help me please

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First check the stannous against a solution you know has gold to assure yourself the stannous chloride is good and working.

The stannous chloride works with or without free nitric, I can't count howmany hot reactions I've tested for gold with stannous and never had a problem.

If the gold is in the foam, it is likely in the metallic state and will not be detected by stannous chloride.
 
the stannous came sealed from factory im not sure how long it would stay good or how i would get it back to being good im not sure if its in solution or the crystals but its in there some where i know there is gold in this solution because as i have said before i put gold of a known purity in it aka a one ounce 999 gold bar
 
spcake89 said:
the stannous came sealed from factory im not sure how long it would stay good or how i would get it back to being good im not sure if its in solution or the crystals but its in there some where i know there is gold in this solution because as i have said before i put gold of a known purity in it aka a one ounce 999 gold bar
I am going to go out on a limb here. Why would you put an known .999 one ounce bar into solution without knowing exactly what you are doing? Its sounds like you do not have the equipment or the testing ability to process this type of material. 4metal, Harold, Geo are some of the best members here to give advice and yet you seem to not follow what they are asking you to do.(test with stannous) If it were me i would put the solution up, get Hokes book and read or re-read the first 100pages and research the forum.

If indeed there is gold in the solution like you say, it is not going anywhere and it can be reclaimed but you will have to get an understanding of what you want to do and do what you are asked of by chemist here. I do not mean to offend you, but that is Just my two cents.
Ken
 
jeneje said:
spcake89 said:
the stannous came sealed from factory im not sure how long it would stay good or how i would get it back to being good im not sure if its in solution or the crystals but its in there some where i know there is gold in this solution because as i have said before i put gold of a known purity in it aka a one ounce 999 gold bar
Why would you put an known .999 one ounce bar into solution

Why indeed?
I am not flaming you, I make my comments to focus not only your thoughts but the thoughts of any newcomers reading this thread in the future.
What were you hoping to achieve by putting a bar of stamped purity gold into solution? You never were going to improve the quality of the metal because it is already as pure as you can get it, with the exception of 9999 or above. If it was stamped 999 and you have dissolved it, at best you will come out of this experience with a button of unknown purity metal (which de values it) and you will have spent time, money and effort on depreciating the value of it,and, thats only if you are lucky and don't loose any of it in your 'processing'.
You could have easily and less expensively achieved the same or better result (depending if you manage to recover the full oz) by placing your 999 bar in a clean melting dish and melting it, this would still devalue it but at least you wouldn't loose any.
Thats my two pence worth.
 
i did cause i wanted to test myself which apparently was a foolish decision but i did test with stannous and nothing happened there was no reaction. i wasnt worried about the little bit that would get lost i just didnt want to lose the whole ounce.
 
No matter your reason, I personally do not want to see you loose your gold.

If it were me, I would try heating the solution to see if the froth at the top would go back into the solution while hot. If it does, then I would continue heating the solution to steaming NOT BOILING and let it reduce to about half its volume, let it cool then add some hydrochloric acid and see if you get a puff of brown smoke. If it does off gas that brown smoke then you still have free nitric that needs taken care of.

If the froth was still there after heating then I would let it cool again and separate the foam from the solution and handle the two separately.

No matter how you decide to proceed, the excess nitric acid has to be addressed.

I hope that if anything I have just posted is inaccurate a more experienced member will correct me because I'm still pretty new at this.
 
spcake---

From your picture, your solution is only 1/2 cup, and yellow. Plus 1/2 cup or more of froth, about the same color.

If the whole ounce was in solution, I think it would be closer to a red color.

If the whole ounce was in metallic form in the froth, there would be so much weighty solid bulk, that I think at least a good part of it would fall to the bottom of the measuring cup.

A half cup of froth would have more air than solution, so if your ounce of gold was entirely in solution, including the froth, you would only have maybe 3/4 cup of solution---and I think it should still be a darker color, at least orange or red-orange. Maybe all the SMB and urea would account for the light color, I have never done that (among the many other mistakes I've made!) so I can't say for sure.

Maybe knowing what you should have done can put things into perspective, and help you sort this out. First, for practice, use a 1 gram bar instead of a full ounce. Put it into about 200 ml of HCl, and add a drop of nitric. Put it on heat to 150 to 160 degrees F (use a $25.00 IR "gun" thermometer). Watch the color change and bubbles (reaction) from the gold bar. When the reaction stops, add a little more nitric. Keep letting the reaction stop, and adding nitric, until you have an orange color, then take it off the heat when there are no more bubbles.

When there are no more bubbles, all the nitric will be gone. You should have a small chunk of the bar left on the bottom. (Whatever the color of the solution, stop adding nitric while there is still a small chunk of gold left, to be sure there is no more nitric in your gold solution.)

Pour this solution into three small bottles with lids. Make it so there is about 125 ml in one bottle, 50 ml in the second bottle, and 25 ml in the third. Cap and keep the 125 ml bottle as a reference. Fill the other two bottles up to 100 ml total each, with water. Use the two diluted solutions as your standard gold solutions for testing---one being weaker than the other will give you an idea of the sensitivity of your stannous chloride testing solution. You can even make another bottle of gold solution which is half the strength of the 25 ml bottle, to see how sensitive stannous is with solutions that are barely yellow. I've seen it indicate on filters which have been sprayed down with water until there is no yellow color at all, even.

Then make some stannous chloride solution for testing for gold in solution. There are several sources of material to make it with. Some people use tin solder (lead-free), some use the white powdered stannous chloride, and other methods. Then dissolve it in HCl. Some add water. Hoke lists her formula, and there are many mentions of various ways in the forum---just use the search feature at the top right of each page. Like the experts say, the most important thing is that you always make your testing solution of the same proportions, so you become accustomed to, and thus understand its indications with unknown solutions.

You said that you have some stannous solution that you bought, so you can test that with your standard gold solutions that you made. This will give you a certainty of what to expect when you test any unknown solutions.

If you are uncertain of your stannous solution, and you are uncertain of your gold solution, the only conclusions that you can possibly come to will always be uncertain when something unusual happens, like what you have now.

Just like in navigation, you absolutely must have some points of known positions. Testing solutions which you are sure about will provide those known points. Your standard gold solutions will provide certainty about your stannous solutions.

Understanding this will help you get out of your situation with your gold solution.
 
You could cut a couple of pieces of electrical copper wire and add it to your solution to cement your gold. Then take everything that cements out and run it again to get it right. I think that would be your safest bet at this point. If you decide to do this let us know and we can walk you through it.
 
Lets slow down here and address one thing at a time. I gather you bought some reagent stannous chloride to make your testing solution from. How did you make up your stannous chloride test solution? What did you store it in? When did you make it?

If the solution was made and stored in a bottle with a lot of air in the bottle it will go bad faster than if it was in a small bottle full of solution. So storage is important, storage where it can freeze or bake in the sun will also shorten its life.
Also if it is just old it can go bad. Adding pure tin metal to a freshly made solution will add to its shelf life.

Stannous chloride is a powerful tool for refiners, lets get to the bottom of how you made it, when and how you stored it before we waste time speculating if it's in the solution or the foam. Your gold is there, and testing will tell us exactly where so lets approach this step by step.
 
I feel you should listen to 4metals, slow down and find the problem with your stannous test or reagent, then deal with the solution.

I just wanted to remind folks of Harold's trick of adding a button of gold to the heated solution to help remove the nitric acid without all of the time involved to evaporate out the nitric in the three times method.
 

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