# Please some advice for proper pH before precipitation



## Butterfly989 (Jun 25, 2017)

Hi,
Please look at my video at youtube: https://youtu.be/ibvTdvuJDXo
I made short video how I try to precipitate gold with copperas (iron sulfate). I have tried to neutralize AR with sulphamic acid but any success of precipitation. Also I tried hydrazine hydrate and tin chloride methods, but still no results. So I think now, i have problems with proper pH level controll. I read that it should be 1pH before precipitation. But still ... I have missed smth. What????

And please tell me can I do smth. with my black solution you see at the end of my video? neutralize it somehow or boil it? After boiling I´ll get more Fe as Au or maybe you know some better trick?

Thank you for advance!


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## Topher_osAUrus (Jun 25, 2017)

Please spell out all words, except acronyms generally accepted here. Like SMB, AR, etc...

Never heard of yeast before, definitely a new one to me.. sorry, that was a different thread.. Im an idiot without caffeine in the morning If it was me in that predicament, I would stop trying to fix it by throwing chemicals at it. Instead, I would hit it with some science. Particularly the reactivity series.. 

Place a copper slab in your solution, and all metals less reactive than it will displace out of the solution (basically just precious metals and mercury)...although one metal chart I have seen showed selenium and antimony(?I believe) That were able to be reduced by copper. 
But thats no matter, copper will save your day. It will use up the free nitric, and allow the gold to reduce out .

Question for you though, 
What on earth is the "tin chloride method?
Are you talking about stannous chloride? ...a TESTing method for precious metals in solution?.. I hope you didnt dump a gallon of that into a gallons of pregnant AR, because if you did, you have a colloid that is already reduced out of solution, and no amount of copper will be able to reduce the already reduced..

Can you elaborate step by step what you did please?

Edit to fix


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## Butterfly989 (Jun 26, 2017)

Thank you Topher_!
Tin chloride=stannous chloride method I mean like this video show by Maximov Ro here: https://www.youtube.com/watch?v=oiYEoP2AhOk. 
He took out gold from old DVD. At 6:25 min he neutralized AR with soda (NaHCO3) (not calcined soda). At 8:45 min he used stannous chloride for precipitation. He made stannous chloride, heating Sn in HCl so it is strongly acidic. You can see how he added a bit HCl with syringe at min 10:25 or 10:50. He explained that soda take out tin and it´s not stay in solution. At min 15:40 he´s gotten the same solution what I have with copperas method now. Only difference is: he saw precipitation not me.

OK
I explain what I did with my 800ml filtered (also diluted) AR what I divided into 3 parts.
A: 1/3 part I used for a method I just described at the beginning
B: For 1/3 part I used hydrazine hydrate 98% what I dropped to my solution (not at home  ). I saw a brownish snot occured to the top of my solution what was dissolved after 15 min.
C: 1/3 part i used for, you saw at my video. It was showed step by step. Not any stannous or any chemicals inside. Only green copperas solution (iron sulfate powder+warm water+ a bit HCl in it) what I poured to my diluted AR. I think it could be 50% pure aqua regia and 50% tap water all my solution before I added green copperas solution.

I placed copper plate into my black solution now. Thank you for info !!! 
Let see what´ll happen. It´d be the happiest day during 2 weeks if I´d see change in my black solution after several tests. I´m quite frustrated already. No one give serious advice I have asked from some youtubers before.

I have that kind of ore on my land I bought filling material some years ago. Now I noticed brownish stones among white brickstones. I was curious to test it because red/brown color looked promising for me.
So what kind of method you would use what would be cheapest for precipitate gold from it? I have not electricity there so I can´t boil anything.


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## Topher_osAUrus (Jun 26, 2017)

Butterfly989 said:


> Thank you Topher_!
> Tin chloride=stannous chloride method I mean like this video show by Maximov Ro here: https://www.youtube.com/watch?v=oiYEoP2AhOk.
> He took out gold from old DVD. At 6:25 min he neutralized AR with soda (NaHCO3) (not calcined soda). At 8:45 min he used stannous chloride for precipitation. He made stannous chloride, heating Sn in HCl so it is strongly acidic. You can see how he added a bit HCl with syringe at min 10:25 or 10:50. He explained that soda take out tin and it´s not stay in solution. At min 15:40 he´s gotten the same solution what I have with copperas method now. Only difference is: he saw precipitation not me.
> I do not know why he would use stannous chloride to reduce gold out of his entire solution. It is merely a test to ensure you know where your values are during the refining process, and the gold that is "precipitated" out, is in the form of a colloid. There are much better ways to actually reduce the gold out of solution...copperas, sodium nitrite, sodium bisulfite, sodium metabisulfite, SO2,
> ...


There is a sticky thread at the top of the Ore and prospecting section of the forum. I know next to nothing of ore,
but that thread is great for testing unknowns. 

Stay away from youtube unless it is a reputable members' video, I watched a few videos on there last night that were so far off from reality it was incredible.. Whats even more incredible, was the guy has like 11,000 subscribers.. How? I dont know, nor do I care, but it sheds light on why so many come here that have been lead so very far astray.


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## Butterfly989 (Jun 27, 2017)

Thank you for detail answer!

One question about AR. The book "Refining Precious Metals Wastes by CM. Hoke", there are told: use one part nitric acid to four parts hydrochloric.
But common is 1:3
I have 65% Nitric Acid and 35%-38% HCl. Since I have used it 1:3 but what do you think should I make AR 1:4 ?


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## kernels (Jun 27, 2017)

You should not really ever pre-mix AR the way that we use it. Cover the material you want to dissolve in HCl, then add HNO3 in small increments until all the material is dissolved.


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## Butterfly989 (Jun 27, 2017)

I report about my tests:
I made new solution, the same AR (18h) from ore as I showed my video. Stannous test showed blackness/gold in it again.

First test tube: 30% golden pure AR, 20% solution of Sulfamic acid and 50% copperas solution = light golden clear solution, any darkness, any precipitation, any change.
Second test tube: 40% pure AR + 50% copperas solution = the tea brown solution and again not any precipitation, any color change.
Is it possible that blackness by stannous test in AR is not gold, not palladium but something else what never precipitate. Or there are something in it what makes solution like glue for gold. Or my concentration of AR turn gold to colloidal form always?


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## Butterfly989 (Jun 27, 2017)

Kernels, Thank you for advice!


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## Topher_osAUrus (Jun 27, 2017)

Butterfly989 said:


> I report about my tests:
> I made new solution, the same AR (18h) from ore as I showed my video. Stannous test showed blackness/gold in it again.
> 
> First test tube: 30% golden pure AR, 20% solution of Sulfamic acid and 50% copperas solution = light golden clear solution, any darkness, any precipitation, any change.
> ...



I find that sulfamic helps denox the solution better if the ar solution is still hot. So, I usually add mine after I have completed the dissolution of metal. That way the NOx gas will readily escape the solution (gasses are much less soluble in hot solutions, as well as for every 7 degree increase in temp, reaction speed doubles [so Ive read])
So, what I do, is dissolve my scrap. Add a small bit of aqueous sulfamic, watch the effervescence. Add more based on how much bubbling it does. Add in small increments until it reacts no more.
I then add 2 to 3x the volume of water, let it settle a few hours, so the silver chloride and lead sulfate are on the bottom of the beaker. Then carefully filter it off.

Then, to the crystal clear filtrate, I add my copperas or smb in small doses, so I dont overshoot the precipitant and shoot myself in the foot purity wise. (Excess precipitant ia never good, nor is too little -stannous test)

--The black solution--
Take a small sample of your black solution, put a little heat to it. After it warms up, add a little bit of HCl, does it clear up?
If not, add a few mL of HNO3, let it react.
I think, if I understood your initial posting, that you made a large amount of colloidal gold. 

Colloids can be broken a few different ways. Redissolving them is one, excessive heating with a strong acid like H2SO4 is another (I wouldn't boil it, just heat it up for an extended amount of time) , and I believe evaporating to a crust then redissolving is the last way. I have only tried the redissolve method. So the other ones may have certain nuances that I am unaware of. 

Do you have any pictures you could upload?


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## kernels (Jun 27, 2017)

Very good advice from Topher_osAUrus there, I follow this procedure for denoxxing - [youtube]https://youtu.be/oN8-7q21Cnw[/youtube] ,using a small gold button to determine when a solution is denoxxed, rather than just rely on the reaction of the Sulfamic and Nitric.


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## Butterfly989 (Jun 28, 2017)

Thank you so much for you time for me!
I leave for a week now and can´t continue my experiments. I´m back on Monday and try to follow all that you suggested. Please don´t disappear... I´ll make a photos.
I was thinking if there´d be somebody (or you :wink: ) who´s been specialized to precipitate gold from ores and has good knowledges, I´d pay for a service if he/she´d take gold out of this ore for me and would teache me step by step how and how much chemicals it needed for this process. First I try myself but I feel that I´m not able to finish it by my own. I was bought 2 bottles of HCl yesterday again and was thinking that it is almost one month I have played with that already.


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## Lou (Jun 29, 2017)

If hydrazine didn't get it out of solution it's not there. Hydrazine doesn't care how much nitric acid is there. While the nitric is there making toxic HN3, the gold stays out of solution.


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## goldsilverpro (Jun 29, 2017)

Lou said:


> If hydrazine didn't get it out of solution it's not there. Hydrazine doesn't care how much nitric acid is there. While the nitric is there making toxic HN3, the gold stays out of solution.


Very true. For years, almost daily, I used hydrazine sulfate to drop the gold from a so-called "reverse AR" solution - 50% HNO3, 3-5% HCl, remainder tap water - @ room temp. Dropped all the gold, with no HNO3 treatment required, with very little Hydrazine sulfate. Hydrazine hydrate would have worked as well.


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## g_axelsson (Jul 1, 2017)

Just a comment on that video, by the way I don't speak Russian so I don't know what he is saying.

I could not see any precipitation, the only thing I saw was a purple solution of gold colloid. The bottom of the beaker was just clear. Not surprising actually, the small amount of scrap he used wasn't enough to get any precipitate that could be spotted without a microscope.

And some very sloppy lab work.

Göran


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## niks neims (Jul 2, 2017)

Hi everybody, this is my first post here at GRF so i guess it also doubles as introduction...

I am nowhere near being ready to refine or eaven give any advice, have so much more learning to do, but, as I was studying this great forum, I stumbled on this thread and, as I am fluent in russian, tought, I would jump at the chance of being at least little bit useful 



Butterfly989 said:


> this video show by Maximov Ro here: https://www.youtube.com/watch?v=oiYEoP2AhOk.



after watching this video and hearing this guy ramble on, I seriously suggest do not watch his videos to try and learn anything about refining/chemistry in general.... I am not going to waste my time on watching more of his videos but my guess is that he is simply trying to boost up his views for some of that sweet youtube money (I guess another way for getting gold )... in any case eaven with my very limited chemistry knowledge (now on hoke`s page 171) I suspect that "maximov ro" is full of it :/

As I understand it, stannos chloride is insanely sensitive test for gold in solution (eaven in incredibly small concentration) and can`t be used to precipitate gold... russian in the video is completely misleading, not to mention you can seriously damage your health if you are trying to learn from him, I would eaven suggest putting that video up in rougues gallery, no wonder commenting on youtube are disabled...

anyways, back to studying, awesome stuff you have here guys, I hope to make proper introduction some day


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## Butterfly989 (Jul 12, 2017)

Thank you for answers! I got back home for now and continue my tests.



> --The black solution--
> Take a small sample of your black solution, put a little heat to it. After it warms up, add a little bit of HCl, does it clear up?
> If not, add a few mL of HNO3, let it react.



Very good advice! The black solution didn´t clear up after HCl but I added a bit HNO3 and it worked.
Only thing what I need to do now is to use Sulfamic Acid but not that I have. It is wrong stuff. It doesn´t give any bubbling reaction. I need to buy new one and continue with that.


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