Tried to clean up my lab here and filtered out the slime of around 50l of used Ap, AR from my stockpot. SC Test=negative. This was my procedure:
1. Decanted as much of the liquid ( Cu(II)Cl, NiCl ) as possible.
2. Then added pure water and washed until the liquid remained clear and only the slime on the bottom remained.
3. Decanted the white slime ( AgCl), let it rest over night, then decanted again.
4. Used a gold pan to seperate the last remains of AgCl and the the grey/black slime
5. Used warm dilute ammonia to dissolve any silver chloride remains. Acified the collected solution with HCl and put it aside.
6. Poured the AgCl trough a cloths, dried it (maybe 30 g) and put it aside.
7. Now turned to the remaining slime an used dilute nitric in the first round, trying to dissolve any possibly precipitated Pd. SC Test was negative.
8. So I added HCl. Immediate reaction was a faint yellow color but the few visible gold flitters did NOT get dissolved, even after some hours. SC test=negative. Swap color =yellow.
9. So I added H2O2 ( did not feel so good about it, but had no other idea on how to increase AR strenght without adding nitric).
10. Reaction imm. turned the color to an orange, which surpised me, because it looked like Pd(IV)Cl. SC test = negative, Swap color = orange.
11. Filtered the liquid several time susing the "stuffed" funnel method.
12. Solution became rubin-red. Cotton swaps had an orange color, SC test shows nothing. => AgCl + SnCl = colloidal gold.
13. I did put a drop of the solution on a copper plate and after some time a black precipitant was noticed.
I assume(!) I have Ag and Pd mixed with SnCl as a colloidale solution now. Precipitation with copper seems to work, at least on a small scale.
Now my questions:
- Should I precipitate using copper or zinc, or is there a better way. respectively would this create more "mess"?
- Any thought on the explosive gold issue, since ammonia was introdcued in an early stage? ( But this is present in a stockpot anyway)
Thanks for comments, input, advice.
Marcel
1. Decanted as much of the liquid ( Cu(II)Cl, NiCl ) as possible.
2. Then added pure water and washed until the liquid remained clear and only the slime on the bottom remained.
3. Decanted the white slime ( AgCl), let it rest over night, then decanted again.
4. Used a gold pan to seperate the last remains of AgCl and the the grey/black slime
5. Used warm dilute ammonia to dissolve any silver chloride remains. Acified the collected solution with HCl and put it aside.
6. Poured the AgCl trough a cloths, dried it (maybe 30 g) and put it aside.
7. Now turned to the remaining slime an used dilute nitric in the first round, trying to dissolve any possibly precipitated Pd. SC Test was negative.
8. So I added HCl. Immediate reaction was a faint yellow color but the few visible gold flitters did NOT get dissolved, even after some hours. SC test=negative. Swap color =yellow.
9. So I added H2O2 ( did not feel so good about it, but had no other idea on how to increase AR strenght without adding nitric).
10. Reaction imm. turned the color to an orange, which surpised me, because it looked like Pd(IV)Cl. SC test = negative, Swap color = orange.
11. Filtered the liquid several time susing the "stuffed" funnel method.
12. Solution became rubin-red. Cotton swaps had an orange color, SC test shows nothing. => AgCl + SnCl = colloidal gold.
13. I did put a drop of the solution on a copper plate and after some time a black precipitant was noticed.
I assume(!) I have Ag and Pd mixed with SnCl as a colloidale solution now. Precipitation with copper seems to work, at least on a small scale.
Now my questions:
- Should I precipitate using copper or zinc, or is there a better way. respectively would this create more "mess"?
- Any thought on the explosive gold issue, since ammonia was introdcued in an early stage? ( But this is present in a stockpot anyway)
Thanks for comments, input, advice.
Marcel