What's happening here?

[Barren Realms 007]

I have a small batch that I have been working on. Here are the steps I have taken after gold removed from items.
Wash and boil with water to clean solution of any previous contaminants(3 times).
Wash with HCL and let sit over night. No color change to indicate base metals.
Wash again with new HCL and bring to a good boil for 15-30 min. Let settle.
Dilute and wash with water.Let settle.
Wash with water.Let settle.
Wash with water. Let settle.
Wash with water and boil for 15-30 min.
Do another round with HCL as above(3 times).
Wash with water again and boil as above(3 times).
Wash with house hold ammonia.
Wash with ammonia again and boil for 15-30 min.
Each wash up till this point the water and HCL were removed by siphoining off the liquid.
Go thru wash process with water again 3 times. Filter the liquid after solids have settled.

My ingrediants on my ammonia bottle say Ammonium Hydroxide & Surfantant.
My solids will settle but I have this persistant cloudy solution as seen in the coffe pot on the left in the picture.
I took the filtered stuff in the center of the picture and mixed up a batch of 2 cups HCL w/1/2 cup clorox. I placed the filter in the mix for about 10 minutes to recover what gold might be in there. I filtered this again as seen in the center of the picture and this is what filtered out, same as before I put it in HCL/Clorox. The solution on the right is what came out of this mix. I did a test on it and got a slight color reaction. And it could be just the color from the solution. My testing solution should be good. The stuff in the filter I guess should just be silver cloride.

Should I run the filtered stuff in hot HCL/clorox? Or did I let it set long enough to recover the gold from it?

This is the correct Ammonia to use to remove the silver isn't it?

Since there has been no color changes in the solution during washes and rinses I feel the lead and tin and other base metals are gone.

Does the color of the HCL/clorox solution indicate something I am missing?

Would I be safe in siphoning the water out of the coffee pot evaporating the reamaning water (with out completely drying the solution) and do my HCL/Clorox treatment?

 

[Oz]

It sure would help to know the starting feedstock.

 

[Anonymous]

Ammonium Hydroxide & Surfantant.
?

Surfacant, that is soap of some sort, helps lift dirt, keeps stuff suspended.

Jim

 

[Barren Realms 007]

The feed stock was removed from pins and fingers.

Yea I know about the surfactant, I assume it is just keeping the silver cloride suspended in solution.

The setting time for this after the ammonia step was done has been about 8 hours. The PM's should have settled since I didn't get much reaction from the filtered material.

 

[lazersteve]

I'm going to assume this black (?) material is from a sulfuric stripping cell.

Here's how I would proceed from this point forward.

1. Rinse the entire contents of the filter into a straight walled beaker and cover the black sediment with HCl to twice it's thickness in depth.

2. Heat to 60C.

3. Add 10 mL of Clorox and stir until the solution no longer fizzes with tiny bubbles.

4. Repeat Clorox additions with vigorous stirring after each until color of sediment changes from black to a tan/light brown/gray or completely dissolves, whichever comes first.

5. Test solution with stannous chloride for gold.

6. Do a coarse filtration on the the liquid to remove the bulk of the sediment.

7. Thoroughly rinse the sediment in the filter.

8. Perform a final fine filtration through a vacuum filter paper and a frit or with a charmin plug.

9. Heat the filtered solution on low heat to drive off any excess chlorine.

10. Add SMB to precipitate the gold.

If the material is not from a cell I may proceed differently.

Steve

 

[LeftyTheBandit]

When you add your stannious do you see color then it disappears?

Your acid solution may be too concentrated. Take a small sample (drop) and dilute 50% with water and test again. You may be dissolving it as fast as it indicates. (this has never happened to me, I have seen others talk of it though)

That orange color to your Acid Clorox solution is similar to an iron contaminated solution I had. If it is iron contaminated you will need to drop and treat the precipitate again with either HCl or Nitric to remove iron.

I learned that using a magnet on your feedstock before digesting will pay dividends when iron is involved. (Harold)

I must admit, your washing is commendable.

 

[Barren Realms 007]

I'm going to assume this black (?) material is from a sulfuric stripping cell.

Here's how I would proceed from this point forward.

1. Rinse the entire contents of the filter into a straight walled beaker and cover the black sediment with HCl to twice it's thickness in depth.

2. Heat to 60C.

3. Add 10 mL of Clorox and stir until the solution no longer fizzes with tiny bubbles.

4. Repeat Clorox additions with vigorous stirring after each until color of sediment changes from black to a tan/light brown/gray or completely dissolves, whichever comes first.

5. Test solution with stannous chloride for gold.

6. Do a coarse filtration on the the liquid to remove the bulk of the sediment.

7. Thoroughly rinse the sediment in the filter.

8. Perform a final fine filtration through a vacuum filter paper and a frit or with a charmin plug.

9. Heat the filtered solution on low heat to drive off any excess chlorine.

10. Add SMB to precipitate the gold.

If the material is not from a cell I may proceed differently.

Steve

None of this came from a cell Steve.
This was harvested with HCL in crock pot (no peroxide added) for the pins. And AP for a few grams from fingers.
Both batches were kept seperate till after the last wash and were combined just before the ammonia washing.

I figure there is still possibly some PM's in this filter that is why I am asking now rather than later for oponions. :shock: :roll: :lol:

Steve since this is not from a cell what would be your other suggestion?

Thanks

 

[lazersteve]

Incinerate the powder to red heat. Be cautious of the fumes.

After incineration try a small sample in HCl again and see if you get a reaction. If not try the procedure I posted above on a separate small sample.

I agree with Lefty, the solution looks like it contains some iron.

Any details on how you arrived at the powder? What color changes did you see in the original solution and powder?

Steve

 

[Barren Realms 007]

When you add your stannious do you see color then it disappears?

Your acid solution may be too concentrated. Take a small sample (drop) and dilute 50% with water and test again. You may be dissolving it as fast as it indicates. (this has never happened to me, I have seen others talk of it though)

That orange color to your Acid Clorox solution is similar to an iron contaminated solution I had. If it is iron contaminated you will need to drop and treat the precipitate again with either HCl or Nitric to remove iron.

I learned that using a magnet on your feedstock before digesting will pay dividends when iron is involved. (Harold)

I must admit, your washing is commendable.

Hi Lefty, yea that was kind of the way it seemed to happen. And I think you might be on to something there.
The picture below shows 2 filters and 2 Q-tips. The filter on the left was the first test that was done you can see a slight bit of color. This was done just before the first message post. The stain on the filter on the right is with your suggestion. I took one Q-tip and put about 3 drops of solution on a plate and then took a 2nd Q-tip and put about 3 drops of water on the plate I mixed it together with a 3rd Q-tip. The stain on the right was the result when this mix was put on the test solution on the filter paper. The Q-tips had no stain on them and I put some test solution on them and got the color you see. So I would aay you are correct in the saturation being a possible problem.


The orange color of the solution gave me the same thought about the iron that was what made me start this thread and ask before I went any farther. I started to do a run in sulfuric but haven't yet. I will admit I didn't use a magnet on the pins in this batch, but I will from now on just to eliminate any problems.

Thank you for the compliment that means alot. :mrgreen:

 

[Barren Realms 007]

Incinerate the powder to red heat. Be cautious of the fumes.

After incineration try a small sample in HCl again and see if you get a reaction. If not try the procedure I posted above on a separate small sample.

I agree with Lefty, the solution looks like it contains some iron.

Any details on how you arrived at the powder? What color changes did you see in the original solution and powder?

Steve

I just spent 45 min writing a detailed brief on what I had done and the color changes like you had asked. I tried at the end to upload a small film I took of the first HCL bath. The system seemed to crash and sent me back to me replying to Lefty's message. This small film showed the solution setteling and you could see the top of the solution that the HCL was fairly clean with not much color change. I will edit this message tomorrow and write the breif again.

Should I continue to wash and siphon the gold laden material in my coffee pot till I get the stuff to settle out?
Shouldn't an 8 hour set time be enough to get this to settle out?
Is the Ammonia so hard to wash out?

 

[Harold_V]

I must admit, your washing is commendable.

Serious overkill! I'm all for good washing and rinsing, but you reach a point of diminishing, or no return.

The point of doing the HCl wash in this type of material is to insure good filtration. I wouldn't be concerned about a wash with ammonium hydroxide, especially if the source of the material didn't include any silver.

Having spoken my piece, I have to admit, if a gold of high quality is the target, you'll never be sorry for too much washing. I am a firm believer in the idea that garbage being carried through a process is going to show up in the final product. It's just a matter of how much you're comfortable in living with.

Harold

 

[Barren Realms 007]

I must admit, your washing is commendable.

Serious overkill! I'm all for good washing and rinsing, but you reach a point of diminishing, or no return.

The point of doing the HCl wash in this type of material is to insure good filtration. I wouldn't be concerned about a wash with ammonium hydroxide, especially if the source of the material didn't include any silver.

Having spoken my piece, I have to admit, if a gold of high quality is the target, you'll never be sorry for too much washing. I am a firm believer in the idea that garbage being carried through a process is going to show up in the final product. It's just a matter of how much you're comfortable in living with.

Harold

Thanks Harold. Why do you feel this was overkill. I did as has been instructed here except for the 2nd HCL wash but I had a little bit of tin left in my mix I felt.

When I processed the original AP material I took my (pins) solution from the crock pot diluted it with water and let all the solids settle I had some silver cloride develope because I had done this with tap water. That was why I washed the way I did.

I felt there was possibly some silver in the mix and that was why I washed with the ammonia. I was trying to make sure I eliminated all contaminants.

Unless there is another white fine product that forms when tap water is induced into your solution.

 

[lazersteve]

Unless there is another white fine product that forms when tap water is induced into your solution.

With AP, copper I chloride saturation is indicated by a white cloud when water is added to the dark colored AP solution. Copper I chloride is soluble in straight ~32% HCl.

Steve

 

[Barren Realms 007]

Here is a link to the first HCL washing I did on one of my batches in this group.
http://www.youtube.com/watch?v=-vK5t-wBMTg

This batch in the clip was from pins still in connectors done in HCL/peroxide. After the HCL wash I tested the solution and got a slight reaction like the one shown on the filter paper it showed positive for PM's. I applied SMB to this batch of HCL and dropped a very small amount of gold after it had set for 2 days. This was why I chose the washing process I did.

Ok I have 3 batches listed
1. Pins in crock pot done in HCL only.
2. Pins in connectors done in HCL/peroxide(couldn't pull the pins out of these connectors)
3. Fingers (1/2 a small baggie say 4-6 oz.)

Group 1 & 2 were combined after 1st HCL wash and water wash because they were same items and I had made sure there was no more possability of loss from the reaction with left over peroxide.

Steve here are the colors that you asked about thru the diffrent cycles.

1st round of water wash
1. Gold floating around(as seen in video above)
2. Blackish brown powdery substance
3. Whitish percipitant( this I presume to be silver cloride)
4. Very fine brownishr on the top layer
5. Slight greenish copper color (this I assume might be a form of Copper)
6. Tin floating around
(Aproximatly combined voulme in coffe pots aprox. 4 cups after setteling)

1st round HCL Wash
1. Gold floating around(as seen in video above)
2. Blackish brown powdery substance
3. Whitish percipitant( this I presume to be silver cloride)
4. Very fine brownish layer on the top layer
5. Slight greenish copper color
6. No more tin floating.

(Aproximate combined volume after this process in coffee pots 3.5 cups after setteling)

Water wash
1. Gold floating around
2. Blackish brown powdery substance
3. Whitish percipitant
4. Very fine brownish/black layer on the top layer
5. Smell of lead boiling.

(Apprimate combined volume after setteling 3 cups)

I did a 2nd HCL wash just to make sure I didn't miss anything in the first round, just because all of you preach purity.

2nd HCL wash
1. Gold floating around
2. Blackish brown powdery substance
3. Whitish percipitant( this has slowly dissapeared, color change I assume?)
4. Very fine brownish powder on the top layer
(No change in volume settled)

(Batches ((1,2) &3) were mixed together at this point)

Ammonia wash
1. Gold floating around
2. Brownish powdery substance
3. Slight bit of white still left
(Approimate volume of settled material 2 cups with lots of material floating in coffee pot as seen in first picture of this thread.)

 

[Barren Realms 007]

Unless there is another white fine product that forms when tap water is induced into your solution.

With AP, copper I chloride saturation is indicated by a white cloud when water is added to the dark colored AP solution. Copper I chloride is soluble in straight ~32% HCl.

Steve

You answered this while I was writing the post over that was what I was meaning by copper cupric I, I was wrong and will change the post thanks for that.

I read your post again and my above statement is incorrect I will do a search and correct this.
But to answer this perticular statement yes I did see the white cloud you are referring to in the saturated solution of the pins in the crock pot (no peroxide added just HCL, this would be batch #1)

 

[shyknee]

Barren Realms 007
from your last two post what i understand is that you have only dissolved base metals
your gold is visible and sparking in this washed down solution
question for you is have you dissoved the gold with hcl and clorox then precipitated with sodium metabisulfite (SMB)



your washing is premature .wash after you have precipitated your gold powder


follow lazersteve's instructions to the "t" for succes (most would say to read hoke's book again untill you understand)

 

[Barren Realms 007]

i

Barren Realms 007
from your last two post what i understand is that you have only dissolved base metals
your gold is visible and sparking in this washed down solution
question for you is have you dissoved the gold with hcl and clorox then precipitated with sodium metabisulfite (SMB)



your washing is premature .wash after you have precipitated your gold powder


follow lazersteve's instructions to the "t" for succes (most would say to read hoke's book again untill you understand)

Sky the video shows the gold flakes and all after I had stirred it, this was the 1st HCL washe . The gold you see in the video is still in flake form it has not been disloved in HCL/clorox.
The only thing that has been put in HCL/clorox is what was filtered out from the water wash trying to flush the ammonia out, this is what was in the picture in the 1st post of this thread.

 

[shyknee]

yes
the hcl -clorox needs to have the gold precipitated with SMB
have you done this



the filter is from what ? the beaker on the right or the orange hcl-clorox

 

[Barren Realms 007]

yes
the hcl -clorox needs to have the gold precipitated with SMB
have you done this



the filter is from what ? the beaker on the right or the orange hcl-clorox

I haven't dropped the gold in the HCL/clorox solution yet but I will be shortly.

The filter is from the orange solution on the right.

 

[shyknee]

i saw the video

from this point 1:let settle
2:decant liquid off the top of the settled powders and sluge
3:add hcl-clorox to dissolve values add clorox in small increments and stir untill all is in solution
4:add water 3:1 in volume and let settle (a white powder may or may not form on the bottem)
5:decante liquid off of this powder or fillter well into a clean glass container
6:add SMB to precipitate the gold into a fine powder (this is what you should be washing )
7:for cleaner gold redo step 3 to 6 then dry and melt your powder