Oneal,
Here are my thoughts:
Junk jewelry, gold plated jewelry, and gold fill, can have many undesirable metals involved depending on what they were from. Copper base metals common (pewter, lead tin and so on would not be uncommon).
Your color of the wash water is an indication of some metals that are going to give you headache, it sounds like colloids, probably carbon-ous trash in solution with tin and other undesirable metals.
(The colloids can be broken with heating and strong acidic solutions (we will not discuss now in detail)
(The rinse water from nitric rinse add it to the spent nitric solution (after filtering) we will boil this down later concentrating the acid and recovering any traces from it).
You had sulfate salts with the lead salts so lead would very possibly be in powders (nitric may not have remove lead here).
This process can be done in one dish keeping powders in the pot removing liquids as needed,
I use a white corning type casserole dish, on electric hot plate with solid metal cast iron burner.
You may see some other details in this post to another member: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=12165
Powders separated from nitric solution these I would wash rinse and dry.
Incinerate powders to red hot, (to oxidize base metals like tin, burn off any trash, remove sulfates, nitrates and so on)
Let cool spray dry powders with mist from water bottle to wet, then add HCl.
Boil in HCl, (then the add water to dilute) keep HCl-water hot but below a boil, let powders settle well in this hot solution, and then decant hot solution, (this will help to remove tin, lead, trash, any copper you may have and other things you do not want in solution later (some gold colloids may follow these rinses).
Add water to powders and repeat these very hot water rinses until water solutions we decant are clear.
(Keep these chloride washes together in jar separate from other waste let them settle we will also concentrate and filter them later to retrieve values they may hold later).
Now heat to dry powders.
Re-incinerate the powders red hot, (This will help to remove chlorides that can give us trouble with our next nitric step), Cool.
Again spray down with mist water bottle, wash sides of pot down (this helps keep fine powder from bubbling and floating away when you pour in acids).
Add dilute nitric acid (70% HNO3 + H20 50:50 solution), bring to boil, then cool, letting powders settle well, decant solution and then, several hot water washes (decanting only from well settled powders).
Now add HCl to cover the powders (with little bit of excess), add nitric in very small amount (drops) with med heat (let reaction complete), if all gold has not dissolved, then add a few more drops (let reaction complete) repeat till all gold in solution.
Now we will eliminate any excess nitric you may have:
Let solution heat (not too hot but fumes evaporating off), (watch for boil over), (keep eye on solution but your nose out of it), (have wash bottle handy if foaming occurs you can spray it down with mist from water bottle).
Add a few drops of sulfuric acid, (this will help to remove lead in later steps, and keep from forming salts on evaporations).
Concentrating solution we want it thick like syrup but do not make crystals or salts, add some HCl to wet again, heat until syrup again, repeat HCL to wet, one more time evaporate to syrup, add water till solution is four times volume, turn off heat cover pot let sit overnight.
Now silver if any will be in powders with lead if any, (it should be cold enough outside to crystallize these out of solution.
(We could test for more dissolved silver with a little non-iodine table salt, but since we will be refining this again, I would not mess with that now).
Decant this gold solution, filtering into a clean vessel; let this settle to see if clear.
Now you can use precipitant of choice to precipitate gold, let gold settle.
(Make up stannous chloride solution) test a portion of solution to see if gold still in solution, if barren, then decant solution (put solution in your container to treat for waste disposal),
Wash the gold powders using Harold’s method for pure gold.(see post on getting gold pure).
Re-refine your gold or save these powders for another re-refining as you accumulate more of these powders later.
Read this through before beginning you and other members can ask questions and check this over as I may have missed some step or forgot some thing.
This is just my suggestion you do not have to follow it, but we must decide on one process and not mix several processes.
Members may have other (better methods) suggestions, you may wish to follow them instead.
Members may give suggestions to improve this then we may need to tweak this process.
