# Ni not letting gold come out



## Charles Connor (Jul 6, 2013)

Hi everybody, Im having some trouble taking my gold out of solution because i think its the nikel. I use the AR and SMB method, ive done it always and i get my gold, but this time i got copper from the solution, I dont know how come i got it from a gold method, i need to know how to take the Ni out of solution.
THANKS!!


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## Lou (Jul 6, 2013)

Nickel doesn't interfere with gold precipitating. It may coprecipitate with it using some reducing agents, but it's unlikely.


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## g_axelsson (Jul 6, 2013)

Have you tested your solution with stannous? What was the result?

Göran


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## Pantherlikher (Jul 6, 2013)

Hi...
From your 3 posts so far, I'm assuming you digest karat gold in Aqua Regia. Use Urea to "rid" AR of Nitric. Then drop gold with SMB.

Now you've run into a problem where you get copper instead of gold.
Correct?.

Better descriptions of what you do and how give better clues as to what's wrong.

From your 3 posts total here on the forum, To me, you've just started doing this and watched a few Youtube screwup videos and feel you know enough...to get into trouble maybe.

I hope you've spent your short time here reading and learning how to properly follow procedures so as to NOT cause harm to anyone, including yourself; and you've learned the right way to do it completely.

Urea does NOT do anything with nitric acid. There is alot of information here on Urea and is easy to find by Searching for it. 

How did you determing that only copper dropped out from the AR and that Ni might be causing the problem?

B.S.
Alittle information makes anyone dangerous... but fully learning how is key to success...


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## Charles Connor (Jul 7, 2013)

-Pantherlikher,
Thats the method i use, exactly like you describe it, it has worked always and thats how ive been taught to, i did read abot the urea and also the sulfamic acid to kinda get rid of nitric acid, the problem is that i got the dust of the pulishing machines from another workshop, when i do it with mine i get the gold from this same method. The most i refine are this dust from the polishing and what we sweep from the floor, i have almost no trouble with this from my workshop, but metal scrap is like 4 times a month, im having trouble with this scrap too i dont get the ammount calculated and the reaction get really hot.
Also i think its copper because i did a karat test with acids and it reacted as a piece of copper i tested too...
And i think its nickel because that factory does a lot of plating and stuff like that, im not really sure, i just thought it was the matter...
-g_axelsson.
And the stannous test i cant get any stannous to prepare it, i know how it is, but i dont get the metal, also i have not look a lot to find it. Once i tried with this chips solder, but i didnt melt with the HCl warming it. thats how i read it was made...


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## g_axelsson (Jul 7, 2013)

Charles Connor said:


> -g_axelsson.
> And the stannous test i cant get any stannous to prepare it, i know how it is, but i dont get the metal, also i have not look a lot to find it. Once i tried with this chips solder, but i didnt melt with the HCl warming it. thats how i read it was made...


I don't understand how people (it is not only you) can't manage to get hold of a piece of tin. It seems like there are gold and platinum everywhere but tin is really hard to find!
I went to the second hand shop and checked for some beat up pieces of pewter. I bought five old damaged beakers for a dollar each, that will last me for a lifetime.
I have dissolved some tin-lead solder from a circuitboard and just for fun tested it and it worked.
Look at a plumbers shop, a hardware store or a electronics shop and ask for solder.
Buy some from ebay.
Without checking I'm pretty sure you can buy tin from amazon too.... checked and, tada! They even have a solder department with more than 1200 objects! 219 was lead free. http://www.amazon.com/b?ie=UTF8&node=13837421
Tin is so much easier to get hold of than acids and that never seems to be the problem.

I would guess that the reason you can't get any gold from your solution is that you don't have any in it.

By the way, you don't melt tin with HCl, you *dissolve* it. Melting is done with heat.

You should read Refining Precious Metals Wastes by CM. Hoke, it will help you.

Göran


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## Charles Connor (Jul 8, 2013)

Ok im gonna try that solder, cause i did it with it and did not dissolved, sorry for my english but its not my first lenguage, also i have read the book, not all of it, but what i needed to know at the moment, thanks for your suggestions


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## butcher (Jul 8, 2013)

Charles Connor said:


> Ok im gonna try that solder, cause i did it with it and did not dissolved, sorry for my english but its not my first lenguage, also i have read the book, not all of it, but what i needed to know at the moment, thanks for your suggestions



Reading just some of Hokes book, you could only learn enough to get into problems, you have to keep reading to learn how not to create these problems and how to get out of problems when they do happen.

The solder you tried before may have been high in lead, try to find 95% tin solder, hammer a piece the tin flat and very thin, it will dissolve easily in heated HCl, store your test solution with a piece of undissolved tin in the bottle to keep the stannous chloride fresh for a longer period of time


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## bswartzwelder (Jul 10, 2013)

I bought tin shot (maybe called pellets) from eBay. NOT expensive. Works very well for me. I made some stannous using stannous chloride crystals and HCl and then dropped in a pellet or two of tin. Stored it in a brown dropper bottle in my fridge and it has lasted for months. Still works very well. I expect it will die soon.


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## Geo (Jul 10, 2013)

bswartzwelder said:


> I bought tin shot (maybe called pellets) from eBay. NOT expensive. Works very well for me. I made some stannous using stannous chloride crystals and HCl and then dropped in a pellet or two of tin. Stored it in a brown dropper bottle in my fridge and it has lasted for months. Still works very well. I expect it will die soon.


you are taking well care of your reagents but keep in mind that its oxygen that will eventually cause your stannous chloride to stop working.every time you open the container, oxygen is causing the solution to convert to insoluble tin oxide.


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## Palladium (Jul 10, 2013)

I have never had stannous go bad myself. I'm wondering if it could be my storage method? I put mine in a eye dropper bottle and it's never gone bad yet.
:?:


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## Harold_V (Jul 11, 2013)

Keep it away from oxygen and it should last a long time. 

I kept my stannous chloride in a two ounce dropping bottle (the type you see in Hoke's book). Because I used it daily, I never turned the stopper so it wouldn't be exposed to atmosphere. As it turned out, about the time I was to the bottom of the two ounces, it was turning milky yellow and was losing effectiveness. I'd suggest that it was good for about three weeks, but my memory is not what it used to be. It could have been longer or shorter. 

I kept a few small pieces of tin in my solution. 

Harold


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## bswartzwelder (Jul 11, 2013)

I always keep a small bottle of (store bought) gold chloride nearby. Every time I get out the stannous chloride, the first drop goes onto a paper towel that has a fresh drop of gold chloride solution on it. Saves a chance of a headache from using stannous that has gone bad.


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## Palladium (Jul 12, 2013)

I to also make sure their is excess tin in the bottle.


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## Lou (Jul 12, 2013)

I add stannous chloride crystals to 6 M HCl and put a couple grams of tin powder on the bottom to keep it from oxidizing to stannic chloride.


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## Charles Connor (Jul 12, 2013)

Thanks again for the suggestions, now i have this question/doubt: i was dissolving some scrap in AR, but it got really hot, it was boiling and i was not aplying any heat, why did that happened, i think it was because i added the ammount of HNO3 at once and not in parts, as i have read in all the posts,being hot affects when adding the SMB, as i read in a Butcher post, so i think thats why i did not got the ammount of gold espected, that was almost 70gs from 170gs of 10K scrap, i only got 60gs and it did not precipitated any more from the solution...
Thanks in advance fopr your suggestions.


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## butcher (Jul 13, 2013)

Heat and even light and sound can be produced from a chemical reaction, actually fire is a chemical reaction, also gases being formed in a reaction can also look like boiling.
heat or cooling (absorbing heat from things around the reaction) can be produced chemically as exothermic or endothermic chemical reactions .

As far as not being able to precipitate all of your gold from solution, there can be many reasons why this could happen, gold not in the solution, free HNO3 or HNO3 forming in solution from excess nitrates, gold becoming colloidal (tin in solution), or a very dirty solution (which can also form a mix similar to colloids), not the right type of chemical precipitant or not enough of it, there can be other reasons, and then there are also conditions that gold precipitates better than it would in other situations, like gold precipitates better from dilute solution than it would from a very concentrated solution, cold solution are normally better than very hot to boiling solutions especially if the precipitant is a gas or a reaction that gas produces gas to reduce the gold ...


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## Charles Connor (Jul 15, 2013)

Ok im going to do it now using 3.8mL of HCl and 0.95mL of HNO3 per gram as i recently read from a post here and to precipitate the gold 1g of SMB per 1g of gold, what i dont understand very well is the part of getting rid of the HNO3, when it says that heating the solution to a syrup, what i understand is that it has to lower the volume but what kind of syrup is it like maple syrup contexture... and then add some HCl and watter to double its volume.
Also when i do this process there is a grey powder at the bottom of the beaker, i filtered and melt it and it looks like silver, i have not read anything about it in the C.M. Hoke book if silver precipitates that way, because i get it as AgCl2 when refining with HNO3 and Cu...


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## butcher (Jul 15, 2013)

Charles,
you will want to be sure to inquarter the gold and pour shot.
if you measure out the HNO3 and add it in small amounts letting each reaction play out and dissolve as much gold as it can, before all of the gold is dissolved raise the heat some, it makes the acids more aggressive, and can be somewhat concentrating the solution as you are working to dissolve the gold, the heat will also make small amounts of free nitric more active and can help to use it up as it dissolves the gold, before all of the gold is finished dissolving, I will normally begin my first evaporation, this uses up nitric already involved and as the solution gets concentrated I can add a few drops of nitric at a time to finish dissolving the gold, this way I end up with very little to no free HNO3 to remove.

I evaporate till the solution is very concentrated, first mostly water evolves then free nitric then any free HCl as we concentrate the solution, as long as you do not boil the solution the gold chloride will remain in solution and will not leave as vapors, so basically this gold salt solution concentrates as we drive off free excess water and acids, the gold chloride will get darker yellow in color (if copper is not involved to make it green or brown), as you concentrate this yellow color gets darker, when really concentrated the solution takes on an orange to reddish color, this is normally my goal during concentrating the solution, but the main thing is you do not cook the liquid gold chloride out to salts or burn these salts to the bottom of your pan, a few drops of H2SO4 as recommended by C.M. Hokes, when she describes the process in her book, can help to keep the gold from forming salts so easily, as sulfuric acid or sulfates are not very volatile at all, and will remain when all most every other acid or liquid has been vaporized off.

I normally will add a sprinkle or two of sulfamic acid, after the above processes, mainly just to be sure.

actually you may not have any free nitric with the first process of adding HNO3 only as needed,but if there was the three evaporation process would take care of that, the sulfamic will get any nitric if there was even a possibility it made it this far, this process I use is overkill, but I really got tire of having free nitric left in solution giving me trouble (so I guess I over kill the nitric acid).

The stannous chloride test is also a good indicator of whether you have free nitric acid in solution, because for the stannous chloride to develop the purple of Cassius the gold has to be reduced to colloidal gold metal particles, this will not happen if free nitric keeps re-oxidizing the gold at the same time the stannous is trying to reduce it, basically with free nitric in solution the nitric keeps taking the electron from the gold the stannous chloride is trying to provide.


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## Charles Connor (Jul 16, 2013)

Im reading the book again and now i understand it more than before, also when i wrote the last post i already had my gold in AR but i did not quart it with silver, I did the dennox with urea and then the SMB, i got it exactly as i calculated, i also use some sodium bicarbonate after i add the SMB, it seems that makes the gold ticker...
Also did my SnCl2 solution test, tried with muriatic acid,29%, and it was no fizzing, then with HCl 37% and it did dissolve the Sn... I found some in a bottle i bought months ago and try it with this solution after taking gold out, with the one i found it turns blue and with the one i did turns yellow, so i dont really know wich one works, i think mine is the wrong
Thanks Butcher for the suggestions in your posts... I will continue reading and researching


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## butcher (Jul 16, 2013)

Charles, 
From when I read your questions and comments, it makes me think you do need to do more reading and slow down on trying to recover or refine until you get more understanding of the processes, spend more time on learning and getting a good understanding, forget about getting gold, that will come easier after you gain more experience.

I feel you are jumping in head first without having a good enough understanding of what it is you are jumping into,or how to even jump the right way, this will normally just cause you trouble, I suggest concentrating on Hokes book, and the forum guided tour, then work on the getting acquainted experiments that are in Hokes book to get a better Idea of the reactions, study well a certain process, or the different processes involved to recover and refine a certain type of material then start processing one of the simpler materials like memory fingers, or karat gold, studying well the processes and working with a material that has less problems involved, this way you learn what to expect, and gain experience, for when you later work with the more complicated materials which will produce reactions you do not expect, this way you can use your experience, if you begin working with complicated materials where you get all kinds of reactions, when you do not know what to expect, you are then not sure what is what.

Muriatic acid is just another name for hydrochloric acid (HCl).

Keep up the good work of studying Hokes.


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