I had a bunch of gold filled jewelry which i tried to refine and recoop costs of investment.
I watched many videos,and read up on subject quite a bit,and I dissolved base metals using Hcl,and Nitric leaving gold foils behind to further process with aqua regia,and drop with Smb. But every time i tried dropping gold, I could not get it to drop. So I put my failed drop solution in to a bucket,thinking when i learned more,I would be able to recover it still. Well after many trial and errors,and failed attempts getting gold to drop, I started accumulating quite a bit of aqua regia and before I knew it i was near a whole 5 gallons of AR.
Meanwhile I read about the process in Hokes book like i was advised to do.
So with more jewelry still to process, I realized the large amount of AR i accumulated was getting to be too much,and after reading many times it is best to process all acids as you go, I decided I was not going to attempt to process anymore gold recovery until I dealt with my accumulated acids.
So i started the pain staking process of evaporating off excess nitric from the 5 gallons of AR i had, and have come to a point where I am unsure of what to do.
I finally got majority of all the AR and excess nitric evaporated after about 2wks or so of time and slow evaporation using 2 slow cookers,and a large evaporation type dish.
Looking back now, I am not sure if it was a mistake to continuously just keep adding acids to the pots as they lost volume from evap.But it is what I did.
When it was on the heat and evaporating, I noticed it seemed as if salts were trying to start to form.
I added some Hcl,and it bubbled and fizzed rapidly,and after some further evaporation I added Hcl again,and got same reaction,Upon doing this 2x, when i tried adding Hcl a 3rd time, it did not bubble or fizz.
But i did notice it seemed to start developing some type of salts or crystals and adding some more HCL had no effect on them.
So i turned off heat after it got to a syrup type consistency that looked similar to cream mixed with honey, a slightly brownish tan color with cream colored streaks,but none the less it was def a syrup type consistency,like warm honey or hot Caro syrup type deal.
These are some pics of it,and I am not sure how to go about processing this at this point in time.
I do not recall seeing in Hokes book anything about this type of stuff after evap of excess nitric from AR.
I did try taking a small sample,and added Hot boiling water,which the salts or crystals dissolved completely.
I tried adding Hcl,and they did not dissolve all the way, they dissolved some,but only partially.Even Hot Hcl,there was still white salts standing in bottom.
I tried to take many pics to show the different effects of hot water,hot Hcl,and cooled solution with brown top,and so on.
After this long tiresome process of evaporating all this Ar down to this point, I want to make sure whatever I do, I am not making anymore unnecessary waste products I dont need to,and also not making more work for myself and wastes.
A side Note, I did not add sulphuric acid to evap process,which am thinking would probable been good idea now, But I did not at the time.
I was careful watching for items that may been tin,since tin seems to melt fairly quickly at lower temps,and I normally can see it when heating item to redness if it is tin based.(not to say it cant be in the mix,but if there is then should be fairly minute amount)
I know there is quite bit gold in here somewhere. And It was all mainly just foils dissolved in all the AR solution I have evaporated down to this point.
tried to post the pics,please let me know if they dont show up.
Thank you in advance for help,and advice.
Edditted Post
Sorry for mix up, I know how vital it is to be accurate with chemicals and solutions using in any process,and I realized I made mistake in beginning of my post describing dissolving base metals with Hcl,and nitric.
But I used dilute nitric to dissolve all base metals from the gold filled jewelry.
Then Only foils went in to the AR solution,which I only used very small amounts of nitric with the Hcl to dissolve foils,but still had issues and could not get gold to drop using smb.
So with small experiments trying to get AR to drop using Smb, I still had no luck,and always tried adding more water here and there to the mix to see if gold would drop,but it never did,so it is how i ended up with so much AR to begin with and is what i evaporated down to what i have now.(excess of H2O and SMB)
After reading book of Hoke, i realized it is best to evap all down to syrup like consistency,which is what i did,and where I am at now.
But it seems it is saturated with a white and brown chlorides,which dissolve with hot boil water, but not with hot Hcl.(partially dissolves with hot Hcl)
Hokes book however does not mention the type of situation i have now, where once evap excess nitric, Now there is Alot of precipitate remaining in cooled dish,(temps were very cold last night) I am sure that there is Alot of Smb in the mix from trying to get gold to drop.
This AR solution has only had foils dissolved in it along with SMB,(lol I know there is alot of Au in the mix,however I cant say exactly how much i expect to recover,only that it should be a few decent Oz 3-4 or so )
My notes on weights of processed items have been mistakenly discarded by another,making it impossible for me to now know exact amounts of jewelry and foil weights processed in my solutions.(I still can't believe there gone but they are)
I have a friend who will help me get some pics up soon.
Thank you
I watched many videos,and read up on subject quite a bit,and I dissolved base metals using Hcl,and Nitric leaving gold foils behind to further process with aqua regia,and drop with Smb. But every time i tried dropping gold, I could not get it to drop. So I put my failed drop solution in to a bucket,thinking when i learned more,I would be able to recover it still. Well after many trial and errors,and failed attempts getting gold to drop, I started accumulating quite a bit of aqua regia and before I knew it i was near a whole 5 gallons of AR.
Meanwhile I read about the process in Hokes book like i was advised to do.
So with more jewelry still to process, I realized the large amount of AR i accumulated was getting to be too much,and after reading many times it is best to process all acids as you go, I decided I was not going to attempt to process anymore gold recovery until I dealt with my accumulated acids.
So i started the pain staking process of evaporating off excess nitric from the 5 gallons of AR i had, and have come to a point where I am unsure of what to do.
I finally got majority of all the AR and excess nitric evaporated after about 2wks or so of time and slow evaporation using 2 slow cookers,and a large evaporation type dish.
Looking back now, I am not sure if it was a mistake to continuously just keep adding acids to the pots as they lost volume from evap.But it is what I did.
When it was on the heat and evaporating, I noticed it seemed as if salts were trying to start to form.
I added some Hcl,and it bubbled and fizzed rapidly,and after some further evaporation I added Hcl again,and got same reaction,Upon doing this 2x, when i tried adding Hcl a 3rd time, it did not bubble or fizz.
But i did notice it seemed to start developing some type of salts or crystals and adding some more HCL had no effect on them.
So i turned off heat after it got to a syrup type consistency that looked similar to cream mixed with honey, a slightly brownish tan color with cream colored streaks,but none the less it was def a syrup type consistency,like warm honey or hot Caro syrup type deal.
These are some pics of it,and I am not sure how to go about processing this at this point in time.
I do not recall seeing in Hokes book anything about this type of stuff after evap of excess nitric from AR.
I did try taking a small sample,and added Hot boiling water,which the salts or crystals dissolved completely.
I tried adding Hcl,and they did not dissolve all the way, they dissolved some,but only partially.Even Hot Hcl,there was still white salts standing in bottom.
I tried to take many pics to show the different effects of hot water,hot Hcl,and cooled solution with brown top,and so on.
After this long tiresome process of evaporating all this Ar down to this point, I want to make sure whatever I do, I am not making anymore unnecessary waste products I dont need to,and also not making more work for myself and wastes.
A side Note, I did not add sulphuric acid to evap process,which am thinking would probable been good idea now, But I did not at the time.
I was careful watching for items that may been tin,since tin seems to melt fairly quickly at lower temps,and I normally can see it when heating item to redness if it is tin based.(not to say it cant be in the mix,but if there is then should be fairly minute amount)
I know there is quite bit gold in here somewhere. And It was all mainly just foils dissolved in all the AR solution I have evaporated down to this point.
tried to post the pics,please let me know if they dont show up.
Thank you in advance for help,and advice.
Edditted Post
Sorry for mix up, I know how vital it is to be accurate with chemicals and solutions using in any process,and I realized I made mistake in beginning of my post describing dissolving base metals with Hcl,and nitric.
But I used dilute nitric to dissolve all base metals from the gold filled jewelry.
Then Only foils went in to the AR solution,which I only used very small amounts of nitric with the Hcl to dissolve foils,but still had issues and could not get gold to drop using smb.
So with small experiments trying to get AR to drop using Smb, I still had no luck,and always tried adding more water here and there to the mix to see if gold would drop,but it never did,so it is how i ended up with so much AR to begin with and is what i evaporated down to what i have now.(excess of H2O and SMB)
After reading book of Hoke, i realized it is best to evap all down to syrup like consistency,which is what i did,and where I am at now.
But it seems it is saturated with a white and brown chlorides,which dissolve with hot boil water, but not with hot Hcl.(partially dissolves with hot Hcl)
Hokes book however does not mention the type of situation i have now, where once evap excess nitric, Now there is Alot of precipitate remaining in cooled dish,(temps were very cold last night) I am sure that there is Alot of Smb in the mix from trying to get gold to drop.
This AR solution has only had foils dissolved in it along with SMB,(lol I know there is alot of Au in the mix,however I cant say exactly how much i expect to recover,only that it should be a few decent Oz 3-4 or so )
My notes on weights of processed items have been mistakenly discarded by another,making it impossible for me to now know exact amounts of jewelry and foil weights processed in my solutions.(I still can't believe there gone but they are)
I have a friend who will help me get some pics up soon.
Thank you