Calamity in progress! (1st attempt)

I started with about 50g of mixed gold plate through 18k. added just over 150g of copper to inquartate. when pouring the mixed metals, i was to close to the surface of the water and didn't get the corn flake effect that I was expecting. also the metals didn't mix the way I expected, I could see bands of different metals in the cooled product. Decided to do the run anyway.

Now for the chemistry...

I was not able to obtain Nitric acid, so I used the poorman's method using potassium nitrate and muriatic acid to create the AR. I used 50g of potassium nitrate, 200ml of muriatic acid and 500ml of distilled water.

Added my metals, and away it went. I left it all overnight. When I got back to the solution, the reaction was mostly complete. The solution was a very dark green color. I divided the solution in half.

I diluted the first half with 500ml distilled water, mixed 120g of smb with 350ml distilled and added to this.
my solution turned a cloudy tan color and no metals dropped.

That is when I started researching this site for some answers to my stupidity.
Findings:
Likely still had free nitric in solution.
Best fix use sulflamic acid. I didn't have any on hand.
Next add some muriatic acid and bring to a boil. I did that, and a very small amount of metal dropped.
Nowhere near the amount that I was expecting.


I decided to split the volume of solution again and dilute a second time thinking that i needed to give the nitrates somewhere to dissolve. OMG, I had a burst of metal precipitate. The solution changed to a pretty golden yellow and I had a brown precipitate.

This is the part that i did correctly. I decanted the liquid and save it for future investigation.

After 4/5 hot water washings, the precipitant was still a very dirty brown color. Next, Muriatic acid wash, no change still very dark brown color. After the 15th wash, it was starting to look pretty. I decided to dry it.
To my dismay the dried product had a green film over all.

I am still washing.

I still have the other half of the original solution waiting to be reduced.

!! HELP !!

Not trying to be disrespectful but you have absolutely no clue what you are doing. Everything from the methods you chose to the execution were wrong. You should safely store all your chemicals and material and study this forum before you get back into this.

I have to agree with goldenchild. I don't understand much of what you've done.

To inquart material, you try to end up with gold being one quarter of the total metal. But you started with 50 grams of mixed material including gold plate and added 150 grams of copper, so the gold content was far below one quarter.

Your metal didn't mix right and didn't form cornflakes, but you decided to do the run anyway? You should have remelted, remixed, and poured it again.

When you inquart, the idea is to dissolve the base metals first with the nitric leach, leaving just the gold to be dissolved in AR. But you went directly to poor man's AR. Then you diluted it with 500 ml of water. Why?

You added 120 grams of SMB. But you only started with 50 grams of gold bearing material. That's way too much SMB.

That's just from the first part of your post. I don't have the time to continue pointing out more errors. As goldenchild said, put your solutions away safely and spend some serious time studying.

Dave

Thanks.

I already knew that I "Messed this up". Hence the name of the post.

Thanks for the pointers.

To recover from a mess, I recommend cementation. Put some large pieces of copper in the solution. Things like heavy copper busbar are ideal. Get an aquarium air pump and put a piece of airline down to the bottom of the solution. The bubbling will keep the solution in motion and keep bringing fresh solution into contact with the copper. Let it do its thing while you study. Any values in the solution will eventually end up at the bottom of the container.

Dave

Kstone its not that we don't want to help you its just that what you have been doing is just very wrong and you need to "learn and understand" what you did wrong. We could hold your hand (by you keep posting questions that have already been answered a 1000 times before and us answering them again) during your whole time learning how to refine. That approach does not help you understand what you are doing. Its like the teacher in class just handing everyone the answer key to every test. That only hurts the students. Don't panic you will not lose the gold that you started with if you cover the solutions and let them sit. Water may evaporate off (if you use a poor container) but the gold will remain in the solution if left to completely dry out the gold solution will just crystallize and just needs to be rehydrated with Hcl when you are ready to begin again. Frugalrefiner gave you one method which will put your gold back out of solution as a black powder. I would suggest you do that. Make some stannous chloride to test your solution. Test it every few days by taking just a drop of your solution and a drop of the stannous and observe the color. When all the gold is out of solution decant and save the powders for later. You should not have combined plated material with karat scrap as they are completely different processes. Youtube can be a very good place to find information some of our members post videos there showing some processes, but youtube can also be a bad tool as there are plenty of people posting videos that are just flat out wrong or they leave out crucial information. That is why it is important to read/study as well. Don't be discouraged stick with it and you will be just fine.

Follow Dave’s advice. Cementation with copper is, by far, the easiest method to begin the process of recovering from your mess. Copper buss bar is best for a variety of reasons that you will learn. Testing your solution every few days with Stannous Chloride will tell you when your gold has cemented from solution.

While waiting the several days to several weeks for this process to finish, please read “Refining Precious Metal Wastes” by C. M. Hoke. You can find links in Dave’s signature line. I can not emphasize enough the importance of this book. Written some 70 years ago to assist jewelers in recovery and refining waste material, it stands the test of time. Read it. Read it again. Read it and make notes. Read it and write down questions you will have.

Time for more coffee.

Gentlemen,

You have deduced the source of my stupidity, Youtube.

I will do as has been suggested and research the why of this procedure.

I appreciate the time you have taken to set me on the path and the constructive criticism.

Please note that I included all the information that I could, because the road to hell is paved with good intentions and little comprehension of the consequences.

I just want to point out something that is taken for granted often is this term "cornflakes", and it is important as the cornflake gives you the surface area you want for a fast and complete processing of your inquart. I have found you have to pour the molten mixture from waste height into a bucket of hot water to get the cornflakes. If the water is cold you will get shot. If you want clean tight shot, spheres, pour slowly from waste height into a bucket of ice water. Make sure the ice is weighed down underwater or removed as you do not want to pour the molten metal on floating ice.