Ferrous Sulfate - Did I buy the wrong thing?
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Topher_osAUrus
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Ive used lead tin solder before, worked well enough for my purposes.
Im not much of a measurement man myself...
I just put in some HCl in my dropper, took a few inches of solder and put it in the HCl and gave the bottle a little heat until I saw bubbles forming on the solder. Removed it from heat, let it sit for a few hours. Tested it against my gold standard solution and it showed purple.
If i were to guess, Id probably say I used 30mL of acid, with around 15 to 20g of solder (so there is some undissolved in the bottle still)
Im not much of a measurement man myself...
I just put in some HCl in my dropper, took a few inches of solder and put it in the HCl and gave the bottle a little heat until I saw bubbles forming on the solder. Removed it from heat, let it sit for a few hours. Tested it against my gold standard solution and it showed purple.
If i were to guess, Id probably say I used 30mL of acid, with around 15 to 20g of solder (so there is some undissolved in the bottle still)
How do you know your stannous doesn't work?Assol said:
I have made stannous chloride from everything from pure tin, pewter, solder and a piece of circuit board with solder on it and it worked every time.
- Put tin in a beaker and add some HCl.
- Wait until the reaction stops.
- If all tin is dissolved add more tin, go back to previous step.
- Test against a known gold chloride solution.
Stannous will keep as long as it is protected from oxygen and having a bit of tin in the bottle seems to help.
Warning, if the HCl isn't fully used up it can build up pressure over time when dissolving the tin in a closed bottle... don't ask how I know that. :lol:
Same for ferrous sulfate, keep it from oxygen then there is nothing that could oxidize it. I've got a bottle full of pale blue copperas in solution and I made it eight months ago, it looks just as when I made it.
Göran
I have always used a bottle that looks similar to a a eye dropper bottle but larger and square. The first time I used it everything went great, put my stuff away, no problem. A couple of hours later I went out to my building for something and just as I opened the door I hear a loud POP and the lid went shooting out in the yard, I am just glad it wasn't a screw on cap. :lol:
Thank you for all your suggestions!!
Now:
"get some sulfamic acid, dissolve it in water. Add the aqueous solution to your pregnant mother liquor while it is hot, add it slowly, in small increments, until no more effervescence occurs. Stir it a few good stirs to release the bubbles and you're good to precipitate.
Of course, if you didnt add sulfuric before doing this, a filtration before precipitation may be required to remove lead sulfate."
I heat my solution, half liter, first i added some Sulfuric and after some sulfamic solution untill no effervescence.
I made a solution with feSo4 7H2o and water,adding some HCl before mixing with "the new acqua regia" at room temperature.(in the BOOK, they say to add hcl until the solution cames green... my was yellow/ light green). Tomorrow I'll se the result.
probably Was SMB better?
first of doing all, i tested my acqua regia with the new stannous chloride... it was positive...brown!
do you have any observation about what i have done?
Grazie
alex
Now:
"get some sulfamic acid, dissolve it in water. Add the aqueous solution to your pregnant mother liquor while it is hot, add it slowly, in small increments, until no more effervescence occurs. Stir it a few good stirs to release the bubbles and you're good to precipitate.
Of course, if you didnt add sulfuric before doing this, a filtration before precipitation may be required to remove lead sulfate."
I heat my solution, half liter, first i added some Sulfuric and after some sulfamic solution untill no effervescence.
I made a solution with feSo4 7H2o and water,adding some HCl before mixing with "the new acqua regia" at room temperature.(in the BOOK, they say to add hcl until the solution cames green... my was yellow/ light green). Tomorrow I'll se the result.
probably Was SMB better?
first of doing all, i tested my acqua regia with the new stannous chloride... it was positive...brown!
do you have any observation about what i have done?
Grazie
alex
Topher_osAUrus
Well-known member
Stannous test for gold should be light purple to black for gold. (Dependent on concentration)Assol said:
I really dont have any astute advice for you beyond these points above, it seems you are just being cautious(not a bad thing, at all) but, unless you dump it down the drain, its next to impossible to lose gold. Just follow proper procedures as best you can, and if something unexpected happens, hopefully you have studied enough to know what is causing the issue. If not, come back, lay out everything you did step by step, and any observations you had, (pictures help alot), and the good people of the forum here will help you
Topher_osAUrus
Well-known member
Since your first reply in this thread mentioned "e water" (whatever that is), I'm going to guess you dissolved a couple cell phone boards in AR and expect to have 10ozt precipitating out. (It's okay...common mistake)
But, I must repeat myself a bit here
But, I must repeat myself a bit here
Topher_osAUrus said:
Topher_osAUrus
Well-known member
Assol said:
Without the step by step, (on everything from material, to pretreatments, to when you tested, etc... Every detail is important), it's all just conjecture.
Your photo though, doesnt look like a pregnant solution.
So, if I were to guess. Id say
-what little gold was in there has been precipitated, and its just too small to see (needs to settle overnight or longer)
-there was no gold to begin with, possibly from cementing onto base metals
(Again. Just a guess, as pretty much no information has been given)
What was the feedstock?
How did you treat it?
Did you remove all base metal?
-how?
If not, and you just did AR
-how much solid stuff remained after dissolution?
Did you save the filter?
Did you test after filtering, or before?
All these questions, plus a few dozen more are pertinent to your problem, but I will wait to ask more until you do the walkthrough of your process.
Hi! Tanks for your help...
Starting... it's firtst time that i workwith this material.
Are more than 10 years that i work with querries toextract gold from the sands.
This is a little part of my job like technic in concrete, cement and aggregates.
Anyway i used quite the same process that i normally use.
1) Nitric Acid
2)Filtering
3) the filtrated in AR
4)new filtration to remove extra material
5)precipitation
6) filtration of mud.
I try to adopt this lay out knowing that in this case i could have excessive nitric acid to denox. i worked 25 kg of the material in 2 liters of nitric and 15 of water at room temprtature. They stay in a bath for 2 days untill the result of the picture
Starting... it's firtst time that i workwith this material.
Are more than 10 years that i work with querries toextract gold from the sands.
This is a little part of my job like technic in concrete, cement and aggregates.
Anyway i used quite the same process that i normally use.
1) Nitric Acid
2)Filtering
3) the filtrated in AR
4)new filtration to remove extra material
5)precipitation
6) filtration of mud.
I try to adopt this lay out knowing that in this case i could have excessive nitric acid to denox. i worked 25 kg of the material in 2 liters of nitric and 15 of water at room temprtature. They stay in a bath for 2 days untill the result of the picture
Attachments
I don't and I didn't know how much material and which type of material could be recover.
i supposed by the selling price ( 5 €/kg) that at minimun it could have 0,2/0,3 grams/kg of gold, excluding by myself other material, except base material.
After thr bath of HNO3, I had not more less than 100 grams of filtered material( gold, dirt, plastic).
i supposed by the selling price ( 5 €/kg) that at minimun it could have 0,2/0,3 grams/kg of gold, excluding by myself other material, except base material.
After thr bath of HNO3, I had not more less than 100 grams of filtered material( gold, dirt, plastic).
After i used AR , 0,8 liter( 1 HNO3 - 3 hCl) at room temperature.
Knowing that i was using much AR and too much nitric, i mixed 200 g of urea in solution with 500 cc of hot water (50 celsius) .
i only used 450 cc of urea's solution step by step untill the AR Stopped to foam... so i think to have add 180 grams of urea.
The next day i found many crystals like in the picture.
Knowing that i was using much AR and too much nitric, i mixed 200 g of urea in solution with 500 cc of hot water (50 celsius) .
i only used 450 cc of urea's solution step by step untill the AR Stopped to foam... so i think to have add 180 grams of urea.
The next day i found many crystals like in the picture.
Attachments
So I heated again the AR, adding some more Chloridric.
The stannous test was positive.
i decided to add 3 littel tabs of urea to see if therewas foam... no foam, i tought to have " neutralized the AR.
i started to Add SMB, I had only 500 grams of it but i tought it could be to much for this operation.. Nooo! 500 grams were not sufficient and the shop was closed. 2 days later I bought Smb and ferrous Sulfate. Heating the AR, i continued to add Smb... untill frizzing.the they after I didn't find a precipitated, just some dirt on the bottom.
The stannous test was positive.
i decided to add 3 littel tabs of urea to see if therewas foam... no foam, i tought to have " neutralized the AR.
i started to Add SMB, I had only 500 grams of it but i tought it could be to much for this operation.. Nooo! 500 grams were not sufficient and the shop was closed. 2 days later I bought Smb and ferrous Sulfate. Heating the AR, i continued to add Smb... untill frizzing.the they after I didn't find a precipitated, just some dirt on the bottom.
Attachments
After a great help from the forum,i filtered all. In the filter probably there is same brown mud, probably 2/3 grams....
I have heated my solution, only half liter to test it, first i added some Sulfuric (8 ml) and after some sulfamic solution untill no effervescence. It was necessary add 40 grams of sulfamic crystals.
I made a solution with Ferrous sulfate and water,adding some HCl before mixing with "the new acqua regia" at room temperature.(in the BOOK, they say to add hcl until the solution cames green... my was yellow).
The result is in the Picture.
That's all!!
Thanks
I have heated my solution, only half liter to test it, first i added some Sulfuric (8 ml) and after some sulfamic solution untill no effervescence. It was necessary add 40 grams of sulfamic crystals.
I made a solution with Ferrous sulfate and water,adding some HCl before mixing with "the new acqua regia" at room temperature.(in the BOOK, they say to add hcl until the solution cames green... my was yellow).
The result is in the Picture.
That's all!!
Thanks
Attachments
Topher_osAUrus
Well-known member
Assol said:
That top picture looks like you added stannous chloride to the entire solution?! Did you?
If yes, there will be nothing to precipitate, as its been reduced already. Take a small sample of the solution in a spot plate or on a filter paper, and add a small amount of the test solution. Never, ever, add stannous to your solution's entirety.
Dont use urea, use sulfamic. But, you shouldnt have to use anywhere close to that much of it. Maybe a few grams. Why, you ask? Because using small controlled additions of nitric, and allowing it to work until its exhausted before another addition is the smartest move you can make.
500 grams of smb could precipitate over a troy lb of gold. I highly doubt there was that much in there. Now there is copious amounts of urea, smb, and metal salts in solution. What I would do-
Get a 5 gallon bucket, get a bunch,of copper tubing or bus bar and throw it in the bucket, dump in your solution mess, and any precious metals dissolved in it, will be displaced by the copper going into solution. It will be the black sludge on the bottom pf the container some time later.
Another huge mistake is-
Dont estimate gold value by sellers price.
If you did, and bought pentium pro's to refine... You would be incredibly disheartened when you only got .35g of gold off each one, and not the 1g+ that the internet portrays them to have.
Gold plating is thin. Extremely thin. Something like 30 to 40 microinches for contact plating. And 5 microinches for general board traces.
A lot of times, when using acid, the gold doesnt cover the cost.
Im sorry, I know there is more points I missed, but it has been a very hectic past 25 hours, I will go over the details again tomorrow morning if time allows it.
Since the facts are still a bit of sketchy I'll make quite some assumptions. Maybe something has been said further up in the thread and I missed it... but here is my explanation.
1. Starting material was 12 kg of circuit boards with ENIG. (Guessing, based on the picture) In this case I would expect less than 1g/kg and with only part of the board covered by gold even less. Maybe around 0.1g per kilo of starting material. So around 1g of gold.
2. The copper on the boards were dissolved in nitric, leaving 100g of solder mask mixed in with the 1g of gold.
3. 0.8 liter of AR was way too much needed. About 200 times more than a gram of gold would require. Correct way to do it would have been to cover the material in HCl and add just a few ml of nitric and heat it to drive the dissolution to completion.
4. That huge excess of nitric acid took a huge amount of urea. That is why you see a lot of crystals. Evaporation would have been better as that isn't adding material and diluting your gold solution.
5. A gram of SMB precipitates a gram of gold, roughly. 500g SMB is 500 times too much! It probably used up any acid still left in solution so now you have an SMB-solution. The dirt on the bottom is probably your gold, the 2/3 of a gram filtered off.
After this you are chasing ghosts. There probably isn't any gold left in solution and any positive tests of stannous is probably only false positives (brown instead of purple) because of the SMB still in solution.
Okay, that is my guess on the events transpired.
And as has been said before, just because the seller thought there was a lot of gold in the material doesn't mean that he is right. Any pictures of the starting material?
By the way, I have refined gold for 10 years now and I'm just getting close to using up my first 500g of SMB that I bought when starting my new hobby. So far it has given me close to 70 grams of gold and most of it refined three times.
Göran
1. Starting material was 12 kg of circuit boards with ENIG. (Guessing, based on the picture) In this case I would expect less than 1g/kg and with only part of the board covered by gold even less. Maybe around 0.1g per kilo of starting material. So around 1g of gold.
2. The copper on the boards were dissolved in nitric, leaving 100g of solder mask mixed in with the 1g of gold.
3. 0.8 liter of AR was way too much needed. About 200 times more than a gram of gold would require. Correct way to do it would have been to cover the material in HCl and add just a few ml of nitric and heat it to drive the dissolution to completion.
4. That huge excess of nitric acid took a huge amount of urea. That is why you see a lot of crystals. Evaporation would have been better as that isn't adding material and diluting your gold solution.
5. A gram of SMB precipitates a gram of gold, roughly. 500g SMB is 500 times too much! It probably used up any acid still left in solution so now you have an SMB-solution. The dirt on the bottom is probably your gold, the 2/3 of a gram filtered off.
After this you are chasing ghosts. There probably isn't any gold left in solution and any positive tests of stannous is probably only false positives (brown instead of purple) because of the SMB still in solution.
Okay, that is my guess on the events transpired.
And as has been said before, just because the seller thought there was a lot of gold in the material doesn't mean that he is right. Any pictures of the starting material?
By the way, I have refined gold for 10 years now and I'm just getting close to using up my first 500g of SMB that I bought when starting my new hobby. So far it has given me close to 70 grams of gold and most of it refined three times.
Göran
