recover values from lead

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wood4lif

Active member
Joined
Apr 7, 2012
Messages
43
after processing several pounds of gold filled pocket watches i managed to accumilate a quit a bit of lead, almost a gallon jug full.
i can use some advice on the best way to recover the values that are still contained traped in the grey lead mud.
ive searched the forum and what i found it seems im a little late in following thise guidelines unless you may think i should just redigest it all in 50/50 nitric/sulfuric acid ?
????????????????
 
cu·pel   [kyoo-puhl, kyoo-pel] Show IPA noun, verb, cu·peled, cu·pel·ing or ( especially British ) cu·pelled, cu·pel·ling.
noun
1.
a small, cuplike, porous container, usually made of bone ash, used in assaying, as for separating gold and silver from lead.

check on this. (cupellation)
 
wood4lif said:
after processing several pounds of gold filled pocket watches i managed to accumilate a quit a bit of lead, almost a gallon jug full.
Click to expand...
Before I could advise anything I would need to know how you think you got almost a “gallon jug” of lead from only several pounds of gold filled pocket watches. I have never seen material like that.

You may have been exceedingly lucky in getting sterling silver core gold filled pocket watches which could give you some silver chloride with perhaps some lead chloride mixed in if you digested in aqua regia. But I still find it hard to imagine the volume you have remaining after processing several pounds.

Tell us what you did step by step from the start.
 
From what I have seen, I agree with OZ, you may have a lot more silver than lead.
 
I agree, the powder is more likely to be silver chloride than lead chloride. What strikes me as odd is his description of the powder as gray colored. Silver chloride is closer to purple in color after exposure to light.

Gray colored powder could be copper I chloride if the solution was allowed to become extremely saturated. A sample of the powder should be separated and subjected to a few simple tests:
1) Attempt to dissolve in hot water: Yes means lead chloride is a possibilty.

2) Attempt to dissolve in HCl: Yes means copper I chloride is a possibilty.

3) Attempt to dissolve in 10% ammonium hydroxide: Yes means silver chloride is possibility.

Steve
 
thanks for your input,
i should clarify that the lead chloride i have in the gallon jug is mostly water now that the lead has settled and left a light blue solution above it.
either way, it is lead that made its way through the filters when washing it with hot water.
the process i used was a simple 50/50 nitric digestion. the larger foils were easliy processed further from there, im just not to sure what the best approach is to retrieving my values left with the lead.
i did do a small sample with hcl+cl. it dissolved the Au to a nice yellow color with powders resting on the bottom. im not sure what those powders are yet. so today after work i was going to filter and see what this sample test brings, but if you have any better thoughts on it im all ears. thanks
 
Well if I were in your place I'd decant as much solution off as possible then refill your beaker with water bring to the boil and decant off while hot, if it is lead you should remove most of it in the hot water, leaving your gold, but if the volume of sludge remains the same you don't have lead so the tests Steve suggested then need doing.
 
ok. i placed the contents in the gallon jug into a 2000 ml beaker stired real good and let its contents boil for a short while. as the powders were settling ( obviously not all disollved ), i used a turkey baster to remove the now green liquid forming on top, the more liquid i removed,the more brown the grey powders were turning ..
il keep you posted as the powders settle and then il do the testing steve suggested
 
i repeated the process several times of adding water, bring to a boil and pour off the liquid untill the liquid went from dark green to a real light clear green. so im asuming most of any dissolved copper is removed along with most of the lead. im suspecting what i have left remaining is copper chloride II and whatever values were trapped in the still grey colored w/ some brown (which im suspecting to be a mix of copper and gold ) sludge.
once it settles again i will take a small sample of the powder remaining and run it through a hot hcl rinse.
ive ruled out silver chloride as a suspecting part of this group right now because i dont see any evidence of a purple color any where in this mix. correct me if im wrong
 
have you exposed it to sun light?

you may try a small sample in a little ammonium hydroxide to see if any of the powder dissolves.
 
ok i put a small sample in a spoon of ammonium hydroxide 10% and it didnt disssolve untill heated all i have left is the gold....and no change of color in the sunlight...
my next step will be to take a small sample and put in a little nitric
 
i failed to mention that when i heated the sample some pieces were jumping out of the spoon when i applied heat (lighter). so in actuality i dont know if it dissolved or it jumped out of the spoon or what "it" even is yet. ... il keep testing
 
thank you for letting me know that....but i also boiled a larger amount in a beaker over a hot plate after i tested in the spoon.. i couldnt tell any difference as far as having a lesser amount. just a slightly darker color change to a more brown/grey and much more metalic showing itself
 
yes i did the hcl test with a small amount that dried on the inside of another beaker. i just filled it up and let it sit for most of the evening, all it did was darken the heavy concentrated areas to a brown color( or maybe thats just what color of this grey precipitant does when wet ) and the area surrounding the brown was a light grey preciptant of some kind.
what i did notice tonight that my fingers tips had blackend where i must of handled some of it with out gloves this afternoon. but no purple stains on the filters after exposure to sunlight.maybe what i have left here is silver mixed with my gold. if that is the case what would you recomend being the easiest way of seperating what i have here with out using AR ?
i guess nitric would do it, dissolve the silver and what ever base metals were left and leave the gold. i would think it might take a quite a bit of nitric though. there is 750 ml in the beaker of this powder.
 
black fingers is usually silver nitrate. id try to digest it in hcl/Cl since its in powder form and precipitate with SMB. after you dissolve and filter, wait and see if anything precipitates on its own. and again after dilution, wait to see if you get a white precipitate.
 
If it is silver chloride it won't dissolve in nitric without converting it back to metallic silver. If your sure there is gold left in this I'd just use AR to remove any gold and filter and rinse the precipitant and then convert back to silver metal by either the karo syrup method or by slightly acidifying it and using zinc dust or if you have a silver cell convert it all and run it through the cell where the values will report in the slimes.
 
interesting reply from both of you for i have a reasonable size sample in hcl+cl right now from the other day i still need to filter and smb any Au values, which im doing today..but i wasnt aware of of what you just said about silver nitrate not being able to dissolve in nitric. i wish i had read your post 5 mins ago because i just put the remaining powders ( 23 grams) in nitric where it gave a little to none rection with only slight red fuming. so i was under the asumption it contained mostly Au value. so....the jury is still out yet. i guess from here i need to rinse, remelt to a metalic form and then nitric or just put the whole lot in AR.
AR is not an option for me because of my location with the lenght of time with the repeated evaporations just isnt wise. i am able to control short heated nitric digestion in a safe manner, but not AR.
il keep you posted. thanks again for your input
 
i could do what GEO suggested and put the whole lot in hcl+cl. im thinking now that woul have probably been the better way to go under the circumstances. its not to late i dont think. i just need to retrieve my powders from the nitric solution/filter/rinse as usaul but i should probably incinerate the powders to eliminate any trace nitric that remains, correct?
 

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