goldsilverpro said:
Harold,
We could argue about these things til the cows come home. I just hope our bantering is instructive to the readers.
Why do you think I challenge you on subjects with which I don't agree? It is my objective to not only expose things that I feel are wrong, but to describe, to the best of my ability, what's wrong with them, as I see them. I'm not sue, who tossed a wet blanket on subjects but refused to say why. Readers should have every opportunity to not pick up bad habits, which both of us have, no doubt. Our discussions serve a good purpose, even if they annoy you.
I think we both have to search our memories to come up with this stuff. I know I do. No matter how we did it, we both came out with very similar final products. I admire you for perfecting a system to put out pure gold. You should realize, however, that probably no one else in the world uses your exact system yet, there are many other aqua regia refiners that put out gold as pure as yours, with one drop, myself included
If that was the case, why would any of them run parting cells, or for that matter, use the Miller process?
Sorry, I don't agree. Everything I've read indicates that even 9995 on a consistent basis isn't a reasonable expectation for a first refining, and my experiences back that notion perfectly well. That isn't to say that you can't achieve it, but to expect it routinely borders on the unreasonable. I'd be particularly hard pressed to believe you can do so with karat gold that has been directly dissolved with AR by dividing it finely in lieu of inquartation, where base metal and silver content are reduced. The direct AR process isn't a great deal different from how I processed filings from a jeweler's bench, which consistently yielded poor quality gold, and that's after a prolonged boil in nitric until there was no further action. This was after incineration and before AR. Why would you, or anyone, expect gold that comes from a dirty solution (dissolved base metals of all kinds) to be as clean as gold that comes from a clean solution? You don't feel there's more dragdown?
In your post, you used words like, "the thinking is flawed" and "stupid", when referring to my methods
Sorry, you're wrong. I did not make reference to them because they are "your methods". I made my comments because they're true. Note that I did NOT tell you you were stupid, nor that your thinking was flawed. I have no clue where you were taught to use those processes, which could have very well been passed to you by someone that was well meaning, but poorly informed.
If you use those procedures, that's your choice, but I outlined exactly what's wrong with them. Remember, doing something for an eternity that is not in your best interest will not turn it to something that
is in your best interest. Hundreds of people doing something stupid doesn't make it smart. You get my drift.
You may have learned to live with the consequences of these things, but I don't think I can stand by in clear conscience while you endorse methods that have a potential to create more problems than they solve. Both of them do exactly that.
Although these words get my blood pressure up a bit, I try to calm down and look at this thing logically. I think that sometimes you feel that anyone with different experiences than you is flat out wrong.
Wrong again. I've clearly stated that there are many ways to achieve the end result, but I've also stated in clear English that if readers follow the advice stated in Hoke's book, one thing is assured. They will achieve success. Not sometime, but every time. Fact is, even Hoke presented options. I chose to exercise those that appealed to me, or were most convenient. I do not think my way is the best, but it was the best for me-----having tried various means for many operations, in keeping with Hoke's recommendations. If they worked for me, they can work for others as well, saving them the task of reinventing the wheel.
I don't know where you got the idea that I cover the gold with flux
This sort of lead me that direction:
http://goldrefiningforum.com/phpBB3/viewtopic.php?t=337&highlight=needle+scaling
In the link you said:
Needle guns are quite powerful. I used to use them to remove slag from ingots. They might break up IC's. The problem is to confine the material so it doesn't fly all over. Your chamber might just work. Not a bad idea."
I poured gold without any flux on my ingots. How did it, otherwise, get there on yours?
Since pure gold ingots have a specific visual appearance, I chose to do nothing that would eliminate these visual effects. I wanted any educated buyer to have no doubts that my gold was pure. I didn't fire polish or buff the surface, for example. I didn't stamp my bars.
Yet you clearly stated "Needle guns are quite powerful. I used to use them to remove slag from ingots."
Not only does slag leave tell-tale signs where it was on the ingot, but the removal by mechanical means, particularly by a scaler, defaces the ingot surface beyond recognition. You can't have it both ways.
I only used very small pinches of flux, mainly alternating between borax and niter. I usually used one pinch of soda ash, at the start, to adjust the flow of the flux. If it did reduce oxides, it made no difference, since all were eventually removed with niter. The molten gold forms a convex meniscus and the flux slides to the edge of the button
That reminds me of the guy that gets pulled over for running a stop sign. He insists to the cop that he slowed down---which is the same as stopping. Cops say to him------"Tell you what we'll do. I'll start thumping the hell out of you with my night stick. When you think you've had enough, you tell me if you want me to slow down, or stop".
Tell me, which would you prefer? You have a container of hot water and some salt. You don't want the salt in the water. Is it easier to keep it out, or to get it out once it's dissolved? That's the type of reasoning you're presenting to the readers. I don't agree, and I'm not going to agree in a week or a year. What a prudent individual does is keep it out, not toss it in and pretend it's not a problem. You, my friend, are passing a perfect opportunity to learn that soda ash is a reducer, and should not be included in flux for fine gold. You want to thin your flux? Use fluorspar. It does a better job, anyway.
I don't recall EVER needing to thin my borax when melting pure gold. The only time it got thickened was when there was an abundance of base metals. I trust you read my comments about melting my second refining. Melting dishes had only one color beyond clear-----a purple tinge----from colloidal gold. Borax, when clean, is not particularly viscous at the melting point of gold, but quickly sets as the gold freezes. Pouring any off when the gold has set is a tall order. You might be successful in scraping it out.
Hoke discusses raising the quality of questionable gold by the addition of niter (potassium nitrate). I tried it several times----never with success that was in keeping with my goal. Maybe you settled for less than I wanted. Dunno. I wasn't content to have gold that had oxides----and I never was successful in eliminating them by that means, not even after a quarter hour of heating with an oxidizing flame (a Hoke torch, fired by natural gas and oxygen). There was clear evidence they were lowered (dirty flux), I'll grant you that-------but-----again------if achieving high quality gold was as easy as melting with a proper flux, that's what we'd all be doing. It doesn't work---although it does remove some oxides. Maybe if I'd have spent a couple hours!
When I had too much flux, I usually let the gold barely solidify and then poured off the still molten flux
Been there, done that, got the T shirt, learned it didn't work. You don't think I tried every dodge in the book, too? I ended up double refining because it DID work, the other dodges didn't. My original method (first year or two of refining) of returning gold was to melt in a dish, with enough flux to reach the edge of the button, but not to cover it. The moment it froze, but was still red, I'd sprinkle a light covering of borax on the surface, then extract the button from the flux iwth tweezers. It was then pickled in sulfuric acid. The button was delivered to the owner, not shot. The flux, by now, was very sticky, and would not pour.
Therefore, the finer the gold, the more likely the gold will be impure.
This is a cause and effect situation. My observations were that gold precipitated from dirty solutions came down very fine---and dirty. I never did get gold to precipitate fine from clean solutions. It was so eager to agglomerate that the particles came down large, often very large. The contamination in dirty solutions prevents that from happening, at least from my observations. You're certainly entitled to see it the way you do------but I'm every bit as convinced that I am correct as you are.
I always shot for lumpy, fluffy, light or medium brown gold. More like a sponge than a powder. This stuff rinses and leaches beautifully, maybe even easier than the heavier blond powder. Sometimes, the last, maybe 1%, of the gold dropped darker than the rest. I don't know why this happened, but it seemed to cause no problems, since the bulk was of good color..
I'm pretty sure I can address the different colors. I've already stated that color is a function of concentration. Here's one for you to consider.
On rare occasion, when I'd re-refine, I'd have a touch of nitric still left in solution. The gold came down fine, but when it came time to wash the gold (with HCL), I'd get the slightest of dissolution. Stop washing after allowing it to boil for a brief period (to consume the nitric with the precipitated gold) and then ice the solution. The precipitation from the now very dilute solution produced gold that was slightly darker than the balance of the precipitated gold. There was so little present that it did not agglomerate as well as the heavily concentrated solution on the original precipitation.
When filtering, our leaching/rinsing system was a bit different. I went hot water rinses - approx. 50% nitric leach - hot water rinses - ammonia leach - hot distilled water rinses. We both used ammonia. I used it for silver chloride and, I think, you used it to detect any blue solution of nickel or copper. Only traces of these metals produce a strong blue color in the ammoniacal solution.
No, I had no need to detect copper. It did expose it if it was present, however, for, as you allude, the slightest trace of copper displays a bold blue color. I'd find hints of blue, but not routinely. I used ammonium hydroxide for one reason. When you change pH, elements that are in solution are prone to precipitate, so by going from acid to basic and back to acid, I had the opportunity to convert any sort of contaminant the could prove troublesome. Washing well with ammonium hydroxide is just one more step you can take to improve the quality of gold without adding anything to it that can prove harmful.
You used HCl and I used nitric. I feel that nitric will remove everything that HCl removes, plus more. I never did understand why you used HCl.
By now you should understand that I am a student of Hoke. I used HCL because it is the recommended wash. You do recall that we're talking about a chloride solution, yes? Unless you take steps to eliminate all traces of chlorides, you risk dissolving your precipitated gold when you wash with nitric. I think so, and Hoke thinks so. I wouldn't dream of using nitric for the final wash, and I'm not concerned that it worked for you, or not. Assuming you do the nitric wash, and have a negative reaction, you'd be walking a very dangerous line when you started introducing ammonia to a gold chloride solution, a risk I'd rather not take. One thing sure, you wash with HNO3 long enough and that's going to happen, just like the occasional batch that contained a trace when I washed. I don't want to be held responsible for providing even a hint of something that can jeopardize a reader unnecessarily. If you can present cites that prove my position to be in error, I'd welcome the input. You likely understand that I'm not all that keen on opinion. I already have some that we don't agree on.
I'm not concerned if readers follow my recommendations, or not. What I am concerned with is that they use practices that don't create problems, and don't harm themselves or their loved ones. Follow the advice in Hoke's book-------the pitfalls have all been addressed. It will tell you how to wash your gold-------although I'm pretty sure it doesn't address the use of ammonium hydroxide. I had to learn that from a novice refiner. Wish I had my book at hand.
Here's the deal. You bring an ounce of pure gold to my shop, and I'll provide one. We'll make a setup to refine the two ounces. I have enough nitric and HCL and sulfuric to do the processing. Together, we'll alloy it to 14 K yellow, then we'll process it by your means. If you can produce gold with a single precipitation that melts without oxides, the gold is yours. If it has oxides, any oxides, the gold is mine. I'm willing to put my money where my mouth is. I trust you have enough faith in your grandiose claims to do the same.
Harold