I was refining 14k gold: I refined down with aqua regia. I then added urea and "by mistake-confusion" baking soda. I then added SMB and no gold came out. I now have emerald green with no gold precipitating out. Can anyone please help me, this is my last project and there is much gold in the solution?
I messed up added Baking soda and gold won't precipitate
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patnor1011
Well-known member
Did you inquart gold before AR? How much of gold, AR and baking soda was involved, more details are needed. Hypothetical answer without more details might be to add more acid to solution and use copper to cement gold out. Incinerate cemented gold and start all over again.
Have you tested with stannous to see if you have any gold left in solution?
Göran
Göran
patnor1011
Well-known member
When it will be saturated with copper decant and test decanted liquid with stannous to be sure if there is no gold present. Go in more details in describing what you did along with numbers.
So how much of what did you dissolved in what volumes of what exactly. Why urea and how much of baking powder.
So how much of what did you dissolved in what volumes of what exactly. Why urea and how much of baking powder.
I was dissolving 2 oz of 14k gold popcorn beads: I put gold in about 5 oz of 32% HCL(muriatic acid). I then added Nitric acid (69%)slowly to about 7 oz over time on hotplate(coffee machine heater). I added 1 oz distilled water near the end because not all of the gold had dissolved.
I then added urea and it boiled over and I know I had lost some, so I poured part(about 3/4) in a glass and left the rest in the coffee pot. I then added more urea in the glass and the urea beads were still there, so I added baking soda(was confused etc.) Pinch by pinch the baking soda would still fizz(about 1 1/2 table spoon). I added some to the coffee pot as well(half teaspoon). I then added enough SMB to the 3/4 glass to get the gold out(about 20g) and it and the beads of urea sank to the bottom and the emerald liquid formed crystals. The coffee pot crystallized as well.
Today I decanted the glass jar(leaving the crystals inside it), put some in a glass jar and set some aside. I added HCL to the small glass and put copper strip in and got coffee color with tan sludge on bottom. I just added some HCL to the crystals-glass and decanted out the crystals. I just put copper in that and it fizzed and it appears to have some sludge too. I just now put copper in the stuff I set aside(adding just a little HCL) and it appears to be sedimentation. The coffee pot with the scraps that didn't dissolve and has crystal in it, I just am keeping aside for now.
I know I have a big mess. If I just skipped the baking soda, I would be melting 24k today. This is my second attempt, and likely my last attempt at refining 14k scrap( the 14k was a bad mix/color for my gold working). I refined 28g of 14k and got 13g of 24K and I thought my mistake was not neutralizing the nitric acid enough(hence the baking soda-I mistakenly saw online- it was a misread). Thanks for your help because it looks that I haven't lost all of the gold.
I then added urea and it boiled over and I know I had lost some, so I poured part(about 3/4) in a glass and left the rest in the coffee pot. I then added more urea in the glass and the urea beads were still there, so I added baking soda(was confused etc.) Pinch by pinch the baking soda would still fizz(about 1 1/2 table spoon). I added some to the coffee pot as well(half teaspoon). I then added enough SMB to the 3/4 glass to get the gold out(about 20g) and it and the beads of urea sank to the bottom and the emerald liquid formed crystals. The coffee pot crystallized as well.
Today I decanted the glass jar(leaving the crystals inside it), put some in a glass jar and set some aside. I added HCL to the small glass and put copper strip in and got coffee color with tan sludge on bottom. I just added some HCL to the crystals-glass and decanted out the crystals. I just put copper in that and it fizzed and it appears to have some sludge too. I just now put copper in the stuff I set aside(adding just a little HCL) and it appears to be sedimentation. The coffee pot with the scraps that didn't dissolve and has crystal in it, I just am keeping aside for now.
I know I have a big mess. If I just skipped the baking soda, I would be melting 24k today. This is my second attempt, and likely my last attempt at refining 14k scrap( the 14k was a bad mix/color for my gold working). I refined 28g of 14k and got 13g of 24K and I thought my mistake was not neutralizing the nitric acid enough(hence the baking soda-I mistakenly saw online- it was a misread). Thanks for your help because it looks that I haven't lost all of the gold.
When you're finished completing the mess you made, do yourself a favor and MARK/LABEL your containers. Baking Soda, SMB, Borax, Urea, Sodium Hydroxide look very similar and you can easily add something you're not supposed to add.
With the above said, do yourself another favor and study more because if you're refining at the level you're confident at, then you should already know that you do not need to use Urea. I still have a 5 lb bag from 3 years ago. I used it once, and after my learning experience with refining got better, I learned that it's not needed. The main thing you need to know is that you have to add nitric acid slowly, and in increments, just enough to do the job. If you do that, then you won't need urea.
Also, when you have made your AR and it stops working, or even if you know your items are dissolved, do NOT add water to the solution. If you are not completed in dissolving your material, then all you would really need to add is some more nitric acid in small increments, and make sure you add it to the hot plate. The only time I would use water (rarely) to my finished solution is if it's thick like syrup or if I want to make sure I thin out the solution to drop the gold with SMB. But, like I said, that's very rare I would even consider it.
Your baking soda is only needed in case of accidental spills and breaches and AFTER you've dropped all your gold and tested it with stannous to make sure no gold is detected. Other than that, keep that baking soda away from your refining powders you're using.
But when it's all said and done, you MUST LABEL your containers because what you did you could have poured the wrong powder in your solution and you could have done something more deadly than what you're already doing.
Your best bet would be to add copper to the solution and let it sit there for a few days. Some processes aren't a 1 day process, and especially if you've made a mistake during the process.
Keep reading the forum and I hope you've downloaded and read Hoke's book.
Be safe.
Added Info.... I forgot to mention that if this will be your last attempt at refining 14K, then you need to quit while you're ahead. The only way you'll learn is to do, and "WHEN" you make mistakes, you have to LEARN from them, and then keep moving on. This is no get-rich quick scheme when it comes to refining. You must have knowledge and patience in order to do this to a satisfactory point. ask every single person here and I'll tell you right now they'll ALL tell you the mistakes they made and how many times of the same and (or) similar mistakes. It happens. Yet, the point is that you learn from it and move forward to better your knowledge in refining. Just last week I made a mistake by not folding some copper mesh in my sulfuric cell and wasted most of my copper. Folding was something I always did, but for some reason this time, I forgot. So, it happens, and even to some of us that have refined for a few years.
With the above said, do yourself another favor and study more because if you're refining at the level you're confident at, then you should already know that you do not need to use Urea. I still have a 5 lb bag from 3 years ago. I used it once, and after my learning experience with refining got better, I learned that it's not needed. The main thing you need to know is that you have to add nitric acid slowly, and in increments, just enough to do the job. If you do that, then you won't need urea.
Also, when you have made your AR and it stops working, or even if you know your items are dissolved, do NOT add water to the solution. If you are not completed in dissolving your material, then all you would really need to add is some more nitric acid in small increments, and make sure you add it to the hot plate. The only time I would use water (rarely) to my finished solution is if it's thick like syrup or if I want to make sure I thin out the solution to drop the gold with SMB. But, like I said, that's very rare I would even consider it.
Your baking soda is only needed in case of accidental spills and breaches and AFTER you've dropped all your gold and tested it with stannous to make sure no gold is detected. Other than that, keep that baking soda away from your refining powders you're using.
But when it's all said and done, you MUST LABEL your containers because what you did you could have poured the wrong powder in your solution and you could have done something more deadly than what you're already doing.
Your best bet would be to add copper to the solution and let it sit there for a few days. Some processes aren't a 1 day process, and especially if you've made a mistake during the process.
Keep reading the forum and I hope you've downloaded and read Hoke's book.
Be safe.
Added Info.... I forgot to mention that if this will be your last attempt at refining 14K, then you need to quit while you're ahead. The only way you'll learn is to do, and "WHEN" you make mistakes, you have to LEARN from them, and then keep moving on. This is no get-rich quick scheme when it comes to refining. You must have knowledge and patience in order to do this to a satisfactory point. ask every single person here and I'll tell you right now they'll ALL tell you the mistakes they made and how many times of the same and (or) similar mistakes. It happens. Yet, the point is that you learn from it and move forward to better your knowledge in refining. Just last week I made a mistake by not folding some copper mesh in my sulfuric cell and wasted most of my copper. Folding was something I always did, but for some reason this time, I forgot. So, it happens, and even to some of us that have refined for a few years.
