# I can't tell if I messed up or what???



## Grelko (Aug 31, 2016)

I'm wondering if anyone could shed some light on this for me? I've been trying to find an answer on here for the last few days.


In the first jar was, the dirty gold powder from the original button that I dissolved in this thread. I had kept it in a mason jar for a while, still in the solution it was precipitated in. The lid rusted and iron possibly got into it. (approx 0.7g dirty powder, that came from IC chips)

I had a second jar with AP in it (lid rusted also, possible iron), that had approx 31g of mixed material.

The material/powder in the second jar, started out as a mix of...

9g of dirty powder left over from ~4lbs plated pins
~1g from ~3/4 pound gold fingers
Around 1 pound of small plastic/mylar strips that come off the side of a flat screen TV "screens", which have gold fingers incased in plastic or glue) After incinerating, the strips weighed ~22g

After filtering the jar with AP in it, *the total material from both jars combined was ~7.8g*

I put the wet filter with the powder/material into a melting dish. There was a little plastic/glue left in it.

I added some borax, then began to re-incinerate, but ran out of fluid about halfway through. Some of it barely melted and I know some of the coffee filter was still in there "burnt".

I don't know why, but I decided to try and dissolve the material with HCl/Cl.

Made a fresh batch of stannous, and tested the solution. Negative. Added a couple more mls of Cl over the next couple hours. Still negative. The solution was VERY dark green. Total amount was approx 20ml HCL, 30ml CL.
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I came back the next day and tested the solution. Negative. I'm guessing there was alot of copper etc., still in it and a possibly a tiny bit of iron, which pushed out any gold.

I filtered the material and put the negative solution into my stockpot, just incase there actually "was" anything in it.

I used a separate beaker for the powder/material. Not sure of the weight for this, which now also has some burnt filter in it.
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Day 3, I tried HCl/Cl again, slightly lighter green solution. Stannous positive for gold finally. I filtered the solution, rinsed it down and tested it again. Negative. :?: Ok, I must have diluted it too much.

Approx 50ml HCl, 50ml Cl and ~60ml tap water. Total solution ~160ml.
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Day 4 (today) Tested negative. I figured I would try to drop the material out, to see if I did have any gold that was getting a "false positive" from iron etc.

I put sand on my hotplate, to evaporate the solution from 160ml to ~75ml, to remove the CL so the SMB works. (Hotplate with sand worked really well)

Stannous showed positive again. It looked extremely black, so I let it sit there for about 10 minutes and rinsed it off. Nice purple stain  

After the solution cooled back down, I took SMB and added maybe a gram or 2. (I'm guessing there was around 3-4g of gold in the material)

Tested with stannous, positive. Added another couple grams of SMB, still positive, a couple more... STILL positive :?: 

I continued to get a positive for stannous "purple/black on paper towel and on spot plate", even AFTER the SMB stopped giving a reaction "I added about 1 gram after that also". There was a strong sulfur smell coming from the solution. (the smell burns the eyes and nose a bit if anyone was wondering, actually made me sneeze, so I went out into the yard for a few minutes). 

Total SMB used was between 12-15g.

I've been thinking, that since the solution was ~160ml, and ~50ml of it was Cl, when I evaporated it to 75ml, if all of the tap water evaporated, there could still be up to 25ml of CL in it, which might be why it took so much SMB, and still shows positive for gold. Unless it's a false positive.

I gave it about 5 minutes and checked with stannous again. still positive, *but this time when I used stannous* , it also made an oily blue/black "grease?", that stays on top. (I have no idea what this is, possibly micro pieces of the burnt coffee filter floating on top?)

The solution is now orange-red and theres a light brown/yellow precipitate at the bottom. Looks almost like the clean gold powder precipitate in other threads.

I couldn't possibly have THAT much gold in there could I?, It has to be iron or something also? (I highly doubt there would be any PD or PL in it) There is about 1 inch of solution in the beaker and 1/2 inch of it is the brown/yellow precipitate.

I only let it settle for a few minutes, when I saw that mass of brown/yellow precipitate, so I may be mistaken on the amount. It looked like a lot.

I'm letting the solution settle for a day. There is probably alot of salt at the bottom mixed in with any gold that dropped making it look like more, since it may have been completely neutralized from adding SMB until it stopped reacting. "Even though the solution still shows positive for gold"

Anyone have any ideas?

I'm thinking about evaporating it dry and starting over with fresh AP.

The left over material, that was in the 3 filters, still has un-dissolved pieces of metal in it, which looks like alot of previously burnt filter paper "powder" and tiny gold copper flakes.

Once I get more fluid for my torch, I may just melt everything and start over. I'm going for 999 :mrgreen:


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## Geo (Aug 31, 2016)

On day two, when you dissolved the solids, did you dissolve all the solids or did you stop when you had a positive for gold? When you filtered the solution, was there any solid metal that you filtered out? Gold can cement out on iron really fast, even before it can pass through a filter. Day three, it sounds like you still did not dissolve all the metal. A simple rule for putting gold into solution, you must dissolve all the metal in the mix or the gold will not stay in solution. Go back and check the solids. Be sure to dissolve everything that will dissolve. I think you are stopping the dissolution short each time and allowing the gold to cement out of solution before you have a chance to filter it.


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## Grelko (Aug 31, 2016)

Geo said:


> On day two, when you dissolved the solids, did you dissolve all the solids or did you stop when you had a positive for gold? When you filtered the solution, was there any solid metal that you filtered out? Gold can cement out on iron really fast, even before it can pass through a filter. Day three, it sounds like you still did not dissolve all the metal. A simple rule for putting gold into solution, you must dissolve all the metal in the mix or the gold will not stay in solution. Go back and check the solids. Be sure to dissolve everything that will dissolve. I think you are stopping the dissolution short each time and allowing the gold to cement out of solution before you have a chance to filter it.



I think that might be what I did. Maybe not enough HCl in the beaker before I use the Cl. Not everything was dissolved in the first place.

The left over material that I still have in the filter has tiny flakes of gold/copper pieces in it. It looks like there's a lot of ash in it also "grey/black powder from the burnt filter"

Edit - the black powder could be gold also.

I was keeping that separate for now and trying to figure out what I did to the solution. Then finish dissolving the rest of the material afterwards.

Edit -


Geo said:


> Gold can cement out on iron really fast, even before it can pass through a filter.



That would explain a lot, thank you. I wasn't sure how quick it could cement out. I figured it would have already passed through the filter.


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## g_axelsson (Aug 31, 2016)

A couple of things...

* Incineration doesn't need borax. Only use borax when melting (or washing).
* SMB doesn't drop gold. It is the SO2 that precipitate the gold. To get SO2 you need enough free HCl or the SMB will only dissolve, doing nothing.
* Carbon (from partly incinerated filter) will absorb gold chloride. You need to make a complete incineration before going to aqua regia.

Göran


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## Grelko (Aug 31, 2016)

g_axelsson said:


> A couple of things...
> 
> * Incineration doesn't need borax. Only use borax when melting (or washing).
> * SMB doesn't drop gold. It is the SO2 that precipitate the gold. To get SO2 you need enough free HCl or the SMB will only dissolve, doing nothing.
> ...



I must have gotten mixed up the on day I tried to incinerate it. I may have been trying to melt it. I was working on a lot of other things "melting etc" that day also.

That's probably why it still shows positive then. I might have evaporated enough of the HCl to have the SMB not work.

I was trying to do this without AR, I was going to "completely" incinerate the material as soon as I got another bottle of fluid for my torch. Possibly just melt it into a bead, flatten, grind and re-dissolve with HCl/Cl again.

I'll definately be refining it atleast 2 more times because I know it's very dirty still.


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## Barren Realms 007 (Aug 31, 2016)

If you had 7g-8g of gold dissolved in the amount of solution you have you would not be getting a purple stain on your stanous test. It should show up as a black stain with that concentration. Also with the amount of solution you have and the amount of SMB you have added you will most likely be showing a false positive test.


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## Grelko (Aug 31, 2016)

Barren Realms 007 said:


> If you had 7g-8g of gold dissolved in the amount of solution you have you would not be getting a purple stain on your stanous test. It should show up as a black stain with that concentration. Also with the amount of solution you have and the amount of SMB you have added you will most likely be showing a false positive test.



The material itself was 7-8 grams (not all of it was dissolved, so I'm sot sure how much would be in solution). I think i might have 3-4 grams of gold in the solution and filter combined. Stannous showed up black "purple stain", but still shows black after all the SMB. I must be getting a false positive, maybe from the burnt paper or dissolved iron, if there's any in there?

I don't think I could get a false positive from the burnt filter. I might just be reading it wrong because of the oily black/blue grease that sits on top after I put in a drop of stannous.

If I get a chance to work on it later, I'll take a couple pictures.


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## Geo (Aug 31, 2016)

Can you show a picture of the stannous test and one of the stain left after.


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## Topher_osAUrus (Aug 31, 2016)

Grelko said:


> I don't think I could get a false positive from the burnt filter. I might just be reading it wrong because of the oily black/blue grease that sits on top after I put in a drop of stannous.




Put in a drop of stannous?

How are you testing with stannous? In a spot plate?

How you phrased that makes it seem like you added stannous to the entire solution?

Use a spot plate or cotton swab.


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## Grelko (Aug 31, 2016)

I didn't get a chance to work on it since it's raining now, but I was able to get a few pictures earlier.
I forgot to take a picture of the stain left afterwards.

I'm using a spot plate and last night I used a spot plate and paper towel.

I'm thinking that the precipitate has alot of salt mixed in.

Picture 4 has a small reflection, but it looks like oil streaks on top. In the sunlight, it looked very dark purple/black.

Could it be possible, that since I ran out of torch fluid, any little bits of plastic ended up melting into bio-diesel instead of turning to ash, leaving the oil streaks on top? Or, maybe even carbon residue from the partially burnt filter paper?

Edit - Actually, could the oil streaks be from borax re-dissolving when I evaporated the solution? It is laundry "soap" after all and looks like soap film on water. (20 mule team borax) sodium tetraborate.


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## Geo (Sep 1, 2016)

Decant what solution you have to another beaker and rinse the powder. Add the rinse into the decanted solution. Heat the solution to steaming and see if you get any reaction or color change. After an hour or so, turn off the heat and let the solution cool all the way back down. This will drive off any excess SO2 gas that may be causing the dark test results. If you are still getting the dark test result after heating and cooling, try a little more SMB. If you do not get a precipitate, check for PGM's. Take a small sample in a small bottle or test tube and add to it a small amount (a few crystals or more depending on the size of the sample) of potassium chloride and see if you get a yellow salt. You could test with DMG which would be faster if you have any.


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## anachronism (Sep 1, 2016)

Given the base material in post 1 the likelihood of PGMs has to be extremely slight. The green colour is most likely to come from the base pin material some of which is left behind before the dissolve.


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## Grelko (Sep 1, 2016)

Geo said:


> Decant what solution you have to another beaker and rinse the powder. Add the rinse into the decanted solution. Heat the solution to steaming and see if you get any reaction or color change. After an hour or so, turn off the heat and let the solution cool all the way back down. This will drive off any excess SO2 gas that may be causing the dark test results. If you are still getting the dark test result after heating and cooling, try a little more SMB. If you do not get a precipitate, check for PGM's. Take a small sample in a small bottle or test tube and add to it a small amount (a few crystals or more depending on the size of the sample) of potassium chloride and see if you get a yellow salt. You could test with DMG which would be faster if you have any.



The only items I have to use are HCl, Cl, H2O2 and SMB. I looked for potassium chloride, but the only "salt substitute" at the store was Morton's. It has Potassium Chloride, Fumaric Acid, Tricalcium Phosphate And Monocalcium Phosphate. I'm not sure if it would work properly.

I'll be decanting and rinsing this in a few moments, then evaporating and testing. I may be done before it gets too dark, so I can take a few more pictures during or afterwards.



anachronism said:


> Given the base material in post 1 the likelihood of PGMs has to be extremely slight. The green colour is most likely to come from the base pin material some of which is left behind before the dissolve.



I didn't give the second jar enough time to dissolve the material completely, so there's still a lot of copper in it.

I don't think there would be any PGMs in it. It could be a bonus, except I don't really have any way to refine them.

I have a feeling that it's just because I didn't fully incinerate the filter and added borax while doing so by mistake. Then added way too much SMB.

The only things that should be in there are... Jar 1 had gold, copper, some nickel and a tiny bit of silver (I had the button tested before I dissolved it). Jar 2 should only be gold, copper and maybe some nickel. (The TV mylars are just gold fingers on plastic)

Both jars had rusted lids, so a little iron might be in there also.


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## Grelko (Sep 2, 2016)

Well, so far so good. The orange solution is now pale yellow. Once it cooled down, it looks like silver chloride at the bottom. It's the same type of "cotton fluff" I've seen before. There's a chance that it might be tiny bits of filter also.

I did get a little dark brown powder, but it's extremely fine. It looked like mist in the rinse water until I let it settle for a while.

First of all, here is one type of the TV mylars I was talking about. 




Here is the left over material that I didn't let completely dissolve in the first place  . I'll be working with this next.




Original solution after decanting.




Before decanting, the original beaker had a yellow precipitate. After decanting, when I added water to it, most of it dissolved. It was mainly just salt at the bottom.




Stannous test for each solution. Decant on the right "orange", rinse on the left "yellow precipitate".


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## Grelko (Sep 2, 2016)

After adding stannous.




Second rinse of the yellow precipitate.




Second rinse, stannous test.




Third rinse, nice and clear. You can see a little of the recovered dark brown powder.




Stannous stains. I gave them atleast 10-15 minutes, before rinsing them out with water. The bottom middle stain, was from the third rinse stannous test. It had almost no reaction, but after a couple minutes under the flourescent lights in the garage, before I rinsed everything out, it got slightly darker.


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## Grelko (Sep 2, 2016)

This is the original decanted solution, after adding all of the rinse water. It went from 75 to 200 ml, then I evaporated it back to 100 ml. The orange is completely gone and it's a pale yellow, with what looks like cotton at the bottom. (silver chloride?) There's a little powder mixed in with it.




Stannous test after evaporating.




Stannous stain afterwards. It looked slightly purple, but more brown under the flourescent lights. (positive for gold with iron giving a false positive mixed together?)


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## Geo (Sep 2, 2016)

So you are getting a dark, almost black test result after heating and letting it cool? It's not the SMB causing a false positive. Did you add any more SMB to the cooled solution to see if you get any more precipitate?


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## Grelko (Sep 2, 2016)

Geo said:


> So you are getting a dark, almost black test result after heating and letting it cool? It's not the SMB causing a false positive. Did you add any more SMB to the cooled solution to see if you get any more precipitate?



Not yet, but I will in a minute and let you know.


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## Grelko (Sep 2, 2016)

I added 1-2 grams of SMB. There wasn't any fizzing. After I stirred in the SMB, the pale yellow solution looks more like a brown "mud water". I gave it about 10 minutes to settle, but that didn't do much. I was going to give it a few hours, or until later today to see if anything dropped. There may have been a little more of that cotton at the bottom. Also, a tiny bit of salt.

The "mud water", looks about the same color as the powder I got from the beaker with the yellow precipitate/salt in it, just more diluted.

Is there any chance, that something "maybe iron?" could have cemented out the gold in such small particles, that it's acting like a partial colloid? That could explain why it's taking so long to settle, if it even will.

I used a paper towel for the stannous test this time. It looks like the black might be a little lighter than before, possibly going dark brown or purple, I couldn't tell. I'll check it again once the sun is out.

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Edit - Could this be possible?

ferric oxide, plus stannous "tin chloride", equals ferric chloride? http://cdn.instructables.com/FHK/ROWL/FEQHFHZE/FHKROWLFEQHFHZE.MEDIUM.jpg

It could explain the orange color of my original solution if there was tin in there also. Concentrated looks almost black (stannous test result?).

The mason jar lids might have a thin layer of tin coating the steel and when it rusted, iron and tin both got into solution, giving it the orange color.

Except that, more iron "ferric oxide" got into the solution, so that when I tested it with stannous "tin chloride" it converted into ferric chloride and gave the black result? 

But, the more diluted my solution got, the more yellow it looked, possibly converting into the pigment "yellow ferric oxide?". Because the tin would have become less concentrated in solution, so the iron [stt]and gold chloride[/stt] would show up more.


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## Grelko (Sep 3, 2016)

I let the solution settle for a good 18 hours straight. It's almost completely clear, maybe a slight hint of yellow.




There is alot more of that cotton at the bottom, and a little more powder.




The stannous result is almost the same. To dilute it a little more and possibly get something besides black to show up, I tried 3 drops of solution to 1 drop of stannous.




Afterwards, I tried adding a few more drops of stannous to the result and it just gets darker.

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I was thinking about decanting the solution, evaporating it dry, adding HCl and testing with stannous.

For the precipitate (cotton and powder) I might try HCl/Cl to re-dissolve, test, dilute with cold water "incase it's silver chloride", filter, then use a little SMB to get the powder back.

The powder from the previous beaker "yellow precipitate", I was going to re-dissolve in HCl/Cl and test it also.

Edit - I made sure to buy plastic mason jar lids, so that I don't have the "rusted lid" problem in the future.


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## g_axelsson (Sep 3, 2016)

Geo said:


> Decant what solution you have to another beaker and rinse the powder. Add the rinse into the decanted solution. Heat the solution to steaming and see if you get any reaction or color change. After an hour or so, turn off the heat and let the solution cool all the way back down. This will drive off any excess SO2 gas that may be causing the dark test results. If you are still getting the dark test result after heating and cooling, try a little more SMB. If you do not get a precipitate, check for PGM's. Take a small sample in a small bottle or test tube and add to it a small amount (a few crystals or more depending on the size of the sample) of potassium chloride and see if you get a yellow salt. You could test with DMG which would be faster if you have any.


If the pH is high this won't help. Then there is no excess SO2, only dissolved SMB and that isn't affected by heating.

Göran


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## g_axelsson (Sep 3, 2016)

Grelko, have you tested to add a bit of HCl to your solution with a lot of SMB and almost black stannous test?
HCl doesn't hurt but could be what is missing. It is rarely said but SMB needs an acid to be able to drop gold. (Add acid slowly or you might get a boil over.)

When you get a black result from stannous testing try to dilute your solution. Put a drop of solution in one spot, then add a couple drops of water, mix and take a drop of this to the next spot. Repeat if necessarily in the next spot and so on... I think this is covered in one of Hoke's books.

Göran


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## Grelko (Sep 3, 2016)

g_axelsson said:


> Grelko, have you tested to add a bit of HCl to your solution with a lot of SMB and almost black stannous test?
> HCl doesn't hurt but could be what is missing. It is rarely said but SMB needs an acid to be able to drop gold. (Add acid slowly or you might get a boil over.)
> 
> When you get a black result from stannous testing try to dilute your solution. Put a drop of solution in one spot, then add a couple drops of water, mix and take a drop of this to the next spot. Repeat if necessarily in the next spot and so on... I think this is covered in one of Hoke's books.
> ...



I forgot to check the PH of the solution. I haven't tried adding HCl to it yet. That may just fix the problem.

I remembered reading about the stannous "acquaintance test" in the book, I was going to do that today. Thanks for reminding me. 

I have a feeling that it would be orange going towards yellow, like the original solution did when I diluted that, but we shall see.


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## Grelko (Sep 3, 2016)

1. 5 drops solution, 5 drops stannous.

2. 5 drops solution, 5 drops stannous, diluted with 5 drops of water.

3. 5 drops solution, 5 drops stannous, diluted with 10 drops of water.

4. empty.

5. 5 drops solution, 5 drops HCl

6. 5 drops solution, 5 drops HCL, 5 drops stannous. Also, I used a paper towel to soak up the solution in this test. The black precipitate was almost solid and came out in 1 piece.

Edit - The PH is around 5.5


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## Geo (Sep 4, 2016)

Take the solution you have left and make sure it has excess HCl. Add a solid piece of copper and see if anything cements out. It will be easier to cement any values and start over.


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## g_axelsson (Sep 4, 2016)

pH 5.5 is almost neutral. Add some HCl to it.

I was too lazy to calculate the strength of the acid... so I googled it.  http://www.oxy.com/OurBusinesses/Chemicals/Products/Documents/hydrochloricacid/tech-calculated_ph_values_HCl.pdf
pH 5.5 is 0.00001150 % HCl in water (by weight)!
In fact, you probably would lower the pH by putting your hands into the solution! *Do not do this!!!!*
Natural skin surface pH is on average below 5, which is beneficial for its resident flora.

Göran


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## Topher_osAUrus (Sep 4, 2016)

Those tests look more brown than purple.

Sure its not a false positive?


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## Grelko (Sep 4, 2016)

Geo said:


> Take the solution you have left and make sure it has excess HCl. Add a solid piece of copper and see if anything cements out. It will be easier to cement any values and start over.



I should be able to do this later tonight. I might give it a couple days to see if anything drops (or heat it). If I would have just added copper in the first place, I'd probably be done by now.



g_axelsson said:


> pH 5.5 is almost neutral. Add some HCl to it.
> 
> I was too lazy to calculate the strength of the acid... so I googled it.  http://www.oxy.com/OurBusinesses/Chemicals/Products/Documents/hydrochloricacid/tech-calculated_ph_values_HCl.pdf
> pH 5.5 is 0.00001150 % HCl in water (by weight)![/url]
> ...



Thanks for that link (wow, I sure didn't have much HCl in there). I was going to add enough HCl, to see if I can get the PH back down to 1-2, then put in copper.



Topher_osAUrus said:


> Those tests look more brown than purple.
> 
> Sure its not a false positive?



It has to be, I haven't seen anything besides black/brown stannous results in the last couple days.

Any powder that I get from the 2 beakers, I was going to add to the rest of the material and re-dissolve it (completely this time).


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## Grelko (Sep 6, 2016)

Well.... I know what should be wrong with my solution and why the stannous tests are black/brown.

I started dissolving the rest of the material from the original filter. The solution was almost black until I added about 20ml of water to the HCl/Cl. It turned darker green, but the stannous was still black.

I decanted about 3/4 of the solution to a separate beaker, then added fresh HCl/Cl to see if I could get the rest of the material to dissolve.

This time the solution was light green/yellow and had black pieces floating "burnt filter I'm guessing".

*I looked up under the bottom of the beaker, to see what needed dissolved and saw 10-15 small MLCCs* :lol:  

I couldn't see them before, because of all the black powder/chunks at the bottom. When I filtered the original solution, they stayed in the filter, so I had no idea they were even there.

I'm not sure how I got those mixed in with the material, but after I had solution light green/yellow, I tested with stannous and it quickly went orange, then black. The stain looks dark grey/black with a hint of purple.

Edit - Since I still have the other beaker with a piece of copper in it, I should probably combine the solutions, now that I know what went wrong and cement all values.

Edit 2 - These little buggers were the problem.


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## Grelko (Sep 8, 2016)

Ever since I started this hobby, not much of it has worked out right. Either I'm too busy, or it's raining etc.

Atleast I can always count on you guys and the forum for help and great information. Plus, I can count on Copper to do it's job  

More dropped out than I thought would, but there's probably a bit of copper in it now.

I'm letting the powder dry out over night, then "completely" incinerating it tomorrow, to make sure I don't have anymore bits of filter in it, if it's not still raining.

I am going to scrape the filter clean once the powder is dry, then add it to my other filters, instead of burning it along with the powder this time.

I thought the stannous was still showing a very slight purple, but it was the flourescent lights (Stannous finally looks clear now) I checked it under different lighting also. By the off chance I missed any PMs, they're in my stock pot.

I'm guessing it looks grey-ish in the picture because the CuCl2 is diluted with stannous and the lighting. Also the solution got stirred up while scraping the copper, so it might be tiny bits of black powder floating around.

Solution on top, stannous test on bottom.




When you guys say it "cements" to the copper, you arent joking. It was hard to get off. I used a tooth brush instead of a wire brush, so that I didn't get any bits of iron mixed in. Afterwards, there was still a tiny bit of black on the copper that wouldn't come off "even after 5 minutes of scrubbing at it", but I'll eventually dissolve that piece someday.

Edit - *The tooth brush will never be used for anything besides scraping PMs from copper.*




Dirty powder in the filter. So far so good.


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## Barren Realms 007 (Sep 8, 2016)

You are developing your patience I see. Nice job. :mrgreen: 

Now you need to learn to let the material settle and siphon off the liquid and you will have less filter material to work with and more sediment to work with.

Hobby, home refiner needs to develope a different mind set than a commercial refiner at times.

Your getting there. Patience.  :G


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## Grelko (Sep 8, 2016)

Barren Realms 007 said:


> You are developing your patience I see. Nice job. :mrgreen:
> 
> Now you need to learn to let the material settle and siphon off the liquid and you will have less filter material to work with and more sediment to work with.
> 
> ...



I have tons of patience haha, I normally do wait and decant the solution, but I was excited to see how much powder dropped to the bottom of the beaker, so I filtered it instead.

I was thinking, if I did happen to have any AgCl mixed in, I probably shouldn't incinerate it just yet. Re-dissolving and filtering it out first would probably work better.

I've been reading for the last hour, about AgCl and I'm thinking, as long as I don't actually melt the powder, I should be ok and not lose any silver as fumes, because it'll turn into silver oxide (Or have I gotten this part wrong?). I know you shouldn't let AgCl dry out.


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## Barren Realms 007 (Sep 8, 2016)

Grelko said:


> Barren Realms 007 said:
> 
> 
> > You are developing your patience I see. Nice job. :mrgreen:
> ...



You are correct in the fact that you have gotten this part about the AgCl loss correct. Once you have put a flame to it you have lost values because of the silver chloride to elemental silver step has been removed. The silver chloride changes it's structure once a flame is put to it. Either covert the silver chloride to elemental silver and remove the silver then the PM's or remove the PM's before converting the silver chloride to elemental silver.

Most of the time as a home refiner or hobby refiner it not an easy decision to make. But once you make the decision or how you will process the silver or silver chloride then stick with that decision so you are limiting the number of processes you are doing to recover values.


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## Grelko (Sep 9, 2016)

Barren Realms 007 said:


> You are correct in the fact that you have gotten this part about the AgCl loss correct. Once you have put a flame to it you have lost values because of the silver chloride to elemental silver step has been removed. The silver chloride changes it's structure once a flame is put to it. Either covert the silver chloride to elemental silver and remove the silver then the PM's or remove the PM's before converting the silver chloride to elemental silver.
> 
> Most of the time as a home refiner or hobby refiner it not an easy decision to make. But once you make the decision or how you will process the silver or silver chloride then stick with that decision so you are limiting the number of processes you are doing to recover values.



Now, is that the actual flame touching the silver chloride? I have a small crucible that I can heat from the side or bottom, until everything is glowing red, so the flame wouldn't actually be touching any powder.

I'm not 100% sure on refining silver as of yet, so I'd be going after the gold first.

Please correct any mistakes if you see them.

I was going to incinerate the powder, then re-dissolve it with HCl/Cl. I think that cotton fluff "AgCl?" will be at the bottom of the beaker again, so I can filter it out (Would I need ice cubes for anything?). Take the gold bearing solution "possible PGMs from those MLCCs" and heat it, to remove the Cl.

Drop the gold with SMB, settle, filter or decant and rinse it, so I have "cleaner" gold powder. The HCl/Cl and SMB solution might have PGMs in it, so I'll put in a piece of copper to drop them out.

I shouldn't need sulfuric, because there shouldn't be any lead in this. If there was, it would still be in solution, while the copper dropped the PMs out.

The gold powder will be rinsed with "warm/hot" HCl, distilled water a few times each, until clear, then re-dissolved etc, again. I was going to do this until the gold powder is a light "blond" brown. 

Add just enough borax to glaze a new melting dish (after heating the dish to get any water out) and after melting, I should have a nice clean button that's possibly 999. :mrgreen: 

Any borax that's stuck to the button, I was going to boil off in distilled water, since I don't want to use sulfuric.

Do I even need borax to melt clean gold powder, or can I just melt it into a bead?


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## Geo (Sep 9, 2016)

Place the copper in a container like a butter bowl and let it dry completely. Any precious metals will dry and flake off.


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## g_axelsson (Sep 9, 2016)

Looking good! The copper plate and cemented powder that is.

When I get powder, sediments or foils stuck in a filter I usually wash it down into a beaker with a squirt bottle and the filter paper against the inside of the beaker. With the filter flat against the glass it is easy to wash off most of the content. Then the filter goes into my incineration pile if there was any values in it from start.

That copper piece can be used again for cementing values and when you are finished with it you just put it in the stock pot and let it dissolve.

Göran


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## Grelko (Sep 9, 2016)

Geo said:


> Place the copper in a container like a butter bowl and let it dry completely. Any precious metals will dry and flake off.



That's great to know, thank you.  I wasn't sure if I'd have to wait until I dissolved it to reclaim any smal pieces that were stuck to it.



g_axelsson said:


> Looking good! The copper plate and cemented powder that is.
> 
> When I get powder, sediments or foils stuck in a filter I usually wash it down into a beaker with a squirt bottle and the filter paper against the inside of the beaker. With the filter flat against the glass it is easy to wash off most of the content. Then the filter goes into my incineration pile if there was any values in it from start.
> 
> ...



I normally just take the filter after it's dry and dump any powder into a container. Fold the two sides and rub them together over a paper plate, or just the container itself and add any powder to the rest of it. Then I add it in with my other filters to incinerate later.

The way you do it should work better, so I'll have to try that next time. My filters look like they still have a thin coating on them.

I was going to continue using that piece of copper until it got too thin, then toss it in the stock pot.


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## Grelko (Sep 9, 2016)

I've been thinking,

Instead of converting AgCl to Ag with Karo and NaOH, if this article is accurate, wouldn't it be easier to do this instead?


Faraday induced the mechanochemical reduction of AgCl with Zn, Sn, Fe and Cu in 1820, using trituration in a mortar. 
(I haven't looked for his actual reasearch papers from back then yet.)

The bad news is that the PDF costs almost $40. The good news, is that the sentence above basically explains what he did.

This article says that it'sa a re-visit of the experiment. They use a ball mill etc. I didn't read the PDF to see exactly how it works though.

http://link.springer.com/article/10.1007/s10973-007-8479-8

Other sites explain it a little more, but it looks as if all he did was grind AgCl and one of the other metals in a mortar and it'll convert to Ag without using any chemicals. It seems to be a pressure conversion. *Edit - Spontaneous dehydration*

Then all you would have to do is rinse it with water, since the chlorides of Zn, Fe, Sn and Cu are soluble in it, but Elemental silver isn't. You could also use acetone for some of these.

Section 1.1.1.2 explains the process a little more.

https://books.google.com/books?id=FldqbSffUMgC&pg=PA3&lpg=PA3&dq=faraday+experiment+with+%22agcl%22+1820&source=bl&ots=-RUheOlt0M&sig=tHMjQ_MebtdGqPUPzG8EnKWUJpw&hl=en&sa=X&ved=0ahUKEwi6y8Wv3oPPAhVFfiYKHTikDQ0Q6AEILTAD#v=onepage&q=faraday%20experiment%20with%20%22agcl%22%201820&f=false


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## Topher_osAUrus (Sep 10, 2016)

Did you look up and see what trituration is?
I believe its much more in depth than just beating up the silver chloride :lol:


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## Geo (Sep 10, 2016)

Silver chloride can be converted with HCl and aluminum, or sulfuric acid and steel.


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## Grelko (Sep 10, 2016)

Topher_osAUrus said:


> Did you look up and see what trituration is?
> I believe its much more in depth than just beating up the silver chloride :lol:



Who knows, maybe all you need to do IS smash it together? I might try this someday.  I noticed while grinding up small wet pieces of broken ICs, that the pressure/friction did cause them to dry out pretty fast. Maybe it's possible that the Cl bonds are broken and move to the Zn, sort of a "dry" version of the reactivity series?

I read the part about lactose and other medical definitions for the word, except this isn't organic chemistry. I just figured since the research was from 1820, It would use the definition of it from back then. 

http://www.merriam-webster.com/dictionary/triturate (since 1828)
1. crush, grind.
2. pulverize and comminute thoroughly by rubbing or grinding

Origin and Etymology of triturate
Late Latin trituratus, past participle of triturare to thresh, from Latin tritura act of rubbing, threshing, from tritus, past participle — more at trite
First Known Use: circa 1755



Geo said:


> Silver chloride can be converted with HCl and aluminum, or sulfuric acid and steel.



Thanks Geo, all I knew about was Karo and NaOH. I'll most likely go with HCl and aluminum, instead of using sulfuric for now.


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## g_axelsson (Sep 10, 2016)

Yes, it is just grinding and smashing the silver chloride together with something else to get the reaction going.

The article can be found at sci-hub.ac by searching for the doi number. The author uses a ball mill, and after 20 minutes have a 97% conversion rate of their 6g sample. In the end they had silver, silver chloride, zinc, zinc chloride and zinc oxide. The reaction is compared to the thermite reaction but not as violent but the energy released is enough to create localized melting driving the conversion forward and a sudden jump in temperature.

Instead of zinc a number of other metals can be used, for example copper, iron, chrome, tin. It seems like the conversion rate has little to do with the energy released but is more dependent on the hardness of the metal, chrome gave very low conversion rates while copper and especially tin powder gave higher rates, almost as high as zinc.

I think it is an interesting reaction but nothing practical for refining. There are too much contamination compared to the rather clean conversion with NaOH and sugar.

Göran


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## Grelko (Sep 10, 2016)

g_axelsson said:


> Yes, it is just grinding and smashing the silver chloride together with something else to get the reaction going.
> 
> The article can be found at sci-hub.ac by searching for the doi number. The author uses a ball mill, and after 20 minutes have a 97% conversion rate of their 6g sample. In the end they had silver, silver chloride, zinc, zinc chloride and zinc oxide. The reaction is compared to the thermite reaction but not as violent but the energy released is enough to create localized melting driving the conversion forward and a sudden jump in temperature.
> 
> ...



You'd still need to rinse the material, plus dissolve the zinc or other metal away with HCl at the end to be able to separate your silver "metal". Still, getting a 97% conversion rate isn't bad for just smashing it together.

Could someone please explain how the HCl and Aluminum process would work? Is it just a simple conversion, dropping the silver out as powder "elemental silver" or is it more involved than that?



g_axelsson said:


> The reaction is compared to the thermite reaction but not as violent but the energy released is enough to create localized melting driving the conversion forward and a sudden jump in temperature.
> 
> Göran



Nice. 8) It's almost like rubbing 2 sticks together to start a fire.


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## Topher_osAUrus (Sep 10, 2016)

That IS interesting stuff...I am quite curious now.. And have much reading to do about it.

Göran, what do you think is the best method for AgCl conversion when there is PGM contaminates as well as lead sulfate?

I was planning on iron and sulfuric, but, a thread i recently viewed, gsp mentioned a book that had 100 or so different conversion methods for silver. So, I figured, out of that many...there has to be one that is better suited for my needs.


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## g_axelsson (Sep 10, 2016)

I have never liked to work with silver chloride and all my tests of converting with sugar have been failures or at least messy. Since I have plenty of copper from scrapping and found reasonable cheap nitric I prefer to treat the silver chloride with lye, converting it to silver oxide and then dissolving it with nitric and cementing on copper.

Lead sulfate should stay undissolved by the nitric and if it dissolve it doesn't cement on copper.

PGM:s should only exist in trace levels since their chlorides are soluble and can be washed away. If there are some PGM:s after cementing on copper it will be sorted out in the cell.

This might seem like an odd way to treat silver chloride but it works for me and my situation. I usually work in grams rather than kilos of silver chloride (from gold refining and MLCC:s). Most of my silver comes from keyboard films and contact points. But I'm just a small time hobby refiner and if my situation or type of scrap changes I might reconsider how I work.

I must put up a warning though, dry reduction of silver chloride with zinc powder is an exothermic reaction and if scaled up too much it might literary blow up in your face. The researchers compared that reaction to thermite and surface area (=heat dissipation) and volume (=stored energy) doesn't scale at the same rate. 8 times the mass have only 4 times the surface area so the heat buildup in a big batch will be larger than in a smaller batch. At some point the heat won't dissipate fast enough and you got a runaway reaction and a potential explosion.

Göran


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## Topher_osAUrus (Sep 11, 2016)

Yes, silver chloride is kind of annoying. I can see why Hoke spoke of it with such disdain. I should have been a more "serious student" in the beginning, and been careful to not create as much....but, i have a large pickle jar half full of it that needs done, and I am certain there are values. I think I will try the lye method you spoke of.

Thanks for the tip G


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## anachronism (Sep 11, 2016)

Topher_osAUrus said:


> Yes, silver chloride is kind of annoying. I can see why Hoke spoke of it with such disdain. I should have been a more "serious student" in the beginning, and been careful to not create as much....but, i have a large pickle jar half full of it that needs done, *and I am certain there are values. * I think I will try the lye method you spoke of.



Yes I would define half a pickle jar of silver chloride as values too. You're better off with the sulphuric/nails approach by a country mile over the lye thing.


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## Topher_osAUrus (Sep 11, 2016)

anachronism said:


> Yes I would define half a pickle jar of silver chloride as values too. You're better off with the sulphuric/nails approach by a country mile over the lye thing.



:lol: 

Yeah, it's been collecting for a couple years..

I have much, much more cemented silver than silver chloride now.. And much more sterling and scrap silver to process. I don't advertise that I buy silver, just gold. It just seems that everyone who sells me bulk goldfilled, always has a little bit of sterling they want gone too.

I have sulfuric, and I have nails.. Ill give it a whirl.


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## Grelko (Sep 11, 2016)

Grelko said:


> After filtering the jar with AP in it, *the total material from both jars combined was ~7.8g*



I decided to go for the gold first, so I went ahead and incinerated the dry material, that was left after dropping it with copper.

There was a small amount of white smoke, which must have been the silver chloride.

After refining this 1 time (then needing to drop it with copper) and "completely" incinerating it, *it now weighs 2.862g* (I bought a better scale)

The dry powder after incinerating still looks pretty dark brown, but I was still going to refine this atleast 2 more times.

I may re-dissolve this later tonight. It's already dry and in my 50 ml beaker.


Sadly, I don't have a graphite crucible, so I had to use my stainless one.
I'm not sure if this would contaminate the powder with iron again or not?


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## Grelko (Sep 12, 2016)

So apparently, I have Platinum in my material.

First things first. Stannous stain is nice and purple.

Nothing else in the beaker seems like it will dissolve. There is now almost 2-3x the amount of "fluffy" material in the bottom. It looks like an actual black sponge, but it's mixed with copper in HCl/Cl, so it looks a bit green also. Some of it is floating also.

After decanting a bit of the solution, I tried adding more HCl/Cl to it and tested with stannous again. It looked nice and orange for about 2 seconds, then went black.

I was going to filter the solution, to catch the sponge material (no idea what to do with this yet, dry it out?), then heat the solution to remove the Cl and drop the gold.


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## Grelko (Sep 20, 2016)

I finally got a chance to drop the gold and rinse it. It was medium-light brown after it dried.

I decided to re-dissolve and clean it once again, since I'm trying to get 999...

Of course, like always, something goes slightly wrong...

Did you know that HCl/Cl evaporated until it's dry, looks like scrambled eggs?

Well, now you do :| 






I'm guessing that I should either add a little distilled water, or HCl to it now, and re-dissolve it yet again.

I'm wondering why the outside turned orange?

Edit - distilled water worked great, the dried salts went right back into solution.


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## nickvc (Sep 20, 2016)

Topher_osAUrus said:


> That IS interesting stuff...I am quite curious now.. And have much reading to do about it.
> 
> Göran, what do you think is the best method for AgCl conversion when there is PGM contaminates as well as lead sulfate?
> 
> I was planning on iron and sulfuric, but, a thread i recently viewed, gsp mentioned a book that had 100 or so different conversion methods for silver. So, I figured, out of that many...there has to be one that is better suited for my needs.



The best way to separate the PGMs which I think will be in solution is to wash and filter the silver chloride fully till the solution coming from it is literally water, cement that solution with copper and convert the silver chloride with the method of choice. To get the silver totally free of other values a silver cell is the best option and very easy to set up and run, I believe Palladium described and showed his mini silver cell which was excellent.


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## Grelko (Sep 20, 2016)

Well, I think everything is back in order now.

I believe that after I accidently evaporated the solution dry, the auric chloride "AuCl3" turned to salt crystals, and around the edges where it was more orange, was chloroauric acid "HAuCl4" crystals.

I was going to reacidify the solution with HCl, but decided to use a tiny bit of SMB first. I was really surprised to see that it worked and I had the cleanest drop I've seen so far.  The wet powder is basically light brown and the stannous test was negative.

Possibly tomorrow, I'll rinse the powder, but I still need to wait until my other melting dishes arrive before I can turn it into a small button.


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## Grelko (Sep 23, 2016)

My new melting dishes arrived, so I took that bit of clean powder I had and made a tiny bead. Well, it "was" a bead, but I pulled it out of the dish too early and squashed it. :lol: It got stuck to the tweezers with borax.

There is still a small amount of black powder in a coffee filter, that may have a little platinum in it, along with at least another .45g of gold (the button from the begining had around .5g). Even though I dissolved everything I could, there was a sponge like material, that I saved to work on later.

All solutions that showed negative, were added to my stock pot for later, so nothing is going to just magically disappear.

You guys are right, it IS hard to take a photo that shows how shiny the gold actually is.

Also, this is my first "real" button. The other bead that I have in the gallery, was just bonding wires "gold panned out" and melted, not refined.


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## g_axelsson (Sep 24, 2016)

Making a pipe with tweezers is to cheat! :mrgreen: 

Now you know how good gold is looking after a melt and you will never be satisfied with less.

Good work!

Göran


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## Grelko (Sep 24, 2016)

g_axelsson said:


> Making a pipe with tweezers is to cheat! :mrgreen:



Shh :lol: Don't tell anyone, they haven't noticed yet. :wink: 

I'm trying to figure out why the rest of the material didn't dissolve. It has to be from the partially burnt filter from the begining, but that has already been re-incinerated to ash, and refined 2 times, filtered and rinsed.

I'm going to see if I can get that black sponge material to dissolve, or I can try to melt it, to see what it actually is. If it does happen to be platinum, I shouldn't be able to melt it with my torch. "mapp gas"


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## Grelko (Sep 26, 2016)

Well, I took that tiny bead to the jewelry store and they tested it with their XRF.
I guess I still need to refine it one more time :roll: I'm pretty sure I refined this 4 times already, 1 more couldn't hurt. :lol: 

90.77 Au
2.31 Ag
2.49 Cu

Also, I took down small silver bead from my other thread about mylars (not just keyboard, but microwaves etc.), where all I did was melt them in a small covered crucible on my hot plate for a couple hours, (until it was a mix of black/white ash), then use the "static cling" from a balloon to collect the silver. It turned out at almost 99%. I think it showed 98.92.


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## anachronism (Sep 26, 2016)

Grelko.

Don't keep re-refining it ad infinitum if you're getting such high levels of impurity. You're trying to work with the tiniest of quantities in the spectrum where the losses as a percentage of your gold are the highest, and if you are still getting high levels of Ag and Cu after 4 refines then to be honest you've got something going awry that you need to improve upon. You're learning to get fine gold and that's far less of a frustrating procedure to learn when you're learning to do it with a couple of grammes. I would suggest from experience that one good refine (not recovery) on a few grammes using all the techniques you have learned so far (and executed correctly) would probably get you fine gold. 

I'd put this little fella to one side and recover some more. Go grab some more feedstock, learn it with a larger amount and then use what you learn on this first button if you still want to. Of course you may want to put it to one side for ever and say it was your first!


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## Grelko (Sep 26, 2016)

I think I know what my problem was.

Using cold rinses instead of warm/hot.

I didn't filter the solution that final time, I decanted/rinsed it, which would leave the silver at the bottom mixed in with the gold powder, instead of in a filter.

The copper, was most likely not rinsed out good enough. (Because of the cold rinses)

I have enough material that I can keep practicing with. 8) I'll get that 999 eventually.


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## anachronism (Sep 27, 2016)

You can take out the silver and the copper with hot concentrated washes of HCl. There are conflicting opinions on the forum with regards to temperature, however I've always favoured hot. Yes it opens the door to a tiny dissolution of gold however this harks back to my comments regarding the quantity of gold you are trying to refine and the economies of scale. 

I have never ever put gold powder in a filter and I don't understand the logic of doing so to be honest. It seems like a pointless exercise to me.


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## Grelko (Sep 27, 2016)

anachronism said:


> You can take out the silver and the copper with hot concentrated washes of HCl. There are conflicting opinions on the forum with regards to temperature, however I've always favoured hot. Yes it opens the door to a tiny dissolution of gold however this harks back to my comments regarding the quantity of gold you are trying to refine and the economies of scale.
> 
> I have never ever put gold powder in a filter and I don't understand the logic of doing so to be honest. It seems like a pointless exercise to me.



That would definitely be the reason copper and silver were still in there. I should have used hot rinses.

My mistake, I should have instead said, that I didn't filter it the final time while the gold was still "in solution", like I normally would to catch any trash, solid pieces, or AgCl.

About the tiny bead, I meant that I wasn't going to re-refine it "by itself". I have more material that I'm processing and will be adding it to process along with the bead when it's finished.

I'll be sure to properly do the rinses/filtering next time and possibly, finally get my first 999 gold.


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## anachronism (Sep 27, 2016)

Thanks for clarifying Grelko. 

What kind of filtration are you using? If you cannot read a newspaper through the solution in total clarity then there's a very good chance that you still have silver chloride particles in your AR. Good filtration is an absolute "must have" and the vast majority of AgCl can be removed this way.


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## nickvc (Sep 27, 2016)

It also pays to allow your solution to settle well before the final filtration to allow any chloride to settle on the bottom which can take time and the simple trick of putting your solution through the same filter twice works well with catching small particles.


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## Grelko (Sep 27, 2016)

anachronism said:


> Thanks for clarifying Grelko.
> 
> What kind of filtration are you using? If you cannot read a newspaper through the solution in total clarity then there's a very good chance that you still have silver chloride particles in your AR. Good filtration is an absolute "must have" and the vast majority of AgCl can be removed this way.




Edit - After I filter my solutions, I have a problem with squeezing the last drop or 2 out of the filter. This would force material through the coffee filters and dirty up the solution again. I need to stop doing that.

I'm using coffee filters for now. Depending where I am in the process, I might use 3 or 4.

Since I didn't filter it that final time, once I dropped the gold out, I made sure and decanted it until it was completely clear, no haze at all. (I normally rinse it until it's completely clear)

Just to make sure that everyone knows, I'm not using AR to dissolve, just HCl/Cl. I still haven't tried using nitric yet. I probably won't until I have a proper lab set up and I have no idea when that'll be.



nickvc said:


> It also pays to allow your solution to settle well before the final filtration to allow any chloride to settle on the bottom which can take time and the simple trick of putting your solution through the same filter twice works well with catching small particles.



When I put gold into solution with HCl/Cl, I'd give it half a day or more (sometimes a few days if I'm busy), filter, then evaporate about 50% to make sure the CL is out before adding SMB.

I'm thinking that when I accidently evaporated the solution dry, whatever was still in it dropped out when I added Dwater to it, since it would be close to neutral. I should have added HCl instead.

I'll remember to run the solution through the same filter twice for certain parts, especially at the end, or if it was very dirty to start with, thanks for the idea.


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