Advice About Twice Refining Gold!

[Anonymous]

Hello members,

I have some gold that I'm refining for the 2nd time (8.6 grams) but something is puzzling me.

* My AR solution is a clear gold color after all the dissolving has been done. Some minute settlement on the bottom. I believe it's some borax.
* My gold pieces were put in a 100ml beaker, and although I used less than 30ml of AR, it seems that I need to add some H2O to the solution.

From what I've read, it would take approximately 1 - 1-1/2 teaspoons (tS) to drop one (1) gram of gold out of solution. Being as though I put 8.6 grams of once refined gold in the solution, with just enough HCL to cover the items, and then I added the HNO3 slowly, over heat. Everything is just fine, but I have about 30 ml of everything. If I were to add at the very least 6 tea spoons of SMB, there would be no liquid at all.

So, my question is:

* Should I upgrade my beaker, put the liquid in it, then add an equal amount of water, then drop the gold with SMB?

I just can't see me dropping 8 grams of gold in a 100ml beaker with about 30ml of solution.

Kevin

 

[Geo]

Dissolve the SMB in another 30ml of water. That will double your volume. Too, If your SMB is fresh, Less than a gram for gram of gold is plenty. Try 5g of SMB and test with stannous after an hour or so. If all the gold doesn't drop the first time, you can always add more.

 

[Palladium]

Why are you saying teaspoons instead of grams of smb? If you were following procedure at this point you would dilute your solution per protocol, allow silver chloride to drop, filter, add smb and drop.

 

[its-all-a-lie]

You only add the equal amount of SMB to the amount of the expected gold yield.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=570&hilit=how+much+smb+to+drop+gold

 

[Anonymous]

Why are you saying teaspoons instead of grams of smb? If you were following procedure at this point you would dilute your solution per protocol, allow silver chloride to drop, filter, add smb and drop.

I'm saying teaspoon because it has been mentioned here on the forum. I'll look for it. That was an estimate per gram of gold. I never said I wasn't following protocol in anything I said or even asked. Some of you use nitric acid based on the amount of silver or other metals you have, or even making AR, but I add nitric acid a bit at time and let it work, and then after that, I make other decisions. Like I said, everything is going well. There is NO problem at all. I'm doing everything as protocol calls.

Protocol doesn't say that if you were to dissolve once refined gold for the 2nd time that it has to be in a certain size beaker. No size beaker is told to be used. Certain size beakers are said what was used. A big difference there.

Also, as far as "protocol" says, I have not heard once that it's STANDARD to dissolve your SMB in water 1st, and it's being practiced that way, even on the forum I use my SMB dry, right out of the bag and I scoop it into whatever I'm working with and it works for me. Since you can...., ok, but it has NEVER been told that it's protocol, or, in my own ways, "It MUST be done that way to achieve 00% expectations". I don't see it that way, although I would like to. I can do the same things other members do, at the same safety level , and accomplish the same EXACT thing. The only difference(s) is that we use(d) "different" methods/protocols/procedures, to do the same EXACT thing.

Who recovered more? Who recovered less?... Well, it's about the same. No difference. Just a different procedure.


Kevin

 

[Anonymous]

You only add the equal amount of SMB to the amount of the expected gold yield.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=570&hilit=how+much+smb+to+drop+gold

That, I already knew. My question was if I need to add some H2O to bigger beaker with the solution in it and then drop it with SMB. My solution will NOT support an "equal amount" of smb, not unless I add water to the solution, and then SMB, or add SMB to water and then pour into beaker.


Kevin

 

[MarcoP]

Also, as far as "protocol" says, I have not heard once that it's STANDARD to dissolve your SMB in water 1st, and it's being practiced that way, even on the forum I use my SMB dry, right out of the bag and I scoop it into whatever I'm working with and it works for me. Since you can...., ok, but it has NEVER been told that it's protocol, or, in my own ways, "It MUST be done that way to achieve 00% expectations". I don't see it that way, although I would like to. I can do the same things other members do, at the same safety level , and accomplish the same EXACT thing. The only difference(s) is that we use(d) "different" methods/protocols/procedures, to do the same EXACT thing.

Hi Kevin, I'm not sure why you used bolds and capitals when nobody in this topic have yet used the words protocol, SMB and dissolve in the same phrase apart from you. Moreover nobody has used the vocabularies "standard" or "must" which are so emphasized by you.

Geo said to dissolve your SMB in water. Probably because the water created in situ by using a dry SMB won't be enough to keep Sodium Chloride (created in situ again by SMB) dissolved in such concentrated solution. Also some prefer to use it dry, others premixed with water, most of the time it's just a matter of personal preference. SMB also needs some free HCl too.

Palladium instead was talking about the protocol of diluting the main liquor to decrease the solubility of any Silver Chloride dissolved in the solution. More dilution will be able to push most it out and will be faster to settle.

In your last reply you can see Geo's and Palladium advices being useful to you.
As I can read they are both giving you the best advice for this particular case. I feel that if diluting the main liquor then there is no need to dissolve your SMB in water.

1. You had a bad day, 2. You misunderstood their advice, 3. I misunderstood your tone.

 

[butcher]

I have referenced milliliters of acids used to dissolve a gram or ounce of gold in teaspoons of acids, this reference of teaspoon (or cups) was only meant to give the reader who was unfamiliar with milliliter measurements an idea of how little acid it takes to dissolve their gold.

Teaspoon or the reference to it, was not meant to be used as a measurement, where measurements of milliliters would the be preferred method.

 

[necromancer]

Also, as far as "protocol" says, I have not heard once that it's STANDARD to dissolve your SMB in water 1st, and it's being practiced that way, even on the forum I use my SMB dry, right out of the bag and I scoop it into whatever I'm working with and it works for me. Since you can...., ok, but it has NEVER been told that it's protocol, or, in my own ways, "It MUST be done that way to achieve 00% expectations". I don't see it that way, although I would like to. I can do the same things other members do, at the same safety level , and accomplish the same EXACT thing. The only difference(s) is that we use(d) "different" methods/protocols/procedures, to do the same EXACT thing.

Hi Kevin, I'm not sure why you used bolds and capitals when nobody in this topic have yet used the words protocol, SMB and dissolve in the same phrase apart from you. Moreover nobody has used the vocabularies "standard" or "must" which are so emphasized by you.

Geo said to dissolve your SMB in water. Probably because the water created in situ by using a dry SMB won't be enough to keep Sodium Chloride (created in situ again by SMB) dissolved in such concentrated solution. Also some prefer to use it dry, others premixed with water, most of the time it's just a matter of personal preference. SMB also needs some free HCl too.

Palladium instead was talking about the protocol of diluting the main liquor to decrease the solubility of any Silver Chloride dissolved in the solution. More dilution will be able to push most it out and will be faster to settle.

In your last reply you can see Geo's and Palladium advices being useful to you.
As I can read they are both giving you the best advice for this particular case. I feel that if diluting the main liquor then there is no need to dissolve your SMB in water.

1. You had a bad day, 2. You misunderstood their advice, 3. I misunderstood your tone.

if you start reading the posts from the top you will see that you are not correct MarcoP
testerman is a smart person that has been a member for a while now, he is not taking the steps to advance his knowlage as a refiner. (good going testerman)

 

[Palladium]

He ain't to smart or he wouldn't be asking dumb questions that if someone had done their studying instead of asking would know. He ask for help in the first thread and then when someone points out what he is doing wrong he says " Well i didn't really need your help anyways i was just asking, but thanks i'll do it my way anyways because it works". Since you're so smart testerman why would i point out the two questions i did? Just answer that and i will know that my time was not wasted pointing out the flaws in your perfect system. The reasons we have procedures or protocols is so that when you follow them you learn the answers for yourself instead of asking questions that any novice should learn from the beginning and wasting others valuable time. Not to mention most of the Eureka processes you seem to come up with is riddled with inconsistencies or wrong information that other will be lead astray by. Just to spoon feed you the answer and stroke your ego is not the objective of this forum and as a side note even though everyone else is quick to forget your transgressions forgiveness from me is earned , not demanded! I'm trying hard to not to judge you based on previous actions, but damn if you don't make it hard. Now if you're ready to learn why did i ask the questions i did? One questions has been answered for you already.

 

[etack]

Teaspoons were made for house wives without scales. nobody should base any measurement off a tsp. in any laboratory environment. I think they should be banned from baking recipes too, but I am working that out.

I learned a saying from a bakery I worked at once. : A pint's a pound the world around but only in liquid measure." They weighed everything from flour,salt, to eggs.

Use a scale.

Eric

 

[Palladium]

I think they should be banned from baking recipes too, but I am working that out.



Eric

Now that's funny!

You know he's right in some ways, but yet that's not what we try and present as a teaching lesson. Even though i teach measurements and protocol the truth is i grab my storage container and i liberally pour the smb without giving though to measurements. Experience dictates that i can do that and the reason i can do that is i don't have to have numbers when i'm looking at real time information to draw my educated conclusions from, not guesses or conjecture! So yes he is right somewhat in the statement he made about everyone does it a little different, but in order to figure those techniques out one must first learn the proper procedures and protocol to follow so that one has a firm understanding and the wisdom ( wisdom is the key not knowledge ) to be able to deviate from protocol and still achieve those results with a margin or error. Things are laid out in a curriculum for a reason.

 

[Geo]

I agree that If you understand the basics, you can work around most unknowns. Using SMB to precipitate gold and the method of it's use is purely a personal choice. Some will swear that they get better results diluting it in water and other would rather add the dry powder. I use dry SMB to gauge the concentration of nitric acid in solution. I seldom use dry powder to precipitate gold. If you watch closely, the powder will normally turn brown in top before you can mix it in by stirring. I don't believe this is gold. I believe the sulfur dioxide gas is forcing all metal, in just the area of where the dry chemical hits the bubbles being produced underneath it, to precipitate from solution. This may not be right but it can't be good for the process. That's my preference. I'm not going to say that my way is better than your way and hope you wouldn't tell me my way was wrong unless you can prove it in a way I can understand.

There's many ways of doing the same thing. If you are learning, you can ask for help with an unknown. You shouldn't be so willing to bite the hand that feeds you so to speak. If you get an answer that you don't like on this question, if you are polite, you may get a better answer next time.

 

[Anonymous]

I am still working on the dissolving of my gold pieces and all is going well. No problems at all.

Here is what came to mind from what I've learned from refining.

* Just add more HCL to the beaker, and if needed add more HNO3, or simply upgrade to a larger capacity beaker.
* Just add more HNO3 to the AR to keep the reaction going.

Right now I added more HCL + HNO3 to the same beaker because I actually had more gold undissolved. At the rate I'm going, I'll have the gold dissolved and then I can simply transfer to another beaker, and use the SMB from there. I might add some H2O to solution. But from the concentration of the solution, even at the low level of liquids in there (40ml) , I am thinking probably 1 - 2 teaspoons (4.9ml each) would drop all the gold. I'm thinking they would be bigger pieces being that they're in a smaller containment unit. It's just a theory of mine.

I was actually thinking about once I filter when all the gold dissolves, and then, without adding any water, add the smb, about 1 - 2 teaspoons. I'm thinking that all the gold would drop, especially in a smaller beaker. Again, just a theory.

Now, this is the part where I would simply take 1 teaspoon (4.9ml) of smb and add just enough water to dissolve it, and then add it to the gold solution, and then stir it up..... that small of a beaker would mix the chemicals upon impact of the smb because it's such a small area to fill. If that would drop all the gold, then I could see in certain instances that you would need to dissolve your smb first, and not pour the powder directly in the solution.

If it wasn't for this forum and all the great members here, I wouldn't know anything about refining.

Oh.. I meant to say this too. I need to study more and understand approximately how much Nitric (HNO3) to use per gram of gold. I've been doing good on my HNO3 additions because I've learned that the Nitric acid can be your killer when it comes to the recovery (dropping) of the metal(s) Only ONCE to this day have I used UREA. I've had my 3lb? of UREA for about 3 years now and only used it once. Personally, I see no need for needing it if you not rush the Nitric (HNO3) reaction. With the right heat, you'll dissolve the metal, hopefully. But all in all, I have used about 10ml of nitric and all my gold isn't dissolved. If I would have read the amount per gram I probably would be finished by now. Yet, learning what I'm learning is worth it simply because of the experience.

Once I'm finished, I'll either try the smb already dissolved in water and add it to the solution, or I'll add water to the solution, and then add the dry smb to it. Either should work, but I'm thinking the dissolved smb would work the best, considering less water. Just a thought.

I'll post results.

Kevin

 

[g_axelsson]

It's a personal style, but this is how I mix my SMB and gold.

I always add it dissolved in water because when I add it as a powder it usually just ends up on the surface and fizzes (probably because I drop the gold from a highly acidic solution). The gas just goes to waste in the atmosphere and I'm adding salt to my gold chloride solution.
When adding it dissolved in water the SO₂ gas is created under the surface and precipitates the gold without a lot of losses. I simply use less SMB when using it dissolved.
The only drawback is that it adds volume to the solution.

Okay, here is how I do it:
1. put a small beaker on a scale and tare it.
2. Add SMB at roughly the amount I think I need.
3. Add some warm to hot water, swirl it around a while to dissolve the SMB.
4. Add most but not all SMB solution to the gold chloride, the saturated solution is quite heavy and sometimes it goes straight to the bottom.
5. Wait for the gold to settle, usually it takes less than a minute or a couple of minutes.
6. When clear, add some more SMB and check for any signs of precipitation. If there is none then the gold is probably all precipitated already. Don't add any more SMB.
7. If there are additional precipitation make some more solution and go back to 4.
8. Decant the barren solution to the stock pot together with subsequent washes.

You could test the solution with stannous if you want, but it won't see any fine gold that hasn't settled. I use the stock pot for catching both dissolved values and fine sediments of precipitated gold.

Here is a picture of SMB solution giving off SO₂ bubbles from the bottom. Each bubble leaves a small trace of precipitated gold before the gas is used up.


Göran

 

[yar]

Good post Goran I was looking for some information on dissolving SMB to precipitate gold. Thank you. I am going to give this a try with some powder from my cell.

 

[Anonymous]

I finished the gold. Everything went smoothly. A picture of it is at the link below:
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=21535#p222510


Kevin

 

[jason_recliner]

Göran, that's a really useful guide. Thank you.

If I understand correctly, the SMB itself doesn't precipitate gold, but generates SO₂ in the presence of HCl. Now I've been keeping a jar of saturated solution of SMB. I'd put way more powder into the jar than can be dissolved, so it would always be at max strength for any given temperature. Over winter it created a beautifully large crystal. But now I see a problem with my method, which I would like to share.

In liquid solution, you can really only add "some", rather than easily measure it out. Without involving lots of maths. Which I hate. I've recently added about twice what I thought would be required and it still leaves my solution yellow. In small increments, I've added about 20ml of saturated SMB solution to my acid which holds maybe 0.5g of gold. It's not been dropping any more gold. My stannous chloride has obviously gone off; it showed nothing though I know there's gold sure left because this is my first "second refine" and it's still a pale lemon colour. Interestingly, there's a little gold coloured scum floating on top, some gold coloured deposits in amongst the brown and some slight gold coloured deposit around the jar surface. A gold "ring around the bath", if you will.

Today I finally have a few new proper borosilicate beakers that I can heat, some decent 0.01 - 500g scales and am trying to tidy up all my previous [stt]messes[/stt] batches before I start any new ones.
Because it's so diluted I had to split the batch, and I syringed 2/3 of the yellow liquid (no gold powder) into a separate beaker. Dropping 0.5g of SMB powder into the batch described above, to which I'd already added "heaps" of SMB liquid, it fizzed nicely, then I immediately saw the brown reaction shown in your post. Half an hour later I have the image below, the clarity of it pleases me.

So here's my question: It is possible that SMB solution will age and lose its ability to release SO₂? I wonder if the gentle, two week old, adding of SMB has contributed to a more gold coloured precipitation. Thinking back, I also may have added too much bleach, even though in small increments too. There were some chunks that just wouldn't dissolve. I added more HCl when I thought it was getting lower than 2:1.

Also, I'm interested in experienced opinions about the powder colour. It looks a little dark to me. Who concurs that it needs refining once more? Without my shiny new borosilicate beakers, I've previously only been able to warm solutions during a HCl wash to about 70-80°C or so. And having cracked a glass jar more than once before (putting a cold jar on a hot coffee maker plate) it's not something I want to get close to again.

 

[g_axelsson]

Good to hear that you could use my advice. 8)

Jason, your first description of yellow liquid not reacting on SMB sounded a lot to me as iron in solution. It would also give no reaction with stannous. In addition it can give a yellow surface film of iron hydroxides that can develop a rainbow colored shine.
But the dropped powder looks like you got some gold out of it. It has to be quite thin layer if it's only 0.5g and with that color I guess it's really fine and would easily be disturbed if you would try to pour the liquid off.

Whenever I get a drop of extremely fine black gold powder I draw the clear liquid off with a syringe and put it in the stock pot. Then I dissolve the fine powder in a bit HCl + Cl and drop it again. (I actually prefer HCl + strong H₂O₂ to dissolve the gold again, it doesn't add any salt to the solution and can be evaporated if I want a more concentrated solution.)
To redissolve and drop the gold takes me circa 10-20 minutes, less time than I spent on writing this response. 8)

Another way to clean up your fine gold powder would be to boil it in HCl, following the advice in the "Get your gold shiny" post by Harry. I think you need to get the temperature up over 70-80°C, among other things that boiling will give is stirring the powder both so the acid can reach all the powders and to get the cleaned gold to clump together.
I might be the wrong person to give advice about this though since I've never done that procedure yet.

To know if your stannous is bad you need to have a gold chloride test solution to test it on. Whenever you get an unsuspected negative reaction test your gold chloride, or first thing every day you are using it as many members are doing.
Don't believe something, test it and know!

Göran

 

[jason_recliner]

Thanks mate.

The 0.5g was only an estimate. I'll know once I get my powder out and dry. As for iron: possibly. You see, when I did my incineration of the first drop a few months back, I used what I thought was a large stainless steel serving spoon. But it turns out not to be [Edit: it was a spoon, just not stainless.] and maybe a flake or two of whatever it's plated with has gotten in my first incineration. Next time I'll have a proper op-shop ("thrift-store" for those in the US) pan. My re-refine was to hopefully rid myself of that contamination and I think it's been a success. It wasn't a rainbow (you mean like oil on water?), it looked like actual, monochromatic, gold coloured, dust on top, but there's very little. It won't even cross the meniscus to reach the edge of the beaker. Water spray didn't help and it's too small to worry about saving from the stock pot.

I'm super happy to boil in HCl and have Harold's triple HCl/water wash and incineration posts saved in my bookmarks. I just wasn't game to get that temperature previously, not having proper beakers until today. I ran a ~20 min boil of today's powder in fresh HCl. (Gentle bubbling - and my new portable gas stove is showing the signs. Glad I've got my gloves!) The acid stayed clear. Maybe this suggests I won't get it a lot cleaner anyway.
In future e-scrap batches, I'm planning to pre-boil in HCl, rinse that off to get rid of tin and not foul my AP.

Regarding the stannous chloride, I know as a positive-only test I have to take any negative results with a grain of salt. In this case, I knew my gold was still in there even without it. But yes, I definitely always try to test it whenever I use it. In this case, it's the actual knowing there was surely gold still in solution has proven (suggested) my most recent stannous to be untrustworthy. The SMB powder has proven the gold was there.

It seems I make Stannous Chloride, and two weeks later it's capable, at best, of determining the existence of a major federal reserve.

I'm still only working with miniscule amounts. I don't know if it's the confidence of finally having a bit of minimum proper kit, but I'm starting to think I might be almost on the right track. Melting, however, is a world away.