

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.

 

[Harold_V]

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

 

[SureShot72]

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.?

 

[Smack]

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.

 

[Harold_V]

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