where did I go wrong?

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goaldspektre

Well-known member
Joined
Sep 17, 2009
Messages
56
I thought I was doing well with all the great advice I've gotten on this site , then today I think I made a mess of things . First off I started with 5lbs cpus , all ceramic (6 pros , 1 lb 486's , the rest were pentium/amd/cyrix and 2 ibm 6 86's. I started with 35% nitric to dissolve base metals . This reaction lasted 1 hour and ceased but all pins were still intact. I thought because of the plating the acid couldn't get to the pins? So I went to AR and the reaction took off for about an hour and a half then slowed to fizzing for 4 hours.There is brown powder in the acid that wont dissolve(i think it's gold that dissolved and was displaced by iron or copper in the solution?)The fizzing is still going after 6 hours and I will check in the morning as all the pins and gold have not dissolved. Now should I filter and redissolve the gold in HCL-CL which I would do anyways because of all the base metals and why did this happen . I ask because I've used Ar from the start before without this happening, is it the higher Au content . Any input is appreciated.
 
Well because you started with nitric and didn't let it finish it's job! When you went from nitric to AR you still probably had residual amounts of nitric from the original solution. This has thrown your nitric level up. Either wait till the rection stops and drop with copper and repeat the process. Or use some urea to neutralize the nitric. Or wait till the reaction stops and siphon off your solution and reprocess your stuff in the bottom of your bucket. Don't forget to test your solution for PM's.
 
I tested a small sample of the batch with stannous and it was negative for any dissolved values.And it was de noxed.The nitric was completely removed before the AR process.I forgot to mention the nitric was left overnight before switching to AR today.
 
I wonder if the watch glass I covered the reaction with may have changed the acid ratios for the worse???
 
Did any color show up in your test and then dissapear?

Just because your solution was left over night and you are seeing no reaction does not mean you got rid of all your nitric.

You can boil your chips in water, heat them till dry, and still have some residue left to cause a reaction. You might be right, I'm not there looking at your solution.
 
No colour at all . The reaction had completely stopped with the nitric so I used the leftover to process fingers (5 Lbs) and it worked lightning fast on them! This is why i'm confused . I have dissolved with success ceramic cpu's with nitric before and had no issue at all. This time the reaction removed the pins on a few lower grade processors but stopped after an unusually short period. Then the Ar rocked for a while but the Gold is precipitating out of solution and the reaction is crawling along . This is why i'm thinking tomorrow brings a clearer view on the situation.Excess nitric in AR would , in my opinion, not cause this though Barren , have you encountered a similar problem and found this to be the cause .

Robert
 
Most of the pros want you to incinerate between acids. In your case
they would want the solids brought to a read heat but not melted between
the nitric acid and the AR stage.
 
Since I'm not a pro, I normally just washed the solids down really well
with water between using nitric and either poor mans AR or HCL-Cl when
dissolving the gold.
 
That's what I did because i'm not a pro either , yet . I want to be a pro though and want whatever advice leads me down the right path.
 
goaldspektre said:
No colour at all . The reaction had completely stopped with the nitric so I used the leftover to process fingers (5 Lbs) and it worked lightning fast on them! This is why i'm confused . I have dissolved with success ceramic cpu's with nitric before and had no issue at all. This time the reaction removed the pins on a few lower grade processors but stopped after an unusually short period. Then the Ar rocked for a while but the Gold is precipitating out of solution and the reaction is crawling along . This is why i'm thinking tomorrow brings a clearer view on the situation.Excess nitric in AR would , in my opinion, not cause this though Barren , have you encountered a similar problem and found this to be the cause .

Robert

I have had it happen in respect that I ran material thru AP, washed it numerous times, ran thru oven to evaporate water out, ran thru nitric and there was still residual HCL to dissolve a little bit of the gold. Unless you incinerate you can still have residuals.
 
Nothing to do with my problem but a buddy of mine thinks i'll get an ounce of gold from all this because he saw it done on you tube. I almost laughed then thought that you tube is why I started refining . I then informed him that no , sadly I won't.
 
glorycloud said:
Most of the pros want you to incinerate between acids. In your case
they would want the solids brought to a read heat but not melted between
the nitric acid and the AR stage.

I'm not a pro, far from it, but I don't think you need to incinerate when going from nitric acid to AR. Two things you gain with incineration is to
1. eliminate one acid to not risk dissolving gold when switching acids, but in this case you are going to AR so you are going to dissolve gold. No need to eliminate the nitric acid.
2. Remove any organic residues (plastic, oil, carbon). But with ceramic CPU:s there shouldn't be any big problem.

Another thing I'm reacting on is why switch horses in the middle of the race? Going from AR to HCl/Cl isn't doing any good, it just complicates things. If you have nitric acid use that through all the processing and skip the clorox.

If I would come with a guess of what is happening here I would say that this is a likely scenario.

1. You start with a lot of scrap in a large batch. (Did you remove any lids on the CPU:s?)
2. You add nitric acid and start dissolving base metals.
3. After a while the exposed base metals were dissolved and the remaining was either quite resistant (Cu - tungsten lids of the PPro) or protected by gold plating so the process seemed to stop.
4. Now you took away the acid which had a lot of strength left which your finger batch proved.
5. You added AR (how much? Which concentration?) and it started to attack your gold and base metals. As you probably had a lot of base metals the gold cemented out on the base metal as a powder.
6. You stopped here and posted on the forum.

As you have brown powder and the reaction in AR have stopped, could it be that the nitric in the AR is exhausted?
I've never tested this myself but I think it should work as a nitric test. : Take a little bit of your solution and drop a bit of urea in it. If there is nitric left you should get a reaction.
If there is no or very little reaction then your nitric is exhausted and that is explaining why you see so little reaction.

I suggest that you decant off the majority of your solution, this removes the dissolved base metals.
Test your solutions, but also test your stannous chloride against a known gold solution so you know that it is working.

Now you have two ways to go, either continue to recover your gold with AR, dropping dirty gold from a dirty solution or incinerate and go back to straight nitric until all base metals are gone and then use AR and drop gold from a cleaner solution.
I suspect that some of your problems comes from the large heat sinks on the PPro:s. Maybe you should separate them out from the other CPU:s before going forward.

Good luck!

/Göran
 
CPU pin and heat sink alloys are much slower to dissolve than the copper in fingers especially if you don't have the ability to heat your solutions.

I suspect your nitric digest was not finished but had just slowed to a crawl. I believe the same to be true of your AR digest.

If you cannot heat your solutions you may have to be far more patient and wait for your processes to finish before moving on.
 
Thanks for the responses . The gold had cemented out, which is what I figured had happened. I did remove the lids on all but the p-pros and think that is where my problem came from.Today I tested the cpu batch and it tested negative proving the gold had cemented out . I poured off the liquid and through a 16 mesh sieve filtered the ceramics from any base metals and gold powder/foils in the mix . I have thoroughly rinsed everything and am now using HCL-CL with success . Thanks again.
 
I have a similar problem with an insoluable brown powder, rather a light fluffy brown precipate. Here is what happened:
Digested various gold bearing electronic materials in HNO3 + DI H20. Allowed to continue for a week, untial all reactions had stopped.
A clear dark-blue transparent liquid remained on top of the batch. I (gad) added moderately hard TAP WATER to the mix.
POOF!! a huge volume of brown precipate formed.

Allowed to settle, poured off clear liquid. Added fresh HNO3. No effect. Tuns of fluffy brown crap.

HELP!!
 

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