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I'm pleased to hear that. I feared you took a wrong turn and had discarded your gold, as you may have noticed.Ageo308 said:Ok Harold, we havent discared any solution and all of them have been filtered.
It was my reasoning that there is far more iron in the waste (from polishing compounds) than copper or nickel, each of which will be dissolved to some degree because they are oxidized by incineration. HCl is an excellent solvent for iron, unlike nitric, although it, too, will dissolve iron. The solutions are very different, however, with the nitric solution eager to precipitate the iron as rust, which would occur when you rinsed the material. That can complicate your processing, and leaves behind unwanted iron.I just re-read hoke's book and revised some of the important areas. A quick question on what she says.
Basically she mentions that you should Incinerate, sift, magnet then if there is shellac/grease etc.. to boil in caustic soda/lye (to remove it). Then she mentions to wash in nitric/water acid unlike your procedure which is HCL/water, it says in her book you can use HCL but it doesnt dissolve copper or nickel (which will be present in these sweeps), the only draw down with using nitric/water is that it will dissolve silver but you can store that and recover it at another time.
* so im interested to know why you choose HCL over the nitric?
My experience in running my wastes by this manner tended to support that logic in that the solution, after precipitation of gold, was relatively clean. If you test your initial wash solution for copper and nickel, I'm quite sure you'll find that a good deal of it does, indeed, get dissolved with the HCl operation. A drop of ammonium hydroxide in a drop of the solution will turn dark blue if there is copper present. Likewise, a drop of the solution, along with a drop of ammonium hydroxed and a drop of DMG (see Hoke) will disclose nickel with a pink display. It left the silver behind either as a chloride, or in the elemental state, although I imagine it was converted to chloride by the gold chloride solution if that was the case. You would be unlikely to be able to recover any silver by this process, but it is not lost, it's still in the dirt. More on this, below.
Note that I did NOT process filings by this method. Only floor sweeps and polishing wastes. Filings are processed with nitric acid, then AR.
You see considerable evidence of my claim in the color of the original HCl wash. Beyond that, what you'll come to discover is that solutions that come from dirty substances and a nitric wash tend to be difficult to filter. Without the HCl wash, your gold chloride solution has a tendency to plug filters. I've had a liter of solution take as long as three days to filter. From that, I learned to incinerate suspect materials and then do an HCl wash, even if the material had already undergone a nitric wash. In that case, the material must be incinerated a second time, to kill any nitric that is present. I found nothing to equal HCl's ability to clean material of substances that were difficult to filter. That is particularly true of refining gold filled objects in volume. There is often a little lead and tin included in gold filled objects. They respond to the treatment I mention in a very positive way.
What you have been instructed by me is a process that evolved through trial and error and was used for many years. To be quite frank, I don't recall what Hoke recommended, so it's been interesting to hear that her version varies from mine. I assure you, if you follow my instructioins, you'll achieve a level of quality and extraction that is very good, although if you have doubts, don't hesitate to follow her instructions. I've commented time and again, I learned refining from her book, and know that aside from her recommendation to use gasoline freely when incinerating, her information is trustworthy.
It's redundant. A boil in lye will remove a good deal of the unwanted material, but it won't eliminate everything that will be troublesome. In the end you still must incinerate, so I see no good reason to duplicate operations unless there is some gain. Incineration performs every possible useful function, and eliminates the hazard of using lye. Should you splash lye in your eye, blindness is guaranteed, yet a drop of nitric in the eye, while painful, is not serious. I've been through that and came out fine. Learned from that to wear eye protection.* And why not boil in caustic as she mentioned to remove the shellac/grease etc?
That's correct. Read the chapter that involves testing of precious metals, and follow her instructions in buying and building the necessary solutions. In her book, I recall that she refers to stannous chloride as testing solution A, but I could be wrong. I haven't looked at a copy in well over 12 years.And i cant see anywhere that stannous chloride is mentioned in hoke's book, is this to determine what metals are present in the solutions???
If you do not have stannous chloride, immediately work in the direction of obtaining it. Do a search on the board if you must, for there's a lot of information available. Many of the guys here are making it with 95/5 solder. Personally, I preferred to use pure tin and stannous chloride crystals, which was my routine. Without it's use, you run blindly, not knowing the status of any of your solutions. Also, do yourself a favor and discard solutions by proper means the moment you conclude they have no value. It takes very little time to find yourself inundated with a huge variety of unknown and unwanted solutions, so you not only trip over them, but you spend a good amount of time screwing with them unnecessarily when you finally decide on disposal.
P.S the sweeps we are using is my partners and he has plenty to spare and experiment with.
P.SS i think im getting you now Harold
I hope so. I'd like to see you succeed. This method is quite good. I have serious doubts that you could come up with one any better.
Correct me if im wrong but when you say combining the wash waters (yellow) solution is the colour yellow because its suppose to be gold?
That's correct. Gold chloride that isn't contaminated with copper or nickel is yellow, deepening to a dark red/orange, depending on concentration. The wash water is nothing more than dilute gold chloride, which is why you combine it with the darker yellow solution. If you had stannous chloride, you'd see by testing that the solution would react with a purple stain. That's what gold looks like when combined with stannous chloride. As the concentration deepens, so too does the color. Very slight presence of gold will yield a faint purple reaction.
we havent discarded this solution and if im understanding right we are suppose to evaporate that yellow solution to basically have clean gold??? Is this correct???
No----evaporation does NOTHING to improve gold quality. That's determined by the washes you do prior to dissolving the gold, by the precipitant you choose to use, and by the washing you do after the gold has been precipitated. Evaporation serves two purposes. One is to concentrate voluminous solutions so you aren't working with gallons when a liter is adequate, but most importantly, it, when carried out properly, eliminates unused nitric acid. That is a requirement to recovering your gold. If you leave it behind, it will react with not only the precipitant, slowing or stopping the operation, but assuming you are successful in precipitating your gold, when you wash it, the residual nitric will re-dissolve some of your gold, until it has been consumed. That's not desirable, as you might understand. Please read Hoke on evaporation of solutions, and learn to do so. Also, if you have a button of gold at your disposal, it really helps to add one, as I've already mentioned. Weigh it before introducing to the solution you're evaporating, and weigh it afterwards if you want to know how much of the button was dissolved in the process of eliminating any free nitric. The use of a button will avoid evaporating the gold solution down to a heavy syrup, so it saves a lot of time. If you choose to use a button, you must still add some free HCl as the solution thickens. That way it will form AR and consume the free nitric by dissolving the gold button. Very slick way to process, if I must say so myself.
If it is i will add more AR to the mud to dissolve any more undissolved gold then wash with the HCL.
I'm not convinced you understand the wash purpose in using HCl. It is NOT used to wash the material once you have introduced AR. In this case, if you subject the material to more AR, simply boil the material in the AR and water mix, then add a small amount of HCl to insure that you haven't depleted what you introduced with AR. If, when you add the HCl, you see brown fumes coming off the beaker, that's a sign that you did just that. If you see no reaction, the next thing to do is add a few drops of nitric. If there is any undissolved gold present, you should see brown fumes coming from the beaker. If you do not, you can safely assume that the dirt is now barren of undissolved gold, and needs no further processing. At this point, add a little water, stir well, and allow the solution to settle.. Decant the solution, then add a generous amount of water and stir, again allowing the contents to settle well. Your objective here is to rinse the mud clear of all dissolved gold-----which requires NO HCl. Just plain old tap water will suffice. Wash the mud until you're satisfied that you are not getting a return worth the trouble, then get the dirt in a coffee filter and extract the last of the liquid, which should be combined with the balance of the yellow solutions we've been dealing with.
The dirt, at this point, is relatively valueless, although it will contain traces of values that you haven't recovered. Included in that there can possibly be platinum, which dissolves very slowly, and silver in the way of silver chloride. I suggest you dry this material by heating, just as if you would to incinerate. You'll see nitric fumes coming off at the very end of drying. Heat until you no longer see the fumes, then cool the material and store in a covered drum. If you collect enough of the polishing waste in this fashion, it has market value, or, down the road, when you have enough, you can run it in cyanide and extract the silver, along with traces of gold, all of which are never fully recovered, try as you might.
DO NOT STORE WET WASTE MATERIALS. THEY WILL RUST EVERYTHING IN YOUR WORK AREA THAT WILL RUST.
Hope some of this helps.
Keep us all informed on your progress.
Harold