# Ferrous Sulfate - Did I buy the wrong thing?



## snoman701 (Feb 4, 2017)

https://www.amazon.com/gp/product/B007ODUI76/ref=oh_aui_detailpage_o03_s01?ie=UTF8&psc=1

That's what I bought. Now that I've researched it a little, it's very clearly aged, which would explain why it wouldn't work for me.

I'm trying to determine if i should return it as defective since it's oxidized, or if it fits within the description. 

It is not green crystals, but brownish white with the occasional speck of green.


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## Topher_osAUrus (Feb 4, 2017)

How did you prepare it before using it to precipitate?

When I had oxidized copperas, i recrystallized it.. Kind of a pain, but I had the time to do it.


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## snoman701 (Feb 4, 2017)

Dissolve in distilled water and add just a small amount of HCl.


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## Topher_osAUrus (Feb 4, 2017)

snoman701 said:


> Dissolve in distilled water and add just a small amount of HCl.



Did it turn vibrant green?
Did you filter it before adding it?(to the gold solution)

Was the solution denoxxed?
What ratio of copperas to gold (to be dropped) did you use?

What happened after adding it?


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## snoman701 (Feb 4, 2017)

No green.

Yes filtered.

Yes denoxx, or at least I thought it was....

I don't remember my ratio, but do remember calculating it based upon Hoke, which was a lb coppers to dwt conversion. 

Nothing happened. lol


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## Topher_osAUrus (Feb 4, 2017)

Yeah, it should have turned green upon the addition of HCl.

I'm not sure if that caused your problem, but it probably didn't help any.


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## Iggy-poo (Feb 4, 2017)

8) http://en.wikipedia.org/wiki/Iron(III)_sulfate


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## snoman701 (Feb 4, 2017)

Topher_osAUrus said:


> Yeah, it should have turned green upon the addition of HCl.
> 
> I'm not sure if that caused your problem, but it probably didn't help any.



Probably didn't add enough HCl. After doing some reading, wet low pH storage is recommended.


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## Grelko (Feb 4, 2017)

You're statement about it being "defective since it's oxidized" is valid. (Brownish white)

The Amazon listing says that it's *Hepahydrate*
Edit - The second picture listed looks more white than green, so they may have the "anhydrous" shown there instead. It should look about the same as the picture on the bag itself.

https://en.wikipedia.org/wiki/Iron%28II%29_sulfate

Other names
Ferrous sulfate, Green vitriol, Iron vitriol, Copperas, Melanterite, Szomolnokite

Appearance
White crystals (anhydrous)
White-yellow crystals (monohydrate)
*Blue-green crystals (heptahydrate)* If it's not this color, it went bad.

If it's not close to this color Green It's not Green Vitriol.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=23647&start=30


butcher said:


> Oxidation of air can change the chemistry of the iron salt turning it white or brown which would no longer be good for precipitating or testing for gold in solution.


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## butcher (Feb 4, 2017)

ferrous not ferric.


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## lanfear (Mar 14, 2017)

I have about 2 pounds of green vitrol, but it has brown oxidized speks in it. Will this contaminate my gold drop or will the filtering remove it?


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## snoman701 (Mar 14, 2017)

Given my frustrations of the last three months....discard it. Go buy a bottle of battery acid and follow butchers instructions on preparation and storage. You'll be thankful.


Sent from my iPhone using Tapatalk


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## anachronism (Mar 14, 2017)

Nah just buy the right stuff. Cheap as chips. You want the nice green crystals. 

I add a bit of HCL then dissolve in hot water till the solution is saturated. Allow it to settle for a few minutes and pour it in. You can see the gold drop right out as your solution turns cloudy. You want it to turn dark and stay dark otherwise you have more gold to come out, but of course your stannous tests will provide you a check.

Here's what you need to buy. Available in 25Kg bags, and it's almost wet when it comes. You're going to use a lot of it so don't be buying small bags if you're doing more than a few grammes per year. It keeps well in a plastic container that's sealed. Any good chemical supplier will know what you mean when you ask for it green and crystalline and damp. 

There's really no drama using this stuff lads IF you buy the right thing.  

Edit for reference link - look at the picture. https://sc02.alicdn.com/kf/HTB1Fj27KVXXXXXPXFXXq6xXFXXXo/Ferrous-Sulphate-FeSO4-7H2O-Iron-II-Sulfate.jpg_350x350.jpg

Hope that helps

Jon


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## snoman701 (Mar 14, 2017)

My opinion was just based on my the difficulty of getting it fresh. I thought I was making a mistake somehwere in the process, and my only mistake was the materials I was using to drop the gold. So I always had to cement it out.


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## Assol (Sep 12, 2017)

Hello!
Usually i use a solution of 400g of FeSo4 in 1 liter of e water ( hot).
can I use FeSo4 7H2O?
If yes, how much do i need compared with anydrous?
Thanks


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## goldandsilver123 (Sep 12, 2017)

If it's Ferrous sulfate (FeSO4) => Fe2+ you can use anhydrous or heptahydrate.

151.91 g/mol (anhydrous)
278.02 g/mol (heptahydrate)

You have to use 84% more of the heptahydrate, but it depends if you have excess nitric.


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## Assol (Sep 12, 2017)

Thank you!
So if i use heptaidtate i must use 84% more...
But if i have an excess of HNo3, what can I do?
Grazie


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## Topher_osAUrus (Sep 12, 2017)

Assol said:


> But if i have an excess of HNo3, what can I do?
> Grazie


Remove the excess nitric by slow evaporation to syrup, then addition of a small amount of HCl (best done with a little sulfuric in the solution to prevent crusting, and only enough HCl to get some of the nitrates to convert to chlorides -dont dump in a liter or anything crazy-)
Repeat that agonizingly long process a few times until no brown cloud comes from the HCl addition.

Or

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.


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## Assol (Sep 12, 2017)

Thank you for your help!!!
If I make the solution of sulfamic and water, how long does the solution keep stable? (Days?)
I can propose the same question making the solution of FeSO4...(in my experience I do it every time)...
I dont understand what is appening whit my chemical store... i bought some pure tin (Sn) to make the stannous chloride for the soution test and doesn't work... Any suggestion? 
Grazie!!!!


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## Topher_osAUrus (Sep 12, 2017)

Assol said:


> Thank you for your help!!!
> If I make the solution of sulfamic and water, how long does the solution keep stable? (Days?)
> I can propose the same question making the solution of FeSO4...(in my experience I do it every time)...
> I dont understand what is appening whit my chemical store... i bought some pure tin (Sn) to make the stannous chloride for the soution test and doesn't work... Any suggestion?
> Grazie!!!!



I just buy the jar of crystals (sulfamic), add water, and stir it like a madman, then add pipettes of the saturated sulfamic solution. Ive never had any decomposition problems (that Im aware of), but I dont try to dissolve the pound of crystals with half a cup of water... I just add the water, stir, and add it a few mL at a time. Thats it.

I presume, of the copperas solution is in a sealed container and cannot get air or direct sunlight, it will stay good for awhile. I had some made up for a few weeks before using it, worked fine.

Just buy some solder and use it to make stannous. Cheap and easy. (And readily available everywhere)


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## Assol (Sep 12, 2017)

Ok, solder has 50% of lead!
How can i do with solder? Can you explain?
now i use 2 different metod:
First: 2 grams of tin and 30 cc of HCl
second: 1 gram of tin plus 1 g of stannous chloride, 30 drops of hCL and 25 of water...
Alex


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## Topher_osAUrus (Sep 12, 2017)

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)


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## g_axelsson (Sep 12, 2017)

Assol said:


> Thank you for your help!!!
> If I make the solution of sulfamic and water, how long does the solution keep stable? (Days?)
> I can propose the same question making the solution of FeSO4...(in my experience I do it every time)...
> I dont understand what is appening whit my chemical store... i bought some pure tin (Sn) to make the stannous chloride for the soution test and doesn't work... Any suggestion?
> Grazie!!!!


How do you know your stannous doesn't work?

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


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## Shark (Sep 12, 2017)

> 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:



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:


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## Assol (Sep 13, 2017)

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


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## Topher_osAUrus (Sep 13, 2017)

Assol said:


> 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 aqua regia" at room temperature.(in the BOOK, they say to add hcl until the solution cames green... my was yellow/ light green).
> I would guess that its fine, Ive had a yellowish,
> neonish green tint before. I think all the HCl does is make sure the crap that got oxidized is in the proper valence before precipitating. Of course thats just a guess, as I am no chemist
> ...


Stannous test for gold should be light purple to black for gold. (Dependent on concentration) 

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


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## Assol (Sep 13, 2017)

Ah ah!!!! Sorry I am a littel bit color-blind... but it was dark color!!
Thanks for all... tomorrow I'll post some pictures.
i hope good pictures...

grazie
alex


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## Assol (Sep 14, 2017)

Nothing append!!!
help me!
I see just this!


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## Topher_osAUrus (Sep 14, 2017)

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



Topher_osAUrus said:


> 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


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## Assol (Sep 14, 2017)

Hello!
I understand all you are telling to me.
" e water " was a writing mistake. The right writing was: 1 liter of water.
Now, if it is possible for you, I'll write all I did.
Thanks
alex


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## Topher_osAUrus (Sep 14, 2017)

Assol said:


> Now, if it is possible for you, I'll write all I did.
> Thanks
> alex



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.


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## Assol (Sep 14, 2017)

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


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## Assol (Sep 14, 2017)

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).


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## Assol (Sep 14, 2017)

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.


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## Assol (Sep 14, 2017)

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.


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## Assol (Sep 14, 2017)

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


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## Topher_osAUrus (Sep 14, 2017)

Assol said:


> 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.




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.


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## Assol (Sep 15, 2017)

I had problem with stannous chloride. And I tested itseveral times. Using a pipette, i think that a few drops of it could gone in the liquor solution.
Do you think that only a few drops are enough for the neutralisation?
Grazie


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## g_axelsson (Sep 15, 2017)

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


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## Assol (Sep 15, 2017)

Thanks all!
the board are new but descarged from production. The producer told me that he use not less than 0,6 g/kg... are big 40cm x 20 cm.... as soon as i've got picture i'll send it.
Grazie


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## Assol (Sep 15, 2017)

Yesterday I put copper tubing in the liquor... this mornind something was precipitated... i'll leave the copper inside the solution untill monday and i hope to find something more


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## Topher_osAUrus (Sep 15, 2017)

Assol said:


> Thanks all!
> the board are new but descarged from production. The producer told me that he use not less than 0,6 g/kg... are big 40cm x 20 cm.... as soon as i've got picture i'll send it.
> Grazie



G is right, the little bit of gold got precipitated in your second picture above, where the 500g of smb was added.

I know the producer told you that he used no less than .6g/kg......but, this is the precious metal game, and to take a seller at their word, is the fastest way to get played


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## Assol (Sep 17, 2017)

Hi,
Before the dissolution in AR, i had 98 gram of solid in the filter.
Afrer dissolution in AR , I had only 41 grams of solid stuff.
This is the picture of solid stuff... just same plastic, i think.
grazie


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## Assol (Sep 19, 2017)

This is the result...
Comment please!!!


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## Assol (Sep 19, 2017)

...


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## Assol (Sep 19, 2017)

...


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## g_axelsson (Sep 19, 2017)

Looks like old coffee, what are we looking at?


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## Assol (Sep 22, 2017)

Nothing precipitated!!!!!


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## g_axelsson (Sep 22, 2017)

Sorry, no one can help you since you don't give us details.

Göran


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