Contamination?

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Puff501

Member
Joined
Feb 15, 2020
Messages
23
Location
Arizona Desert
I just completed my process of refining some karat scrap I've accumulated over the last year or so. The processes all seemed to go smoothly but when I went to the melt, this is the bar I got as a result. It shows contamination, I'm not sure what but it isn't pretty.
Some very experienced people in this forum may well know what the contamination is and may be able to advise.
I realize I will likely have to re-refine this. This bar weighs 31.23g.
Also on a re-refine, Should I start from the beginning with inquartation or would I just go to the aqua regia step over again?
I am leaning to going through the entire process again but if you think it isn't necessary and I can just go to AR then that would be an advantage.
https://ibb.co/vsgC5T8
https://ibb.co/tBvsKdS
https://ibb.co/CswH9w6
 
Puff501 said:
Also on a re-refine, Should I start from the beginning with inquartation or would I just go to the aqua regia step over again?

I'll let others give opinions on the discoloration.

The reason we sometimes inquart is when both gold and silver are in the alloy. When silver content in a gold alloy gets up to around 10% or higher, it creates a problem dissolving the material.

If it's put in nitric to digest the base metals, the reaction will slow to a crawl and may never reach the center of the material because the gold becomes like a sponge and protects the base metals in the center.

If it's put in AR, the silver will form a crust of insoluble silver chloride. This crust stops the AR from reaching the center of the material just like the gold did above.

Your gold is very pure. No need to inquart. Granulate and dissolve in AR.

Dave
 
Puff501 said:
Some very experienced people in this forum may well know what the contamination is and may be able to advise.

Sorry for the delay in responding --- based on the second pic (bottom of the bar) copper - & lots of copper at that

First pic (top of bar) looks like "possible" other contamination (iron, nickel, etc. etc.) --- or could be (just) more copper as "oxides"

I say that because in the third pic you can clearly see the copper on the (upper) edge of the bar - so the very top of the bar could be just more copper as copper oxides - or combination of copper along with "some" other base metal contamination --- what ever the case - copper is the main contamination - & it looks like a lot of copper

Also on a re-refine, Should I start from the beginning with inquartation

so you used inquartation in the first place

Based on the amount of copper contamination I "assume" you used copper to do your inquarting --- or did you use silver :?:

Also - based on the amount of copper contamination I see - I "assume" you only did "one" hot nitric leach to remove the copper (&/or silver) & then "some" water washes --- is that right :?:

When doing the inquartation method/process you will almost never (if ever) get all the copper (&/or silver) out with the first nitric leach --- just like with gold dropped from a normal AR drop you need to put the gold sponge through hot water & acid washes to rid the gold sponge of contamination --- how many washes will depend on contamination left behind in the first leach (inquartation leach) or the first gold drop (from AR)

Lets stick to inquartation - with copper as the inquarting metal - you need to do hot "boiling" (as in a simmer boil) water washes (boiling forces the copper nitrate "out of" the sponge) you need to do those washes until you see NO blue in the washes (in other words it can take 3 or more hot (boiling) washes to get all the copper nitrate out

But you are not done yet because you may not of dissolved all the copper in the first leach - therefore you need to do another hot nitric (simmer boiling) leach to insure all the copper was dissolved in the first leach

If you get a blue solution in this second leach/wash you did not get all the copper the "first" time --- so you will have to do the hot water washes again - & then another hot nitric wash followed by hot water washing

In other words - you need to do the water washing (after first leach) followed by an acid washing & you need to do that how ever many times it takes until you get no blue out of the acid wash --- keep in mind that after each acid wash - you need to repeat the water washing until all the blue is gone from that acid wash

normally - it takes at least 3 acid washes to get all the copper out (& can take even more)so you do the acid washing until you get an acid wash that produces no more blue --- & like wise each of the water washes need to be done till the blue copper nitrate is washed out

Inquarting with silver --- you need to go through the same washing process - except that you need to test each wash with HCl or salt to insure you have washed all the silver out --- in other words - the HCL or salt will produce silver chloride (which will appear as a white cloud) so you need to do the washing until NO silver chloride cloud is produced when you test the washes with HCl or salt

It is possible to get all the copper (or silver) out in the first leach (thought that is "rare") so no mater what - you always have to at the very least do at least one acid wash (after first water washing) to insure all the copper/silver came out in that first leach

or would I just go to the aqua regia step over again

That is what I would do - at this point there is likely very little silver left - so I would re-melt the bar & pour it to shot/corn flake - the AR will dissolve the gold & copper (&/or other base metals) once you have dissolved the shot/corn flake in AR - there "may" also be "some" dissolved silver in the AR --- so you want to then dilute that AR by 2 - 3 times --- by diluting the AR IF (big IF) there is any silver (small amount) dissolved in the AR - it will drop out as silver chloride when you dilute the AR --- the silver chloride will be VERY fine (you may not even see it) so let it sit for a day for the silver chloride to settle out

Keep in mind that after dropping your gold from your AR solution - you still need to put your dropped gold through the water/acid washing --- if you want clean (pure) gold as your end product --- & you use HCl for the acid washing of gold dropped from AR --- instead of nitric acid to wash gold sponge from inquartation leaching

to clarify - to wash gold dropped from AR - you put the gold sponge through water/HCl washing --- gold sponge from the inquartation process goes though water/nitric washing --- if you want clean (pure) gold

Kurt
 
Thanks Kurt for this detailed reply.
To answer your questions,
1. I used silver for the inquartation. I tested the jewelry to calculate karat and added silver to make the inquartation 25% gold.
2. I did 3 nitric treatments total. The first 2 treatments, I used used dilute nitric I had left over from the last refining of karat scrap that I did. The second treatment didn't seem to pull any more copper out of the inquarted gold and that surprised me. I saved that 2nd acid treatment as used dilute nitric and cleaned the inquarted gold with 5 rinses until it was clear. I did not test the rinse solution with HCL to test for silver. I then went into a 3rd nitric treatment with new brand new nitric and let that boil for about 20 minutes. The solution was crystal clear, perfect crystal clear, so I thought I was done this step. I saved that solution as used dilute nitric as well and rinsed the processed inquart to go into AR.
Now note, I am not near an expert by any means. This is only the third time I have processed karat scrap. The first time I processed, I needed 5 nitric treatments and the second time I processed, I needed 6 nitric treatments. So when I was in this third batch of karat scrap, I was surprised to find the nitric treatment was complete basically after the 2nd treatment because the 3rd treatment appeared to just verify I was done after the second.
I hope I'm clear on all this.
Also I notice that the pure gold powder from this last refining did not match the color I had in my pure gold powder from the last 2 refinings even though I did 2 ARs in all 3 of my refinings. In the first 2 refinings, the final pure gold powder looked like the picture below. In this 3rd refining, I have no picture but it was much browner. That was apparently an indicator that I still had some kind of contaminants still present.
I will take your advice which is also the advice of Frugal which is to make shot and go to AR process again, drop again and clean with HCL and water rinses. I'm likely going to run the AR process on this bar next week and I will keep you posted as I go.
https://ibb.co/YhQZyCd

Thanks again for your advice
Steve
 
While this will not help with your current problem I’d advise that you use a good rinse process on all your precipitated powders, put your powders in a beaker and cover well with water and boil it for 10 - 15 minutes, be sure to use a watchglass, you will probably see some color in this water, pour off and rinse quickly with warm clean water pour off and then cover the powder with HCl and again boil using a watchglass, do this process until you get no color in your HCl, this will dissolve small amounts of your gold so keep either for the stockpot or other recovery processes, once the HCl is clear after boiling repeat the water boiling processes at least twice, this will remove a lot of the contaminates in your powders including traces of silver chloride.
 
Thanks nickvc
I will be doing the water and HCL boils this time as well for the rinses.
All I did this time was rinsed cold, HCL then water, 3 times.
That may be why I have what I have right now.
 
I finished re-refining that contaminated bar.
I turned the bar to shot, did an AR on the shot, dropped it with SMB, did a water rinse and then a water boil, then an HCL boil, and it looked nice and caramel. Did one more HCL boil and then a water boil. Then filtered it and got this.
https://ibb.co/59pYTkD
Too late to melt it to a bar today, maybe I'll get to it tomorrow.
Thanks folks for your help.
I think I have something nice here.

Steve
 
OK, I think I tried this before and I had trouble but it may have been my file size was too big.
Reduced it to 117kb

Thanks Frugal

Steve
 

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