Recovering precious metals from polishing sweeps

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Ageo308 said:
Well I decided that the urea option was just not for me as the volume of water I have is just too large to handle with. I had no choice but to ring the customer and let him know that it will take a little longer if he wants quality results. I will keep you posted on how it goes.
I congratulate you on your decision. I made it a policy of assuring my customers that quality was my objective, and there were no shortcuts taken to quicken processes if they compromised quality.

For the record, I promised 7 day delivery on polishing waste, assuming they didn't have hundreds of pounds. Once you get on to the processing, you don't generate huge volumes of solution. It becomes a tradeoff where you can't make a profit by being 100% accountable----so you charge a reasonable fee for your work, which includes washing the waste one time, leaving traces for later recovery by other methods. That way the customer isn't cheated---and you can get the work out in good time. If you choose to be 100% accountable, you must charge a higher fee, so the customer isn't any better off than if you charge a slightly lower one, and not account for minor traces. Once again, this becomes an excellent savings plan.

I explained the above to my customers and had none that were unhappy with me-----especially when they realized that the return on their waste material was greater than they used to get----which was almost always the case because they had been using major refiners, many of which are known to treat the consumer with less than honesty.

Things are looking up for you!

Harold
 
You have to pick a balance between profit and the amount of business that you are able to handle.
That's what competition is all about.

You have to decide if you are running a business or a charity.
 
Hehe well I was back on track evaporating (been 2 days now as I have about 30 litres of solution to go through), been following everything as per normal and when I filtered it (because I did a poor job beforehand so I wanted to make sure the gold solution was clean as so once precipitated it would be cleaner) I noticed a crust of some form at the bottom of the dish I had been filtering? I also noticed it at the bottom of my buchner funnel? could it be I'm evaporating for too long and it's starting to cake?
(I thought that only happens when the liquid becomes low)? I'll take some pics tomorrow and see if anyone knows what the story is. I'm using a grade 2 on top of the buchner and grade 5 on the bottom which is filtering the solution quite good but this flakey crust is annoying me.
 
Did you dilute your solution after evaporation? If not, that may be the problem. If so, it's common for a lot of flocculence to come out of the evaporated solution when it's filtered, but none of it should be getting through the filter. If that's what's happening, I'm stumped.

I suggestion for you; A Whatman #5 is an exceedingly slow filter. It catches everything, but it also clogs almost instantly. You're usually far better off to use a #2 when filtering an evaporated solution that isn't clean, reserving the #5 for the occasions when you re-refine your gold. By that time, the amount of contamination borders on zero, so the solution will filter quite well through a #5. Surprisingly, if you can get a #2 to run and not pass the fines, it will be far faster, and will eventually retain all of the contaminants. It wasn't unusual for me to re-filter a portion of my solutions once the filter settled down, and they always do. In the very end, a #2 will often yield solutions every bit as clean as the #5, and costs you a lot less money, with the added bonus of speed.

On the outside chance that you may have some lead in your solution, did you include a little sulfuric in the evaporation process? It doesn't take much ---a few drops. Lead will self precipitate when the solution cools if you don't expel it as a sulfate. Just a thought.

If you can post a picture of the stuff you're talking about, please do. I'm not sure what it might be if it's not crystals of what ever you have in solution-----but I think there's a good explanation. All we have to do is determine what it is! :wink:

Harold
 
Harold I haven't diluted the solution, I did add sulfuric to each batch I was evaporating. I must admit a mistake I made thow (due to me rushing) was when I tried expelling the nitric with urea I then added my precipitant. The next morning obviously because of the excess nitric it didn't precipitate but I'm assuming the crust could have been caused by that. Anywayz I will post a pic today showing you what I mean.

I learned 1 thing from this batch, be patient and follow the procedure as per normal (no shortcuts)!


:)
 
Just to update:

I think where I went wrong was not adding HCl during the evaporation. I decided to add some of the crystals in a beaker with water and some HCl to see if it will dissolve or wash the gold chloride out of it. Well it dissolved a lot of it and the remaining crystals were left white. I can't help but think the urea must of added to this. Anywayz to fix up the error I made I'm going to wash all the solution I have left with water/HCl then filter it so when it's ready to be precipitated the solution is not dirty.
 
Adrian,

I have to confess, I'm lost. I don't recall having a situation like that, ever. I won't eliminate the addition of urea as being part of the problem, but I never used it, so I have no concept of what it does to a batch of gold.

A couple things come to mind. You talked about evaporating and not adding HCl. My procedure was to evaporate until the solution had turned quite dark, then add HCl to expel the nitric. Assuming it had none to expel, but the solution bubbled somewhat and formed a trace of what is likely silver chloride, I assumed it to be fully evaporated. Because the evaporated solution contains no water, the boiling point is higher than one that does, so the evaporated solution is usually hotter than the boiling point of water----so you should see a slight boiling when you introduce the HCl.

Keep in mind, I always had a button of pure gold included, which assured the consumption of any free nitric. At that point, I would take up the evaporated solution with water. I can only assume you did that, too. If not, anything that got included in solution that didn't get diluted past a level of saturation would surely grow crystals. What they are I don't have a clue---but your remedy sounds like you're on the right track. Crystals are pretty good at rejecting any impurities, so if you wash them as you suggest, you should recover almost 100% of the traces of values.

If you have any doubts about the contents of the crystals, toss them in your stock pot and let them do what they will---which is likely to re-dissolve in good time. When you decant the solution from your stock pot, what ever it is will be discarded. which should be your objective. Any values that may have been carried over will be recovered from the wastes collected from the stock pot at some future date.

Sorry I'm not more help. Without having had a similar incident, I have no way of knowing what the score is.

One thing to remember----the initial wash you do after you've incinerated polishing wastes should be adequate to dissolve and remove any traces of things like that. If the solution came from polishing wastes, it's entirely possible you didn't do an adequate job of eliminating things that are soluble in HCl, and they got dissolved later, and included. With proper washing and rinsing, they would have been discarded earlier.

All of this is nothing more than me thinking out loud. I am not suggesting that I know that it's true. Just something for you to consider.

Good luck with the next step. Let us all know how it goes.

Harold
 
Hi Harold, a couple of questions I have:

* When you evaporate, what happens if you let it evaporate right down till there is minimal liquid? Would you be evaporating gold? The reason I ask is because my fans are yellow in colour and I can only think that's some from of metal chloride staining it (hopefully not gold).

* The reason I ask is because when you're dealing with litres of solution it's hard to determine what's being evaporated.

* Also how much precipitant would you allow for? And is too much no good or it does no harm? The reason I ask is because if I fall short then you need to wait another night for it to drop.
 
Ageo308 said:
Hi Harold, a couple of questions I have:

* When you evaporate, what happens if you let it evaporate right down till there is minimal liquid?
When you take the solution too far, elemental gold will begin to precipitate. That's a sure sign that you have eliminated the nitric. Depending on how clean the solution is, it is usually a dark red, leaning on red/brown/black when that happens, and it's very obvious. The solution, assuming you've kept if hot, will appear to have metal flakes ----much like aluminum or bronze paint. Hoke has a procedure to recover from the condition, but it has risks. I simply would add a drop of nitric, along with a few drops of HCl, and watch to see the gold dissolve.

Using an added button of pure gold during the evaporation process pretty much eliminates the need to evaporate to that point. I evaporated until I knew the nitric was gone, then I'd evaporate a little more if I had excess HCl present, but only to guarantee no filter failure. Excess HCl does no harm otherwise. Once evaporated properly, the solution would be taken up with tap water to dilute it well. A target volume is 3 ounces of gold per liter before precipitation, although I didn't follow that rule. I also precipitated with SO2 gas, and iced my gold chloride before precipitating.

Would you be evaporating gold? The reason I ask is because my fans are yellow in colour and I can only think that's some from of metal chloride staining it (hopefully not gold).
That's not a good sign. Get some sunlight on the fans. If it's gold, they'll turn purple. You can also test with stannous chloride. If you don't see a color develop, you are seeing something else, but you may still be evaporating too quickly. Your solution should never boil unless it's covered with a watch glass. You must not hurry evaporation. Might pay you to read Hoke on that subject. Also----when you're dissolving your values, keep them covered with a watch glass. It's not a novelty--it's mandatory. The gasses that are evolved come off with considerable energy and carry droplets with them. A watch glass will collect the values and return them to the beaker.

Also how much precipitant would you allow for? And is too much no good or it does no harm? The reason I ask is because if I fall short then you need to wait another night for it to drop.
A rule of thumb is that an ounce of ferrous sulfate will precipitate an ounce of gold, but as Hoke suggests, an excess is a good idea. You might consider setting your sights on 1¼ ounces/ounce.

There is no need to wait for gold to settle when precipitating. Test your solution immediately after introducing the precipitant. The reaction should be instantaneous. If, after you've mixed your precipitant with the gold chloride solution, you still show values when testing with stannous chloride, you can immediately introduce more precipitant. I used to mix what I expected I'd need, then hold back on a small percentage. Mix, test, then either discard the extra, or introduce it to complete the precipitation. That way you wait only once for the gold to settle.

What you add may not be harmful----depends on the precipitant. Ferrous sulfate will wash out quite well, so I wouldn't be too concerned about using too much. Just insure that you follow the guidelines I set forth for washing. They work, and work very well.

From this you can conclude that there are benefits to using SO2 from a cylinder. You test constantly as the gold precipitates, and stop introducing the gas when it's all down. It pays to stir the bottom when you have an abundance of gold, for gold chloride gets dragged down with the gold that comes down first if there is not a complete precipitation (assuming it settles quickly-----which is often the case).

Harold
 
Thanks for the tips Harold, I recovered a small batch (9 grams of gold) and I'm going to finish the next batch early next week.

I'll keep you posted
 
Hi Harold
Since everyone here likes those pictures of your old factory I was wondering if you had a picture of the furnace you used for incinerating the polishing sweeps.
Thanks
 
No furnace was used. I did all of my incinerating in a discarded stainless frying pan. You can burn a surprising amount of material in one.

I don't recommend this process unless you have a hood that will accommodate the considerable heat, and has a filtration system to recover dusting.

I simply heated the pan from below, using a gas hot plate. The single burner used for incineration was adjusted to provide a maximum flame. Once the material was burned, I'd raise the temperature in the pan using a large Hoke torch, to insure that I had consumed all of the carbon. Any that remained would glow brilliant yellow white when oxygen was played on the material.

Harold
 
Polishing sweeps are composed of grease (the binder in polishing compound), sandy grit (the active ingredient in polishing compound), lint (from the buffs) and very tiny balls of karat gold (from the gold that was polished). Sometimes it will also include paper and buffs.

personally, the very first thing I'd probably do is take the sweeps, put them in a closed container filled with technical grade Acetone and place the container in an ultrasonic tank for a few minutes. This will help get rid of NVOCs (non volatile organic compounds) ie: waxes, greases, etc. Then I would rinse off with Isopropynol to rinse away those NVOCs (without rinsing away any "solids"). Remember that order.. Acetone THEN IPA, IPA is not a good degreaser and does virtually nothing for NVOCs.. and if you just let the Acetone evaporate off without rinsing, you've just wasted it, because it will just leave the NVOCs behind.

After that point, I think incineration would be a good way to go, but I'd definitely try to clean some of that other crap out first.

There's a phrase you will see quite often on these boards GIGO ("garbage in, garbage out").. it's proven to be a VERY handy thing to keep in mind. 8)
 
Mixed hexanes are a great way to degrease things, even better than acetone and much safer than leaving either acetone or isopropanol on material that concentrated acids may be added to (always incinerate after any solvent is used!). I prefer using hot caustic as it gets more of the silicaceous material dissolved and saponifies any grease but it's very dangerous to one's eyes.

Lou
 
For that, and likely other reasons, I simply incinerated such wastes. Often with the plastic bag in which it came. More smoke, but less of a hazard for the refiner, and perfectly effective. I couldn't see wasting the time (and chemicals) involved, when in the end it had to be incinerated, anyway.

Harold
 
Harold_V said:
More smoke, but less of a hazard for the refiner, and perfectly effective.
:?:

ummm... I'm a heavy-smoker and even I prefer not to expose myself to the nasties that could come from incineration.

(I only bring this up because, I suspect some people who visit these boards would do this in their garage/living room/kitchen/kid's bedroom.. without proper ventilation and not even think twice about it..)

I'm not ball-busting you, Harold, I promise. :mrgreen: I hold your experience and opinions based on such experience in very high regard, I'm just surprised by that particular statement coming from you without some form of cautionary note to go along with it. 8)

Derek
 
I have 10 kg of incinerated powder dust from silver polishing waste. How much nitric acid do I need to leach it. How long is the process? Do I have to heat it? Can you give me more idea on the process of leaching. many Thanks.
 
silveras said:
I have 10 kg of incinerated powder dust from silver polishing waste. How much nitric acid do I need to leach it. How long is the process? Do I have to heat it? Can you give me more idea on the process of leaching. many Thanks.
There is no logical answer to your question, because no one can predict the amount of silver and/or base metals present without an assay.

What I suggest you do is start with a small amount of dilute nitric and allow it to work. Keep adding in small portions until you get no further reaction. Be careful not to add too much too quickly, to avoid a boil-over.

Unless the waste came from a bench were silver was the only value worked, you can expect the resulting material to yield gold as well, maybe even platinum and palladium.

Read Hoke.

Did I mention you should read Hoke?

Harold
 
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