Cursed
were you trying to do HCl-Peroxide, thinking that subzero was an oxidizer like peroxide or bleach? Just trying to understand your motivation here.
As was stated by mic, you have made an inprecise version of Poor Man's AR - Lazersteve's recipe for which follows. This is the updated one. Notice that, as mic advised, heat is required for the process to work effectively, needs to be monitored closely, and additions of nitrates should be incemental. As your acid becomes saturated, it needs to be decanted, filtered & tested with stannous for gold content, & replaced with fresh.
As BR 007 stated, you have way too little solution for the amount of copper & nickel that will be dissolved. Boiling the crap out will just hasten the expulsion of acid, unless your container is covered, and you'll also hasten the build-up of salts, which is no fun either. You will boil in this process but it is controlled & precise.
Once i figured out what was going on, & since my ADD/OCD finds waiting (what seems like) days & days for crockpot- HCl to work agonizing, it has become my method of choice for pins, since I don't have the quantity of material either that would justify separating steel pins from Kovar or brass.
Again: THIS IS LAZERSTEVE'S RECIPE, for processing the pins from ceramic CPUs. i have it saved on my PC; it was easier to cut and paste it than to find the thread again. Maybe someone can go right to it.
Processing ceramic cpus
Here's how I proceed with Poor man's AR:
1.Remove lids (top and bottom) from ceramic cpus using MAPP gas.
2.Add cpu's into large beaker or coffee pot.
3.Fill with HCl (31.45% approx 10 M). Add just enough to cover the cpus.
4.Add and equal volume of tap water
5.Place small ceramic saucer on top of pot to prevent vapor from escaping.
6.Heat to just below boiling.
7.Add in 2 teaspoons of sodium nitrate.
8.Boil for 30 minutes or until brown fumes are no longer visible.
9.If salts form pour off dark acid through tight filter and start at step 3 above. Filter may contain gold foils or powder.
10.Repeat steps 6 and 7 until all metals are dissolved.
11.Remove ceramic saucer and let the solution evaporate down to 25% of it's original volume, or until salts form.
12.Add fresh HCl to expel nitric as brown vapors.
13.Repeat steps 9 and 10 two more times.
14.Dilute with equal volume of tap water.
15.Filter through packed funnel under vacuum until 100% free of sediment and suspended particles.
16.Add Sodium Meta Bisulfite to precipitate gold as brown powder.
17.Let settle and siphon liquid off brown powder.
18.Add enough water to cover brown powder.
19.Repeat steps 17 and 18 two more times.
20.Add enough HCl (32% 10M) to cover brown powder.
21.Boil HCl with brown powder until color of HCl no longer darkens.
22.Repeat steps 17 and 18 two more times.
23.Slowly dry gold in beaker by shaking beaker over medium heat until the gold powder moves freely about the beaker it's was precipitated in.
24.Transfer brown powder melting dish and heat to red heat (incinerate) DO NOT MELT!!!
25.Transfer incinerated powder to beaker and repeat process steps 3 to 21 on the brown powder.
26.Prepare melting dish as shown on my website melting videos.
27.Melt dry gold powder in properly prepared melting dish.
dtectr