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Sorry for the long wait. my phone had issues and all the pictures are gone. So this is what I have done. I didnt boil the powder. I must have gotten a head of myself. I did incinerate the powder and washed in HCL and then filtered it. The powder was red and so was the acid I filtered. Trying to melt it was hard turning into red slug. I ended up heating it and scraping out with my carbon rod. And I started think this crucible isnt that small and there isnt that much here compared to the four times I filled it when I started. So I looked in my 5 gallon water bucket and collected all the flux pieces that had some silver and gold? So I remelted that and poured it in my bucket, so I could see what I have total. The stuff in the bucket the missed the metal bowl didnt react to my strong magnet. The reprocesssed red powder mix is magnetic. Each have gold and silver swirls and alitte of the rainbow coloring. And I cemented out a bunch of silver . so I put the not magnetic in a bag and left the other in the bowl. I think Butcher was right about the colloidal gold. Which I will be testing that process sunday. It supposed to get in the 60's it will give me a chance to working on that. Any Idea why the red? Here are some new picks.
 

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o.k I have taken the silver and melted it down. I thought there would have been more then what came out, But not as important as what I found. There must have been alittle AR in the wash because some of my silver is gold and some dark red. Any idea what the red is.
 

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Well it turns out that today was a good day to be outside. So I started checking my solution. I have to say I'm not sure if there is gold there were flakes that the HCL didnt dissolve. The qtip was yellow dripped some stannous chloride and there looks like two spots turn dark. If there was AU or PM's wouldn't the whole Qtip turn dark? Here are some pixs of teh process. Just so you know when the acid cleared there was more powder then what you can see here. What do you think?
 

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The Q tip does look like there may be some gold (violet spot), I am not sure why it did not wet the whole Q tip, the yellow only seems to be on one side, also you can test your stannous chloride, as it has a shelf life, and can go bad.
The red metal in the filter could be copper; actually it looks like you have a wide range of metals there.
The red in your solution could be iron. Iron can alloy with gold when melted with gold, the red powder is likely iron oxide / hydroxide (which will not easily dissolve even in strong acids), the red Iron powder will be nonmagnetic (hematite). unless roasted which can then be convert it to magnetite, it can be reduced to iron metal in a melt (although usually not easily without a reducing flux, but in a mess of metal in the melt, the other base metals may take the oxidation, and reduce some of iron in the melt.

Being magnetic confirms iron in solution (red powder rouge iron hydroxide),after melted became magnetic, put this magnetic metal in your stock pot.

The other metal pieces may look like silver or gold, but these will most all be alloys, of each of these metals and a big possibility with other base metals, once you separate the iron magnetic material, and incinerate and treat the powders for tin (HCl boil and washing) neutralize them with NaOH sodium hydroxide solution, then wash well in hot water, dry and incinerate the powders again, to remove chloride salt traces from the powders.

From here I would add all the metals and pretreated powders and metal (except magnetic pieces), and add some sterling scrap and melt them, pour shot, and start over with 50%:50% 70% nitric acid : H2O, to remove silver and base metal.....
 
Thanks butcher. It turns out yesterday was the better day. Today turnout rainy. Oh one more thing after rinsing the pot I reswabbed it, and it took a couple of minutes but the swab turned a light purple. I was thinking maybe, because the solution sat for a month maybe most of the tin/gold started to settle. Which may explain why its not green anymore but light blue.
How should I process the solution? Should I calculate how much solution I have and add the same ratio of sulfuric acid. Like in the last time to check for gold?
 
reign21male,
I am sorry I am kind of lost here; I am not sure what solution you are talking about.

If this is a collided solution that at one time tested for gold,(a solution of gold contaminated by tin, it would probably have reduced more gold from solution over time. And so it can have less gold dissolved in solution, but with tin in solution it will easily reduce gold back to metal, the problem is it may not settle, but stay suspended, as negatively and positively charged particles repelling each other, the thing is these gold colloids will not show up in our stannous chloride test.

The way our tin chloride (stannous chloride) test works is it reduces our gold back to metal colloids, these gold metal particles do not settle, and to our eye we see a violet color by their reflection of light, If gold is already reduced to metal the stannous will not test for it,the tin in our stannous chloride cannot reduce gold that is already a metal.

Oxidize = lose of electrons
Reduction = gain of electrons

Colloidal solution’s can be hard to deal with, how I deal with them is usually dictated by how bad they are.
First if you can let solution settle well, so as much insoluble material is on bottom, decant solution try to filter it, if it filters easy you do not have a problem with tin or colloids.

But if it filters very slow or not at all, and you once had gold in solution with tin, you will have gold in this colloidal mess.
Sometimes you can filter out the bulk with filters like fiberglass Charmin plugs in a funnel (these can be incinerated later), and then filtering solution to catch more insoluble’s with finer filters.

Sometimes boiling with a strong acid solution (sulfuric acid), will help to break the colloids, and let things settle so can collect them.

Sometimes the mess is so bad about the only way to deal with it is to evaporate everything down to powders dry and incinerate it red hot.

Once we get these tin and gold and other metals out of solution we do not want to put them back into solution, until after we oxidize the tin, by the incineration process, wash in boiling HCl with hot water washes (to dissolve the tin oxides as best we can), you can read more details of this process in Harold’s posts he has explained this many (many) times.

Your filters can also be incinerated the same time or saved up.

Also if we wish to use nitric acid on the remaining powders (to remove silver, or base metals), we will have to remove the chloride from them first to do this we can wash, I use a NaOH sodium hydroxide wash in solution to help oxidize the base metals in the powders, the sodium will also form salt water NaCl from the chlorides with the sodium, which can be washed out with hot water, the reason I do this is gold with chlorides can be somewhat volatile at the roasting temperature, and removing as much of the chlorides before can help us from lose of gold in the smoke.
Once well washed these powders can be dried and incinerated, sometimes dry crushed powders will fuse while raising the temperature, becoming like a thick bubbling syrup, when this occurs lowering heat and keeping stirred can help from forming big popping bubbles, which will splash stuff out.

There are a few other tricks I use, do not fill the whole pot (having molten syrupy powders in the pot like an egg, I can get the pan hotter, and stir them around cooking off acids without bubbles popping,

Another trick when I am incinerating large batches is to add some of the previously incinerated powders to the syrupy fused powders, this remove some of the acids or liquids from the syrup, and allows me to dry out the whole batch under higher heat and stirring, without hot syrupy bubbles splashing things out of the pot.

The powders will not always fuse, but when they do they will dry out again with more heating, they will also get hard if dried, I normally let them get almost dried (but not all the way), and re-crush them back to powder, I used a big piece of thick Pyrex glass (old boiler sight glass), for a pestle to crush the lumps to powder, the heat is raised to red hot, keeping the powder stirred, and exposed to air, the metal powders red hot in air oxidize, this will help make the metals to be more easily dissolved in acids later.

If this does not apply to what solution your talking about, then I guessed wrong and I do not know what to say.
 
Yes you hit the nail on the head. And you let know I wasn't necessarily wrong with possible colloidal gold settling to the bottom. I think I will boil it down in small batchs with sulfuric acid. Thanks for the help. I will get started once weather permits.
 
It's been cold and snowing so I haven't gotten to cook down the solutions to powered yet for the collide gold. I did filtered it and burnt my filters and got about 22 grams for gold and silver mix button. It tested for 9k. I put it in with my non magnetic lot.
Which brings me to this question here. I have around 75 grams of what I hope to be just inquarted gold and silver. I know I need 300 ml of nitric acid for ever tzo. So I would need over 700 ml of acid. Will this substitute work?
IN A WIDE-MOUTH GALLON GLASS JAR OR GLASS JUG POUR IN 1 QUART OF SODIUM NITRATE. ADD 1 TO 1.5 CUPS OF WATER AND LET IT SIT OVERNIGHT.(12 HOURS) THEN FILL THE CONTAINER 3/4 FULL WITH SULFURIC ACID (BATTERY ACID/ ELECTROLITE - AVAILABLE FROM AUTO-PARTS STORES)

LET THE MIXTURE SIT FOR 24 HOURS, STIRRING THE MIXTURE EVERY 8 HOURS. (THE SODIUM NITRATE WILL NOT DESOLVE COMPLETELY)

YOU NOW HAVE A HOMEMADE NITRIC ACID THAT IS APPROX 70% AS STRONG AS FULL STRENGTH NITRIC. STIR THE MIX DAILY AND JUST ADD MORE SULFURIC ACID AFTER YOU POUR OFF THE MIXED ACID. Will this work or be strong enough to do the job?

Nitric is just getting too expensive.
Thanks in advance.
 
reign21male said:
I know I need 300 ml of nitric acid for ever tzo
.
The last time I checked, it takes 1.17ml of Nitric Acid, along with the same amount of water to dissolve 1 gram of silver. So, to dissolve 1ozT of silver, you would need 36.387 ml of Nitric Acid and the same amount of water, for a total of 72.774ml of solution. Also, from what I've read, if you heat the Nitric, it'll dissolve even more silver.

Kevin
 
testerman said:
reign21male said:
I know I need 300 ml of nitric acid for ever tzo
.
The last time I checked, it takes 1.17ml of Nitric Acid, along with the same amount of water to dissolve 1 gram of silver. So, to dissolve 1ozT of silver, you would need 36.387 ml of Nitric Acid and the same amount of water, for a total of 72.774ml of solution. Also, from what I've read, if you heat the Nitric, it'll dissolve even more silver.

Kevin

I meant to correct that. Thank you for doing it for me. And as for the recipe Butcher was kind enough to add me on it. It isn't all that it claims to be. thanks to Kevin and Butcher
 
Butcher, I ran into a problem when I was evaporating 8 QTs of waste looking for colloidal gold. At the end my pot over flowed so i poured baking soda on the spillage and scraped it up and put it in the pot with the last of my waste solution. It foamed up and got syrupy like yopu said it would but after a short time with the torch it looks like this. Here are pictures of what I filtered out. Should I boil this with water or HCL?
 

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Jason, when you neutralized the acid, all the metals came out of solution. what you have now is all the metals mixed up again. i would crush and powder the mass you have and screen it very fine. give it a hard boil in hcl to remove as much oxide as you can.alternate hcl bath and water rinse until the hcl stays clear. then process any remaining solids in AR and test with stannous for values. also test the first hcl bath for values as well.
 
Geo said:
Jason, when you neutralized the acid, all the metals came out of solution. what you have now is all the metals mixed up again. i would crush and powder the mass you have and screen it very fine. give it a hard boil in hcl to remove as much oxide as you can.alternate hcl bath and water rinse until the hcl stays clear. then process any remaining solids in AR and test with stannous for values. also test the first hcl bath for values as well.

Thanks geo I will get started on that asap.
 
Nitric acid and baking soda, fist gives sodium nitrate and a carbonic acid:
HNO3 + NaHCO3 --> NaNO3 + H2CO3
Then:
NaNO3 + H2CO3 --> NaNO3 + H2O + CO3 gas

So we see here you also formed a nitrate salt in your powders.

This is not considering other acidic metal salts in the mix or other reactions, which would be involved.
As Geo stated you would drop most all of the metals from solution from adjusting the pH, and you can also form other salts, and in the evaporation, you will also concentrate, to further precipitate metal salts.

When you say this is what this what your material looks like after a short time under the torch, and you show a wet gray powder in the filter in the picture.

It sounds to me like you were working towards incineration, but a short time under the torch to me does not sound like you had a completed the process of incineration, unless you got these powders to glow red hot, keeping them crushed and stirred to oxidize them, keeping them glowing red hot, until no smoke of acid or carbon based material leaves the powders, and allowing the powders to get hot enough to glow red hot and long enough to oxidize completely the base metals in the powders, which can take time at this high red heat, to drive off acids from the salts as gas (many times noticeable by a color change in the powders as the powders oxidize).

So for some reason I feel you may have torched the powders a little, but I wonder if you actually gave them a good roast or incineration, which would actually improve what your working with, and oxidize these powders.

First make sure you did incinerate them well, if you did not I would redo that process, getting them glowing red hot, and keeping them red hot about a half hour...

It looks like you filtered these powders (which would help to wash out some of the acid salts or soluble metals.

At this point (since I do not believe these to be roasted well), I would put filter and powders in a ceramic casserole dish on the hot plate solid burner, slowly raise heat to dry the powders, raise heat as they are dried keeping powders stirred and crushed to powders, a Pyrex pestle works good to crush the powder, raise heat but (keep heat low enough to prevent forming gas bubbles that will pop and splash powders or syrup out of dish), continue till powders give off no gases, then when powders completely dried and crushed with hot plate on high heat from below use the torch from above (keeping powders crushed and stirred) make the powders glow red hot and keep them red hot and stirred for long enough time to drive off all acids or other salts and oxidize the base metals in oxygen (or air) stirring them well to get good exposure, glowing red hot for 30 minutes or longer at a glowing red heat.

Turn down hot plate to cool powders, spray the dish with a mist from a water bottle to wash sides of the dish down add water to cover the powders give a boil in water, lower heat and let powders settle, remove the water wash after powders settle well put keep water hot, decant wash water from dish with suction bulb tool and pipette, if this water is highly colored with metals repeat water boil wash and decant till water comes off fairly clear.

Leaving powders in the dish cover with HCL, raise heat a little at a time till at a slow boil, keeping powders stirred well and crushing out any lumps, give this a good long boil to dissolve some of the metal base oxides, as metal chlorides, and converting some like silver or lead to chlorides as well, lower heat add just a small amount of water (we do not want to dilute this acid too much, but we also do not want to pick up silver later if left too concentrated) let powders settle well but keep it as warm as you can without the heat stirring the powders, after it has settled well decant this acid wash with your suction bulb tools while still hot to pick up lead chloride, tin chlorides and other base metal chlorides, the this liquid is decanted to a cooling and settling jar (you may see lead crystals form in this jar as solution is cooled, there also may be traces of value carried over to this jar,
(So I normally save these to process later when I collect a jar full of these powders).
If this HCl wash is highly colored with metals I repeat the HCl wash.

Again powders stay in the dish all the time.

Then I give boiling hot water washes until these washes come clear, and I no longer am picking up metals like lead, following the techniques described above.

This helps to remove many of the trouble some metals, like tin, lead, and base metals oxides as chlorides.

From here I will process a couple of different ways depending how much, and what I have left in these powders.

Much depends what I am dealing with, and what I wish to do with it or how I plan to process it.

If much copper or other base metal I may go to an acid peroxide process to remove more base metals (but leaving my more valuable powders) being careful not to dissolve gold or remove the fluffy silver when I decant.

Or for a material with higher grade powders of gold and silver and possible PGM I may just dissolve silver and palladium and copper and so on in nitric acid, letting powders settle well before decanting these metals to a jar, settled and filtered before cementing values out this solution with a copper metal buss bar, then the powders left in the dish would go to aqua regia to put gold into solution.

Or if the material was just gold which was in high content to base metal and silver I may just go for the gold, using HCl/NaClO bleach (easier to deal with) or using aqua regia

I normally keep powders in the dish on the hot plate from beginning of the process till the end of the process, as much as possible, decanting solutions with suction tools as the metals dissolve into solution, depending on what these decanted solutions are is how they are processed, most of the time they are decanted to settling jars, let sit for a long period of time till solution is clear, then solution is decanted and filtered before being further processed.

The remaining powders in my dish after all of this may contain sand, or maybe even some PGM or other undissolved valuable metal, just because it did not dissolve I do not consider it invaluable, depending on what I am working on these insoluble powders may go to a plastic coffee can with other material to be incinerated and processed again later, the scrap in this bucket may contain many other things like IC chips, ceramic capacitors bits of filter scrap and other material which may hold some value.

The goal is to incinerate the troublesome metal powders driving off all previous acids or salts to oxidize the metals that will oxidize, then remove these troublesome metals in washes, also removing the base metals, and then put only the valuable metals in solution, and to process each of these solutions to recover them for values for further refining.

The Idea is also a one pot heating vessel continued reaction and process reaction from beginning to end, keeping powders in the pot as much as possible, and just removing dissolved liquids to remove troublesome metals and base metals in washes,(although several jars are used) keeping from moving powder from place to place and losing values in each move, or in filters and so on, use settling as much as possible, and filtering only fairly pure liquids, processing the powders in each step to remove unwanted metals and keeping the valuable metals in the pot until you can dissolve the values in a fairly pure condition, to recover the values in the purest condition possible.

Since your powders I believe came from electronic scrap you should choose a process to deal with what these contain.

Also keep in mind any time a powder has come from, or contains salts of chloride or which has previously seen a reaction with HCl and you wish to use nitric later, and your goal is not to put the gold into solution, but to remove base metals with the nitric, these powders will need to be incinerated again to remove the chlorides before using nitric acid, (this can be done in the same ceramic casserole dish). But if your goal is to dissolve gold you can move on to the next step.

Keeping in mind and using what you have learned from Hokes book (how metals react in solution).
 

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Thank you Butcher, even though this may not change the process I will clarify. This isnt e scrape. This was a mess I made when I melted gold fill and real gold together. I boiled it in nitric and then I had made the grave mistake of using AR which in the I guess 2.5 months that i have been working on this. I really havent come out with any gold maybe a 1.5 grams 18k which would only be a tiny bite of what I put in. So I was left with my solution. In which you believed I had made colloidal gold which I most likely did, since the gold could only be in the solution or waste. So I started but pouring 98% sulfuric acid In the big vat. Then I started the long process of evaporating what I think is 8 qts of solution. So when I almost had all of the solution evaporated I saw a bunch stuff that had settled over the 2.5 months and so I filtered it. After the pot boiled over I cleaned up with banking soda and add all of it back to the pot. As the liquid started to foam and bubble it turn from dark green to gray. And it would start to bubble up and I would have to turn the heat down and then finally, when I started to stir it I became hard powder. And what you see in the pot is what was left of the solution. For some reason my picture always show up out of ordered. so this is what it should look like. Sorry I didnt clairify that earlier. I only had a a few mins at lunch to post my question. I hope this was clearer.
Thanks GEO and Butcher.
 

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Ok if I understand it was captured in the filter first, and dried it is now dried clumps in the vision ware dish.


Crush, to powder, heat raise heat slowly, and keep raising heat, it will most likely fuse the salts to a syrup, if this happens lower heat just below the point where gases form and try to pop and splash out of the dish, heat to drive acid gases from fused salts (keep stirred) till they dry again.

Sometimes if I have filter dried papers from previous processes I will add these to the fused syrupy salts, this clumps the syrup allowing me to raise the heat without gases bubbling and popping syrup out of the dish making the process a little faster.

The syrupy fused salts will dry again as acids leave the salts, keeping this stirred and this point will make re-crushing easier later when fused salts dry to hard clumps, crush the powders again, raise heat, when at high heat cook until no more fumes evolve then use the torch to incinerate as described in the above discussion...

I have incinerated in a vision ware skillet, similar to the pot you have, but I have not tried it in a vision-ware soup pot like in your picture, also my hotplate uses solid cast iron burners, not the coil type burner it looks like you are using, I know the vision-ware skillet will take the punishment on the solid cast iron hotplate and me using my torch, but I do not know if the soup pot would handle it and with the coil hotplate without breaking.

You could also use a stainless steel pan (non magnetic) to incinerate the material in.
 
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