Bright Yellow Precipitant in Auric Chloride

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Captobvious

Well-known member
Joined
Aug 22, 2012
Messages
208
Location
Omaha, NE
Hey guys, I just had a quick question and think I know what happened mainly looking for confirmation. I was running a batch of sediment in my waste bucket that I had dumped the leftover liquid from a previous SMB gold drop from Auric Chloride (later realized there was probably still gold in the solution that simply hadn't had a chance to fully precipitate and settle to the bottom), rinse water, various HCL washes, etc. I started off by filtering off all the sediment in the bucket, then proceeded to boil the sediment (filter and all) in 32% HCL to try and remove any tin or iron in the sediment. Filtered off the remaining sludge and then proceeded to fill it back to 400ml of 32% HCL and 100ml Clorox to make Auric Chloride. I allowed the reaction to subside and moved it to the hot plate to drive off any remaining chlorine.

While it was evaporating I noticed some salts forming on the bottom of the pot.

IMG_20130722_192356_735.jpg

I decided to filter this off and it came out as this bright yellow precipitant of some sort.
IMG_20130722_192302_666.jpg
IMG_20130722_192238_445.jpg

Now my gut instinct tells me this is from excess tin or copper. Can anyone confirm or correct me please? Also does anyone think there could be gold trapped in these salts? I saved the filters just in case.
 
You'd do yourself a world of good to learn to incinerate things. If you're dealing with solutions that have been subjected to sulfur, what you are seeing may be just that---sulfur. It would be easy enough to detemine--try burning a small amount. It it burns with a blue flame and emits sulfur dioxide ---you will have your answer.

When you process materials recovered from a stock pot, begin with incineration, then follow up with a hard boil in HCl and careful rinsing. Tap water is more than adequate for this operation. That should remove anything that can be troublesome in later operations.

Test the resulting solution with stannous chloride--as HCl dissolves palladium oxide. If it tests positive, return it to your stock pot.

I wonder---when will you guys start using incineration? It's a critical part of refining.

Harold
 
Thanks Harold, I'll try that out to see if that's what happened. In the meantime I guess I'll be looking up incineration methods, which unfortunately I don't currently have the equipment for (still collecting certain recover/refining supplies... this happens to be one of the few major items I have left to procure), which also happens to be why I didn't incinerate. Good lesson to learn. I've tried roasting my filters in the past with a MAP torch but the times I've tried that bits of burning filter paper get tossed into the air and fly all over... didn't seem very efficient.
 
Gratilla said:
Looks like ferric chloride (hexahydrate), aka iron (III) chloride, ie FeCl3, to me.
If it is, I suspect it would have been eliminated by the process I suggested. Incinerating would have eliminated carbonaceous matter, and the hard boil in HCl should have put such material in solution, where it would have been eliminated. The whole idea here is to get rid of unwanted materials, leaving behind those of value.

Harold
 
HCl and bleach will form salts mostly NaCl, and a tiny bit of chlorate salt, these can hold gold chloride, a little water will dissolve the gold chloride and these other water soluble salts, if left with white salt after diluting they could be silver, or lead or even silica sand or several other possibility's, lead chloride is soluble in boiling hot water, silver chloride is not soluble in water hot or cold, the yellow color could come from metal, or since this was from the stock pot sulfur as Harold suggested.
 
Geo said:
a drop of stannous chloride would solve the mystery.

directly on the yellow salts? Guess I always thought it was for just testing solutions, I'll give that a try later.... feel kinda dumb for not already trying that... :oops:
 
you should see my table top. :oops: looks like its been painted purple. the hcl in the stannous will hydrate any dry salt and the tin will give a positive if gold is present.
 
Definite positive result on stannous test so they went into the filter/paper towel bucket for the next time I get masochistic.
 
Ugh what a mess this was to recover.... but WORTH IT! Once all was said and done I only had about 1 to 2 grams of powder dropped from the filtered clean solution and at least another 3 to 4 grams recovered from the filters, paper towels, etc following the cleanup of these yellow salts. I ended up deciding to do the recovery sooner than I planned as there was known 2.5 grams in the original solution, in addition to the foils from another pound of fingers so I knew there was a significant amount (to me anyway) trapped in these salts So here's what I did, hopefully it helps someone else in this situation...

Initially I did try to incinerate, however on my budget I was only able to setup a charcoal furnace with a cheap grill. Unfortunately I was unable to get the heat anywhere near hot enough to do anything with so I moved onto plan B. On the gut feeling that there was tin and/or copper in solution (due to the original recovery from waste solution that was admittedly, STUPIDLY added to clean known solution, and that I know I rushed the pre-cleaning of the waste salts originally) I went ahead and took the filters/towels and began introducing them into a 1:1 solution of 32% HCL and tap water totaling about 6 cups in my coffee pot. Once the solution had dissolved the filters down (after a day of sitting on medium heat as I didn't want to boil it just yet but instead just break down the paper/organics) I would continue to introduce filters and papers until again there was insufficient room for further papers. Allowed to soak in the warm HCL solution for another day until it broke down to the pulped paper sludge again. Repeated this procedure for the next two days until I had all paper towels and filters with these yellow salts (adding more clean HCL/water solution as needed) dissolved down to a pulp-like sludge. Next I took the pot off the warmer and put it on my hotplate inside a pan with sand to boil for about an hour. Allowed it to cool slightly and filtered. Took the filtered mass (filter and all) and returned it to the hotplate to boil for most of the day until the paper was pulped and solution was very dark brown. Allowed the solution to cool for about an hour and again filtered off. Following this I proceeded with the standard HCL + Clorox method intentionally using too much bleach (approximately 300 ml bleach into 8 cups of HCL) to ensure anything trapped was dissolved. I then spent the next two days filtering off this dirty AuCl, pouring off about two cups of solution at a time as the filters would fill with the pulp sludge. Using my spray bottle I then rinsed the sludge/filter 3 times to ensure all AuCl was rinsed from the sludge as well as taking sampled from the sludge and doing a stannous chloride test to make sure no gold was still there. Poured off the filtered solution into a crock and repeated this procedure 3 or 4 more times with the remaining dirty solution all the while looking for indications previously seen (cloudy solution, salts sticking to the sides of the crock, etc). As there was a rather large amount of solution at this point (approximately 8 cups in the coffee pot and 600 ml in another beaker, in addition to the presumed chlorine still in solution I evaporated it back down to a manageable amount. Diluted and dropped with SMB as normal.

This will obviously need another refining but one thing that I found curious was that the AuCl after introducing the SMB remained a light yellow with a greenish tint to it. Checked for gold in solution with Stannous Chloride which was negative reaction. For now I'm allowing it to sit and settle however after two days if anything further has dropped it's an imperceptibly small amount. My gut feeling says that there was copper still in solution (given the green tint) however it's of no real consequence either way. But in the end there was easily twice as much powder dropped from the filter recovery as was dropped from the filtered mess in the OP.

Let this be a lesson to the newbies. When you're impatient and rushing a process you WILL get nasty results as happened here. This entire week and change of recovery effort could have easily been avoided if I had A) Not introduced the dirty solution to the main solution crock B) Allowed for the solution to properly dissolve the base metals (should have boiled that for another day before making AuCl originally) and C) Just being patient.

Comments? Criticism? Fire away! :)
 
Geo said:
you should see my table top. :oops: looks like its been painted purple. the hcl in the stannous will hydrate any dry salt and the tin will give a positive if gold is present.


I will bet anyone the top of my truck is the purplest
Off all
i even have runs down the side
(Funny ,i dont ever remember spilling :shock: :lol:

Steyr223 rob
 

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